.
«
1 03/19/87 United Stat** Environmental Protection Agency
Washington, D.C. 20460
' EPA OSWER Directive Initiation Request
2. Originator Information
Nam* of Contact Pvrwn MalCod* Offic*
CARTER OERR/HRSD
1.Dir*ctlv*NumtMr
9240.0-01
T*l*phon* Number
382-7909
3.T1U*
USER'S GUIDE TO THE CONTRACT LABORATORY PROGRAM
4. Summary of Directly* (Includ* brtef atatarrwnt of purpow)
Oraganic and inorganic analytical program
descriptions; outlines the requirements and
analytical procedures of new CLP protocols
developed from techinical caucus recommendations.
Reflects the status of the program as of July
1984. (10/84, 220 pp) Table of
contents and front matter only. Handbook
available upon request.
k 5. Keywords
* SUPERFUND, CERCLA, CLP, CONTRACT LAB PROGRAM, LAB ANALYSIS, SAMPLE
ANALYSIS
6a.Do*»thl»Dlr»ctlv*Sup*fOKi*Pr*vtou»DirMrttv^a)?| | y** | X| No What directly* (numb*r, tltto)
b.Do*s It Supptenwrt Pr*vtoua Dk*ctlv**(s)? | \ y*» Lxl No What dlr*ctlv* (numbw, tltto)
7. Draft L*v*l
A-Sign*dbyAA/DAA j 1 B - Signed by Offlc* Director I 1 C-ForH*vtow&C
This nvqiwvt Mi*w OSWEH Dr*CtlV*c 9jf*t*m rvrfntn
8. Signature of L«ad Offlc* Dk*ctKr*s Coordinator
9. Nam* and TK1* of Approving Official
BIGLANE
tomrrxnt I" in D*v*lopm*nt
Oat*
Dat*
10/01/84
OSWER OSWER OSWER
DIRECTIVE DIRECTIVE
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UniMd Sartw ~" .'. •
Environmental Protection "~ .
Offia of
*nd FUmcdbl Rvporat
OC 20460
Oentur 1984
P/EPA
User's Guide r^r-;;
.to'the .r"'::-V--^i.$~'-i,J^::;''-.v
Contract Laboratory Program
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FOREWORD
This document has been prepared by the CLP Sample Management Office
specifically for the guidance and direction of program clients.
The organic and inorganic analytical program descriptions herein outline
the requirements and analytical procedures of the new CLP protocols
developed from technical caucus recommendations. These protocols are
being implemented into CLP analysis contracts in 198V. Other analytical
programs, procedures and documentation described herein reflect the
status of the program as of July 1984.
Updated User's Guide sections containing changes to CLP analytical
programs, procedures and documentation will be provided to clients
periodically, in the form of User's Guide amendments. For further
information on the CLP or to obtain additional copies of the User's
Guide, contact the Sample Management Office at 703/557-2490 or FTS
557-2490.
Second Printing
Issued: October 1984
Rev: 10/84
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CHAPTER n DESCRIPTION OF ANALYTICAL SERVICES
Menu of Routine Analytical Services (RAS)
Menu of Special Analytical Services (SAS)
A. Organic Routine Analytical Services (RAS)
1. Sample Matrices, Concentration Levels and Volumes Required
2. Compounds Identified and Quantified
3. Contract Deliverable Requirements
^. Analytical Protocols
a. Water Method
b. Soil/Sediment Method
o Method Detection Limits
5. Contract Quality Control Requirements
B. Inorganic Routine Analytical Services (RAS)
- 1. Sample Matrices, Concentration Levels, Volumes Required
and Preservation Techniques
2. Constituents Identified and Quantified
3. Contract Deliverable Requirements
4. Analytical Protocols
a. Water Method
b. Soil/Sediment Method
c. Detection Limits
5. Contract Quality Control Requirements
C. Oioxin Routine Analytical Services (RAS)
I. Sample Matrix and Volume Required
2. Isomer Identified and Quantified
Page
12
15
16
17
17
19
!9
20
21
21
22
22
25
25
27
27
28
28
29
29
30
33
33
34
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CLP USER'S GUIDE
TABLE OF CONTENTS
CHAPTER 1 BACKGROUND AND INTRODUCTION
A, CLP Objective and Orientation
B. CLP Structure
1. Program Management
a. National Program Office (NPO)
b. Sample Management Office (SMO)
c. Office of Research and Development (ORD), Environmental
d.
Monitoring Systems Laboratory (EMSL/LV)
National Enforcement Investigations Center (NEIC)
Regional Program Support
a. Contract Deputy Project Officers (DPO)
b. Regional Sample Control Centers {RSCC)
c. Technical Caucuses
d. Regional/Laboratory Communication System
Clients/Users
a. EPA Regions
b. States
c. Non-Superfund Clients
Analytical and Support Contractors
a. Contract Analytical Laboratories
b. Hazardous Substances Laboratories (HSL)
c. Sample Bottle Repository
2
3
3
3
5
6
7
7
8
S
9
9
9
9
ID
ID
11
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C. (Dioxin RAS - continued)
3. Contract Deliverable Requirements
4. Analytical Protocols
a. Soil/Sediment Method
b. Method Detection Limits
5. Contract Quality Control Requirements
a High Hazard Sample Preparation (RAS)
1. Sample Matrix, Concentration Level and Volume Required
2. Preparation Procedures
a. Organic Preparation
b. Inorganic Preparation
3. Sample Preparation Deliverables
4. Potential Follow.Up Analyses
E. Special Analytical Services (SAS)
1. SAS Services
a. RAS Plus SAS
(1) Fast Turnaround
(2) Organic - Special Requirements in Addition to RAS
(3) Inorganic - Special Requirements in Addition to RAS
(4) Dioxin - Special Requirements in Addition to RAS
b. All SAS
(1) Organic - Special Requirements Not Provided by RAS
(2) Inorganic - Special Requirements Not Provided by RAS
(3) Dioxin - Special Requirements Not Provided by RAS
(0) High Hazard Sample Analysis - Organic and Inorganic
(5) Special Topics Analysis
2. Contract Deliverable Requirements
3. Contract Quality Control Requirements
34
35
35
36
36
39
39
00
00
00
01
02
04
00
04
45
45
46
46
46
47
47
47
48
48
OS
IV
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CHAPTER m UTILIZATION OF ANALYTICAL SERVICES
A. Regional Allocation System
B. Analysis toitation/Request Procedures
1. RAS Initiation Procedures
a. User Information Required
b. Lead Time Requirements
c. Case Number Assignment and Laboratory Scheduling
d. User Knowledge of Analytical Protocols
2. SAS Initiation Process
a. User Information Required
b. Lead Time Requirements
c. SAS Number Assignment and Laboratory Scheduling
d. User-Provided Analytical Protocol
3. Initiation of RAS High Hazard Sample Preparation
a. User Information Required
b. Lead Time Requirements
c. SAS Number Assignment and Laboratory Scheduling
d. Sample Preparation and Shipment to Analysis Laboratory
«. Procedures for Making Changes to Analytical Requests
C. Sample Documentation
1. Sample Traffic Report (TR)
2. Dioxin Shipment Record (DSR)
3. SAS Packing List (PL)
4. Sample Tag
5. Chain-of-Custody Record
49
51
52
52
52
53
53
50
55
55
56
57
58
59
59
61
61
61
62
63
63
65
66
67
69
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EX Sample Packaging and Shipment
1. Packaging Requirements
2. Shipping Instructions
3. Shipment Coordination
E. Procedures for Problem Resolution
1. Resolving Problems Concerning Sample Shipment and Analysis
2. Resolving Problems Concerning Analytical Data
71
71
72
73
75
75
75
CHAPTER IV AUXILIARY SUPPORT SERVICES
A. Sample Bottle Repository Program
1. Types and Quantities of Bottles Available
2. Ordering Procedures
3. Shipment Information
*. Procedures for Problem Resolution
a. Resolving Problems Concerning Bottle Shipment
b. Resolving Problems Concerning Bottle Contamination
5. Summary of Bottle Cleaning and Quality Control Procedures
B. Information Services
1. Regional Sample List Report
2. Sample Status Information
3. General Program Information
77
78
78
81
82
83
83
83
85
87
87
88
88
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C, Enforcement Support
i. Generation of Enforcement Quality Data
a. Chain-of-Custody and Document Control
b. NEIC Evidence Audits
2. Additional CLP Enforcement Support
a. Request Procedures
b. Requestor Information Required
c. Documentation/Support Provided by CLP
O. Cost Recovery Substantiation
1. Request Procedures
2. Requestor Information Required
3. Documentation Provided by CLP
E. Data Review Services
1. Types of Review Provided
2. Request Procedures
3. Requestor Information Required
4. Documentation Provided by CLP'
89
89
89
90
91
91
91
92
93
93
9*
94
96
96
98
99
99
VII
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F. Analytical Data Review
i. EWSL/LV Data Review
2. Regional Data Review
3. SMO Data Check for Completeness
4. SMO Data Review Services
G. Analytical Methodology Improvement/Development
1. Protocol Standardization and Improvement
2. Method Development
Page
111
111
111
112
112
113
113
ix
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CHAPTER V PROGRAM QUALITY ASSURANCE
A. fctterface with Agency Quality Assurance
B» Laboratory Selection Process
1. Bid Price
2. Pre-Award Bid Confirmation
a. Performance Evaluation Sample Analysis
b. Standard Operating Procedures
c. Laboratory Evaluation
C. Laboratory Start-Up Process
1. Provision of Standards to Laboratory
2. PO Review of First Data Packages
3. PO/DPO Laboratory Visits
4. PO/DPO/SMO/Lab Communication
D. Laboratory Performance Evaluation
1. Performance Evaluation Sample Analysis
2. Laboratory Site Evaluation
3. Corrective Action
E. Sample Data Evaluation
1. Inter comparison Check Sample Studies
2. Regional Sample Split/Spike Programs
101
102
104
104
105
105
106
106
106
106
107
IDS
108
108
108
110
110
110
Vlll
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Index to Appendices (continued)
Page
Sample Packaging and Shipment: C-25
Sample Packaging Sum mar/ C-26
Sample Shipment Coordination Checklist C-27
Potential Problems with Sample Shipment and Analysis C-28
Telephone Record Log C-29
APPENDIX D: AUXILIARY SUPPORT SERVICES DOCUMENTATION D-l
Sample Bottle Repository Delivery Order Form D-2
Sample Bottle Repository Packing List D-3
Example oi Regional Sample List D-4
Case File Purge Materials D-5
Example of NEIC Sample Profile for Organic* Samples D-6
Example of NEIC Sample Profile for Inorganics Samples D-7
OWPE Cost Recovery Checklist D-8 •
SMO Data Review Request Memorandum D-li
QA/QC Compliance Report: D-14
Example of Organics Report Forms D-l 3
Example of Inorganics Report Forms D-29
APPENDIX E: REFERENCES E-l
Analytical References E-2
Safety References £-3
Sampling References E-4
Shipping References E-4
XI
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CLP USER'S GUIDE
INDEX TO APPENDICES
APPENDIX A: CLP DIRECTORY
EPA Headquarters and National Laboratories
Regional Deputy Project Officers
Regional Sample Control Centers
Sample Management Office
APPENDIX B: RAS DELIVERABLES AND DATA REPORTING FORMS
RAS Organic Deliverables Index
RAS Organic Data Reporting Forms
RAS Inorganic Data Deliverables Summary
RAS Inorganic Data Reporting Forms
RAS Dioxin Data Deliverables Summary
RAS Dioxin Data Reporting Forms
APPENDIX C: SAMPLE INFORMATION AND DOCUMENTATION
Planned Sampling Activity Requiring CLP Analyses Form
Organic Sample Collection Requirements - Water
Organic Sample Collection Requirements - Soil/Sediment
Inorganic Sample Collection Requirements - Water
Inorganic Sample Collection Requirements - Soil/Sediment
High Hazard Sample Collection Requirements - Liquid and Solid
Dioxin Sample Collection Requirements - Soil/Sediment
Special Analytical Services Client Request Form
Sample Documentation:
Organic Traffic Report and Completed Example
Inorganic Traffic Report and Completed Example
High Hazard Traffic Report and Completed Example
Dioxin Shipment Record and Completed Example
SAS Packing List and Completed Example
Examples of Sample Tag and Custody Seal
Chain of Custody Record and Completed Example
.A-l
A-2
A-5
A-8
B-l
B-2
B-6
B-2 8
B-2 9
C-l
C-2
C-3
C-*
C-5
C-6
C-7
C-8
C-9
C-ll
C-12
C-l*
C-I6
C-1S
C-20
C-22
C-23
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NouonooHiNi ONV
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CLP Structure
The CLP effort Involves numerous Agency, contractor and other groups through-
out the country. These organizations are identified and their rote in the program
described in the following sections. The following table, Interrelationships of
Program Principals, graphically illustrates the interaction of these groups in the
CLP operation. In addition, Appendix A is a program directory containing
addresses and telephone numbers of key program personnel
I. Program Management
a. National Program Office (NPO)
The CLP is directed by the National Program Office, in EPA
Headquarter* Support Services Branch (55B), Hazardous Response
Support Division (HRSD), Office of Emergency and Remedial
Response (OERR), in Washington, DC The NPO is comprised of the
National Program Manager, Organic and Inorganic Technical
Officers, and a Quality Assurance Officer, who also provides QA
support to the OERR.
NPO responsibilities include: overall management of the CLP in
terms of program objectives, expansion and interface with clients and
*
other groups; policy, and budget formation and implementation;
administration of analytical and support contracts; development and
technical review of analytical protocols; review of analytical special
services subcontracts and CLP-generated laboratory data; develop-
ment of CLP analytical and support services contracts; monitoring
and formal evaluation of analytical and support contractors; and,
direction of CLP quality assurance (QA) in coordination with overall
OERR QA activities.
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CHAPTER I
BACKGROUND AND INTRODUCTION
The purpose of this chapter is to present the basic Contract Laboratory Program (CLP)
objective and orientation, and to familiarize the reader with program structure. This
background information is provided to facilitate better understanding and more
efficient utilization of program services.
A. CLP Objective and Orientation
The CLP supports the Agency * Super fund effort under the 1980 Comprehensive
Environmental Response, Compensation, and Liability Act (CERCLA) by
providing a range of state-of-the-art chemical analysis services of known quality
on a high-volume, cost-effective basis. The central and overriding assumption
governing the structure and function of the CLP is the basic requirement to
provide tegallyxJefensible analytical results for use in supporting Agency
enforcement actions. Therefore, a high level of quality assurance and docu-
mentation has been incorporated in all aspects of program activities.
The ongoing CLP objective is to develop, manage and improve its analytical
programs in support of all Super fund requirements. This objective is
accomplished by continuously increasing analytical capacity and adjusting
analytical program requirements and related support services to better meet
Agency needs.
The CLP supplies analytical services in direct response to requests from the EPA
Regions, the primary users of the program. The CLP is a service program
designed to provide a wide range of enforcementxjuality analytical services in
response to the changing needs and requirements of the user community. This
client orientation is a key factor in the design and application of ail CLP
services and responses.
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The National Program Manager (NPM), in addition to directing
program staff, is responsible for the formulation of program policies
and direction; communicates with the Regional and Agency
communities on a continuing basis, keeping all parties apprised of
program activities and receiving input on program effectiveness;
administers several program support contracts; and handles financial
and contractual aspects of the program.
The Organics and Inorganics Technical Officers serve as Project
Officers (POs) on laboratory analytical contracts. The POs are
responsible for technical program decisions, contract administration
and contractor performance evaluation. The POs work closely with
the Regional Deputy Project Officers (DPOs) and laboratories on a
daily basis in resolving technical issues. The POs direct the ongoing
effort to improve contract language and analytical methodologies,
and conduct technical caucuses for purposes of CLP data and
protocol review.
The Quality Assurance (QA) Officer coordinates all aspects of
program application of QA procedures. The QA Officer works closely
with EPA Headquarters Office of Research and Development (ORD)
and the ORD's Environmental Monitoring Systems Laboratory in Las
Vegas (EMSL/LV) which provides QA support to the CLP. The QA
Officer also coordinates with the POs and EMSL/LV in refining and
updating analytical method QA procedures.
b. Sample Management Office (SMO)
The contractor-operated Sample Management Office functions in
direct support of the NPO, providing management, operations and
administrative support to the CLP. The primary objective of the
SMO operation is to facilitate optimal use of program analytical
resources. SMO activities fall into the following areas: (1) sample
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d. National Enforcement Investigations Center (NEIC)
The NEIC advises the NPO in defining and applying program enforce.
ment requirements. NEIC-developed sample custody procedures,
chain-of-custody records, sample tags and custody seals are utilized
in the CLP to maintain the validity of sample analyses for supporting
Agency enforcement actions. NEIC routinely performs evidence
audits of CLP laboratories and generates sample profiles used in
Agency enforcement litigation. A description of NEIC* evidence
audit process appears in Chapter IV, Section C.
2. Regional Program Support
The Region plays an integral role in program activities, both as the primary
CLP user and as a key part of analytical program management. The
decentralization of program responsibilities to the Regions has evolved
with the expansion of the program, as a means to more effectively direct
program operations nationwide. Extended Regional participation in the
program has and will continue to increase the program's responsiveness to
Superfund requirements.
a. Contract Deputy Project Officers
*
*
In January, 1984, Regional Administrators appointed a CLP technical
Deputy Project Officer (DPO) for each Regional office. Under
direction of the NPO, the Regional DPO assumes a portion of the
responsibility for monitoring the laboratory contractors physically
located in the Region. The DPO works closely with the NPO Project
Officer in responding to identified problems in laboratory operations
and performs laboratory site evaluations. Other specific DPO
responsibilities will be defined as the system evolves.
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scheduling and tracking; (2) Special Analytical Services (SAS) subc-
ontracting; (3) laboratory invoice processing; (<0 maintenance oi
CLP records and management reporting; and (5) NPO management
and administrative support
SMO routinely receives analytical requests from the Regions,
coordinates and schedules sample analyses, tracks sample shipment
and analyses, receives and checks data for completeness, and
maintains a repository of sampling records and program data. In
response to client requests for non-routine types of analyses, SMO
subcontracts for SAS, performing scheduling and tracking for SAS
efforts as outlined above. SMO maintains a comprehensive data base
of CLP services, performance and utilization, and generates a variety
of management and user reports.
c. USEPA Office of Research and Development (ORD), Environmental
Monitoring Systems Laboratory/Las Vegas (EMSL/LV)
Program quality assurance support is provided by EPA ORO through
EMSL/LV. EMSL/LV functions as the quality assurance arm of the
CLP, providing advice and support to the NPO. Specifically,
EMSL/LV assists in performing pre-award and post-award facilities
audits of laboratories; prepares performance evaluation (PE) samples
for pre-award and post-a ward evaluations of laboratory performance;
evaluates pre-award and post-award PE sample data; and performs
QA audits on CLP-generated data. Additionally, EMSL/LV is
responsible for: providing analytical standards to program
laboratories through the contractor-opera ted QA Materials Bank;
operating the program's QA Database, performing program and
laboratory trend analyses used in developing and updating contract
QC criteria; directing operation of the Superfund Quality Assurance
Support Laboratory (QASL) at the University of Nevada, Las Vegas;
and, assisting in evaluation of CLP analytical methods and protocols.
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The two tables which follow outline the menu of services available under the CUP'S
RAS and SAS programs. The remainder of Chapter II describes each analytical
program in terms of:
o Sample matrices, concentration levels and volumes required.
o Compounds identified and quantified.
o Description of analytical protocols and detection limits.
o Contract quality control requirements.
o Contract deliverable requirements.
The organics and inorganics RAS sections present the caucus-revised protocols being
implemented in 1984.
The client should carefuly consider the provisions of each CLP analytical program
during the planning stages of a sampling event to determine the applicability of the
analysis to user needs.
In addition to the material included in this Guide, Regional DPOs maintain a Master
Copy notebook of each Statement of Work under which CLP RAS laboratory
contractors operate. Users are instructed to consult the Region's Master Copy SOWs
for detailed analytical information.
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CHAPTER II
DESCRIPTION OF ANALYTICAL SERVICES
The Contract Laboratory Program provides standardized and specialized analytical
services to support a variety of Superfund sampling activities, from those associated
with the smallest preliminary site investigation to those of large-scale, complex
remedial, monitoring and enforcement actions. h response to the increasing
analytical demands of its client base, the CLP has continually expanded its analytical
capacity for standardized analyses through frequent IFB solicitations. Currently the
CLP is able to provide over 6,000 sample analyses per month through its routine and
specialized analytical services programs. The CLP will continue to adjust analytical
capabilities and capacity in response to Regional client needs.
The CLP operates five separate analytical programs:
o Organic Routine Analytical Services (RAS),
o inorganic RAS,
o Oioxin RAS,
o High Hazard (HH) Sample Preparation RAS, and
o Special Analytical Services (SAS).
Organic, inorganic and dioxin RAS program analyses are performed by a network of
laboratories operating under firm, fixed-price contracts with the EPA. The HH sample
preparation RAS program provides preparation and extraction of high concentration
samples prior to organic and inorganic compound analyses through CLP or Regional
laboratories. HH preparation services are provided through the program's contractor-
operated Hazardous Substances Laboratories at EPA* NEIC and EMSL/LV facilities.
The SAS program provides unique, non-standardized analytical services for organic and
inorganic compounds in a variety of matrices, to meet specific analytical requirements
which do not fall under RAS programs. SAS services are provided through individual
fixed-price subcontracts awarded to qualified laboratories.
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CHAPTER II
DESCRIPTION OF ANALYTICAL SERVICES
12
L
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concentration liquid and solid samples for subsequent organic and
inorganic anal/sis by CLP or Regional laboratories. A description of
the HH sample preparation RAS program appears in Chapter II
c. Sample Bottle Repository
The Super fund Sample Bottle Repository program was established by
the NPO in May 1982, to provide a common source of clean, QC-
tested sampling containers for samples processed through the CLP.
The objective of the program is to eliminate the potential of bottle
contamination that would affect the validity of sample data. The
contractor-operated repository serves as a central source for several
types of pre-cleaned sampling bottles and is routinely utilized by
Regional and contract personnel performing Super fund sampling
activities. Repository services are detailed in Chapter IV.
11
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c. Non-Super fund Clients
Program services are available to support non-Su;>erfund clients on a
turn-interfering" basis. Non-Superfund analyses are provided by the
CLP through use of an accounting system whereby analytical costs
are charged back to the requestor. Non-5uperfund clients currently
include other government agencies and other EPA programs, such as
Acid Rain, Solid Waste and the National Oioxin Study.
Analytical and Support Contractors
a. Contract Analytical Laboratories
The CLP* analysis contractors come from the nationwide community
of chemical analytical laboratory facilities. To become part of the
CLP, laboratories must meet stringent requirements and standards
for equipment, personnel, laboratory practices, analytical operations,
and quality control operations. Firm, fixed-price contracts are
awarded competitively to the lowest responsive, responsible bidders
through the government's Invitation for Bid (IFB) process. Low-
priced bidders miist successfully analyze performance samples and
pass a pre-award laboratory audit before a contract is awarded.
After contract award, laboratories are closely monitored to assure
compliance with the terms and conditions of the contract. Details of
pre-award and post-award evaluations are addressed in Chapter V.
b. Hazardous Substances Laboratories (HSL)
High hazard (HH) samples are processed by the program's contractor-
operated Hazardous Substances Laboratories at NE1C and EMSL/LV.
Under direction of the NPO, the HSLs prepare and extract high
10
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d. Regional/Laboratory Communication System
In January 1983, the NPO established a system of direct
communication between the Regions and contract laboratories, as a
routine method for Regional data review staff to obtain answers to
technical questions concerning program data in the timeliest and
most direct manner possible, fn this system, designated Regional
communication contacts call designated laboratory communication
contacts as needed to resolve technical data questions. This
communication link also benefits the laboratory by providing direct
feedback on its data product.
3. Clients/Users
a. EPA Regions
The ten EPA Regions are the primary clients of the CLP. As
described in the previous section, each Region has established a
Regional Sample Control Center (RSCC), which schedules ail CLP
analyses requests for the Region, coordinating Regional sampling to
balance with allocated numbers of CLP sample analyses available
each month, and prioritizing the Regions analytical workload when
conflicts occur. RSCC personnel coordinate closely with SMO
throughout Regional sampling events, assisting in tracking sample
shipments to the laboratory and resolving any problems which arise.
to this role, the RSCC also processes analytical requests from state
or other users that are located in the Region's geographical area.
b. States
Under RCRA Section 3012, states undertaking initial site investiga-
tions and entering into cooperative agreements with the government
for cleanup of local waste sites, can utilize CLP services. States
must access CLP analytical services through the RSCC and data
packages are distributed to states through the RSCC.
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b. Regional Sample Control Centers (RSCC)
ti January, 1984, each Region established a Regional Sample Control
Center to centralize ordering of CLP sample analyses within the Region.
The RSCC is comprised of three or more individuals designated as
CLP Authorized Requestors, with one individual named as the
Primary Authorized Requestor (AR) directing the RSCC The RSCC
is responsible for coordinating the level of Regional sampling
activities to correspond with monthly allocations of CLP analyses.
The Primary AR makes final determinations regarding Regional
analysis priorities when conflicts occur. RSCC ARs routinely place
all Regional requests for CLP analyses, coordinate with SMO during
sampling and sample shipment, and resolve any problems which arise
concerning the samples. The RSCC serves as the central point of contact
for questions concerning Regional sampling efforts.
c. Technical Caucuses
In September 1982, the NPO implemented the concept of Technical
Caucus sessions as a means to consistently utilize the scope of
available technical resources in updating analytical program
methodologies and data reporting requirements. Technical caucuses
are held on a regular basis (usually quarterly) and involve
participation of the following groups: EPA Regions, EMSL/LV,
EMSL/Cincinnati, NEIC, contract laboratories, program support
contractors, SMO, NPO and others, as appropriate. These caucuses
have been instrumental in improving CLP protocols and orienting
deliverables directly to user needs. Revised organics and inorganics
protocols developed from caucus recommendations, as presented in
Chapter II, Description of Analytical Services, are being
incorporated into program analytical contracts in
8
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or four 1 -liter amber glass bottles, and two 40-ml glass vials. For RAS
organics analysis of a water sample estimated as medium level, a lour liter
volume is required for extractables and 80 ml for volatiles. The sample
should be collected in four 1-liter amber glass bottles or four 32-ounce
glass jars, and two 40-ml glass vials. For RAS analysis of a soil/sediment
sample estimated as low or medium level, a six ounce volume is required.
The sample should be collected in one 8-ounce glass jar for extractables
and two 120-mI glass vials for volatiles.
Each sample estimated as medium level (both water and soil) must be
enclosed and sealed in a metal paint can for shipment. If it is not certain
whether a sample should be categorized as low or medium level, volume
should be collected as specified for low level samples, however shipping
procedures must be followed as designated for medium level samples.
Sample portions for volatile analysis (water and soil) should be collected so
that the containers are completely filled, leaving no headspace.
Water samples for duplicate analyses must be collected at double the
volume specified for extractables, and triple the volume specified for
volatiles. Additionally, for water samples one field blank should be
supplied per Case, and one volatile trip blank should be supplied per
shipment. No additional volume is required for soil sample duplicate
analyses, and no blanks are currently required for soil samples. Soil blanks
will be used in the future and will be supplied to Regions by EMSL/LV.
If sufficient sample volume is not provided, complete analysis may not be
possible. If this occurs, SMO will contact the RSCC to determine
appropriate adjustments in analysis.
Required sample volumes and container types for RAS organic analysis of
water and soil samples are illustrated in Appendix C. Pre-cleaned sample
bottles are available through the Sample Bottle Repository, as detailed in
Chapter IV.
Rev:10/84
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A. Qrf anic Routine Analytical Servkes (RAS)
!• Simple Matrices. Concentration Levels and Volumes Required
The organic RAS contract methods apply to analysis of water (aqueous) and
soil/sediment samples. Samples for analysis should be tingle-phase,
homogeneous samples of a similar matrix. Sample matrices other than
water, sediment or soil are processed through the SAS program.
Organic RAS contract methods determine concentrations of organic
compounds ranging from low or environmental levels of concentration to
medium levels, where a compound may comprise as much as 15 percent of
the total sample, at the lowest appropriate detection limits. Low level
samples are considered to be those collected off-site, around the perimeter
of a waste site, or in areas where hazards are thought to be significantly
reduced by normal environmental processes. Medium level samples are
most often those collected on-site, in areas of moderate dilution by normal
environmental processes. Low and medium level designations are made in
the field by the sampler to determine packaging and'shipment procedures.
Low and medium level analysis designations are performed within the
laboratory to determine the appropriate analytical protocol to be used.
Samples collected on-site where high levels of contamination are suspected
(i.e., drum samples) are routinely shipped to a Hazardous Substances
Laboratory for sample preparation prior to analysis. High hazard sample
preparation is discussed in Section D of this chapter. Alternatively, HH
sample preparation and analysis can be obtained through SAS as described
in Section E.
The sample volume and container types required for RAS organic analysis
vary according to the matrix and estimated concentration level of the
sample. For RAS organic analysis of a water sample estimated as tow
level, one gallon sample volume is required for extractables (B/N/A), and
SO ml for volatiles (VOA). The sample should be collected in two SO-ounce
17 Rev: 10/84
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2. Compounds Identified and Quantified
The organic RAS program provides identification and quantification of EPA
Hazardous Substances List (HSUst) organic compounds in water and
soil/sediment samples. These compounds, which include priority pollutant
compounds and other organics of interest, are identified on the organic
data reporting sheets in Appendix B.
In addition, the laboratory is required to execute a maximum of 30
EPA/NIH Mass Spectral Library searches for compounds not identified on
the HSL. The 10 peaks of greatest apparent concentration in the volatile
fraction and the 20 peaks in the base^eut^al/acid fraction are tentatively
identified and the concentration estimated, following a visual comparison
of sample spectra with the nearest library matches. The tentative
identification of non-HSL organic compounds provides information on
potential organic contaminants outside of the analytical parameters of the
RAS program.
3. Contract Deliverable Requirements
The organic RAS program specifies contractually-required deliverabies for
sample extraction, volatile analysis and data reporting. These
requirements include: completion of sample extraction within five days of
sample receipt by the laboratory, completion of volatile analysis within
seven days of sample receipt, and completion of extractabie analysis and
reporting of data within 30 days of sample receipt. Laboratories are
subject to financial penalties for late delivery in meeting these deadlines
and incentives for early delivery of the final data package. Illegible data
reports are considered unacceptable, and the laboratory is required to
resubmit readable versions of any illegible pages.
19
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The organic RAS data package supports independent sample data review by
the client user. Through review of data package components, the client
can determine the quality of the analytical data.
Each organic RAS data package includes the following components:
o Narrative report, describing analytical problems encountered and
internal decision tree processes applied.
o Copies of sample Traffic Reports.
o Quality control summary, containing surrogate, reagent blank and
duplicate matrix spike analyses recoveries and instrument tuning and
performance information.
o Sample data, including tabulated results of the organic HSL compounds
identified and quantified, and the tentative identification and estimated
concentration of up to 30 non-HSL organic compounds in greatest
apparent concentration, reported in ug/1 or mg/kg.
o Raw sample analytical data, including sample chromatograms, spectra,
quantitation reports, and calculations.
o Standards data package (for each Case of samples), including chromato-
grams, spectra and data system printouts.
o QC data package, documenting instrument tuning and analytical QC
criteria.
The organic RAS deliverables index and copies of organic data reporting
sheets are contained in Appendix &
Analytical Protocols
The standardized organic analytical methods are based on Federal Register
(FR) Methods 623, 608, and 62* modified lor CLP use in the analysis of
both water and soil samples. Analysis for the organic HSL compounds
includes a GC and GC/MS analysis to achieve the lowest appropriate
detection limits for each sample fraction.
20
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a. Water Method
Water samples for full organic analysis (base/neutral/acid, volatile
and pesticide/PCB compounds) are first prepared and/or solvent
extracted, resulting in three individual sample fractions: eztractable
or semivolatile (B/N/A); volatile (VOA); and pesticide/PCB. Extracts
are cleaned up when necessary, using optional column chromato-
graphy techniques.
The identification and quantification of the organic HSL compounds
in water samples is performed by GC/MS for B/N/A and VOA
fractions, and by GC/EC for the pesticide/PCB fractions.
h addition, the 20 highest non-HSL base/neutral/acid compound
peaks and the 10 highest non-HSL volatile peaks are tentatively
identified and their concentration estimated, using a forward search
of the EPA/NIH Mass Spectral Library.
b. Soil Method
Soil samples for full organic analysis (base/neutrai/acid, volatile and
pesticide/PCB compounds) are prepared by sonification prior to
solvent extraction. Extracts are cleaned up using optional column
chromatography techniques when necessary.
The identification and quantification of the organic HSL compounds
in soil samples is performed by GC/MS for B/N/A and VOA fractions,
and by GC/EC for the pesticide/PCB fraction.
ti addition, the 20 highest non-HSL base/neutral, acid peaks and the
10 highest non-HSL volatile peaks are tentatively identified and their
concentration estimated, using a forward search of the EPA/NIH
Mass Spectral Library.
21
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c. Method Detection Limits
Low level analysis method detection limits (MDLs) for water samples
are based on MDLs for each organic compound using FR Methods 62
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analysis of water and soil samples. CLP contracts define extensive QC
procedures that must be performed and documented, and criteria that must
be met. These include, but are not limited to, the following:
o GC/MS instrument tunes for both volatile and semi-volatile
compound analyses.
o frtitial multi-level calibration for each HSL compound.
o Continuing calibration for each HSL compound.
o Addition of surrogate compounds to each sample and blank for
determining percent recovery information.
o Duplicate matrix spike analyses.
o Reagent blank analyses.
Certain of the above-listed QC procedures demonstrate that the
instrument is operating within contract specifications. These include: a
demonstration that the two tuning compounds (DFTPP for extractables and
BFB for vo la tiles) meet the defined ion abundance criteria; determination
of an average response factor (RF) based on a calibration using several
concentrations of each HSL compound that must meet a defined relative
standard deviation (RSD) and minimum RF; and, a continuing calibration at
a single concentration for each HSL compound for which specified
compounds are flagged as controls which must meet defined percent
difference (%D) from the initial RF or a new initial calibration must be
performed.
Other QC procedures are required to demonstrate the quality of the
analytical data generated. These include: addition of surrogate spikes to
all samples and blanks to monitor sample preparation and analysis and to
provide percent recovery information for each sample, so that the
suitability of the method for each sample (regardless of matrix) may be
established; analysis of duplicate matrix spiked samples to display the
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precision of the method for the particular Case and also to provide percent
recovery information for defined HSL compounds (specified matrix spikes)
as for surrogates; analysis of reagent blanks for each Case or each set of
20 samples (whichever is less) and for each matrix within a Case, to assure
that laboratory contaminants are not reflected in data results.
It is the responsibility of the contractor laboratory to document, in each
data package submitted, that both initial and ongoing instrument and
analytical QC criteria have been met. The laboratory must demonstrate
that instrument tuning and calibration criteria have been met, that
interferences from the analytical system are under control, and that
surrogate spike, matrix spike and matrix spike duplicate recoveries falling
outside contract acceptance windows are attributable to sample matrix
interferences and not to laboratory analytical errors. Any samples
analyzed when contract QC criteria have not been met are re-analyzed by
the laboratory when sufficient sample volume is available.
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&. tiorgank Routine Analytical Services (RAS)
1. Sample Matrices. Concentration Levels, Volumes Required and Preserva-
tion Techniques
The inorganic RAS contract methods apply to analysis of water and
soil/sediment samples. Samples for analysis should be single-phase, homo-
geneous samples of a similar matrix. Sample matrices other than water,
sediment or soil are processed through the SAS program.
ttorganic RAS contract methods determine concentrations of inorganic
priority pollutant (PP) constituents ranging from tow or background levels
of concentration to medium levels, where a compound may comprise up to
15 percent of the total sample. Low level samples are generally those
collected off-site, around the perimeters of a waste site, or in areas where
hazards are thought to be significantly reduced by normal environmental
processes. Low level samples are estimated to contain less than 10 ppm of
the inorganic PP contaminants. Medium level samples are most often
those collected on-site, in areas of moderate dilution by normal environ-
mental processes. Medium level samples are estimated to contain concen-
trations of inorganic PP contaminants up to 15 percent. Low and medium
level designations are made for sample collection volume and shipment
purposes, and for determination of appropriate analytical methods and
QA/QC requirements. Samples estimated to contain concentrations of
inorganic contaminants higher than 15 percent of the sample must be sent
to a Hazardous Substances Laboratory for sample preparation prior to
analysis. High hazard sample preparation is discussed in section D of this
chapter.
The sample volume and container types required for inorganic analysis vary
according to the matrix and estimated concentration level of the sample.
For RAS inorganic analysis of a water sample estimated as low level, one
25
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liter volume is required for metals analysis and one liter volume for
cyanide analysis. The sample should be collected in two 1-liter polyethy-
lene bottles. For RAS inorganic analysis of a water sample estimated as
medium level, sixteen ounce volume is required for metals and sixteen
ounce volume for cyanide. The sample should be collected in two 16-
ounce glass jars. For RAS inorganic analysis of a soil sample estimated as
low or medium level, six ounce sample volume is required for both metals
and cyanide analyses. The sample should be collected in one 8-ounce glass
jar.
For the inorganics RAS program only, it is recommended that a Case of
samples be collected over no more than a three-day period and samples
shipped collectively when the Case is completed.
When collecting low level water samples, a sample aliquot for cyanide
analysis must be collected separately, and different preservation
techniques applied to the metals and cyanide portions, as follows. For the
metals analysis aliquot, the sample should be filtered, then acidified to pH
<2 with HNO.. (If filtration is not possible, the sample should not be
acidified.) For the cyanide aliquot, the preservation techniques specified
in Methods for Chemical Analysis of Water and Waste should be applied.
(Consult Appendix E for complete reference.) No preservation is required
for medium level water samples or low or medium level soil samples.
•
Each medium level sample (water and soil) must be enclosed and sealed in a
metal paint can for shipment. If it is not certain whether a sample should
be categorized as low or medium concentration, volume should be collected
and the sample preserved as specified for low level samples, however
shipping procedures must be followed as designated for medium level
samples. For water samples, one field blank should be supplied for each
Case. No blanks are currently required for soil samples. No additional
volume is required for duplicate analyses of either water or soil samples.
26
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If sufficient sample volume is not provided, analysis of ail required
parameters and/or complete QA/QC determination may not be possible. If
this occurs, SMO will contact the RSCC to determine appropriate adjust-
ments in analysis.
Required sample volume and container types for inorganic RAS analysis of
water and soil samples are illustrated in Appendix C Pre-cleaned sample
bottles are available through the Sample Bottle Repository, as detailed in
Chapter IV.
2. Constituents Identified and Quantified
The inorganic RAS program provides identification and quantification of
metals and cyanide in water and soil/sediment samples. These compounds
are listed on the inorganic data reporting form included in Appendix B.
3. Contract Deliverable Requirements
The inorganic RAS program specifies contractually-required deliverables
for completion of metals and cyanide analysis and submission of the final
data package within 30 days of sample receipt at the laboratory. Labora-
tories are subject to financial penalties for late delivery and incentives for
early delivery of the final data package. Illegible data reports are
considered unacceptable and the laboratory is required to resubmit
readable versions of any illegible pages.
The inorganic RAS data package supports independent sample data review-
by the client user. Through review of data package components, the client
can determine the quality of the analytical data.
Each inorganic RAS data package includes the following components:
o Cover sheet, listing the samples included in the report and narrative
comments describing problems encountered in analysis.
o Tabulated results of inorganic compounds identified and quantified,
reported in ug/1 or mg/kg.
27
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o Analytical results for QC spikes, duplicates, standards, preparation
blanks calibration verification and interference checks.
o Tabulation of instrument detection limits determined in pure water
solutions.
o Raw data system printouts, identifying calibration standards, calibra-
tion blanks, preparation blanks, samples and any atypical dilution,
duplicates, spikes, interference checks and any instrument adjustments
or apparent anomalies on the measurement record.
A summary of RAS inorganic contract deliverables and copies of data
reporting forms are contained in Appendix B.
Analytical Protocols
The standardized inorganic analytical methods are based on Federal
Register (FR) methods, EPA Methods for Chemical Analysis of Water and
Wastes (MCAWW). and Test Methods for Evaluating Solid Waste (SW-8^6).
for the analysis of water and soil samples. Analysis for specified metals
and cyanide is performed by flame, furnace and cold vapor atomic
absorption (AA), colorimetric, distillation, and inductively coupled argon
plasma (ICP) methods.
a. Water Method
Water samples for metals analysis are prepared, acid digested and the
digestate filtered to remove insoluble materials prior to analysis.
Samples are analyzed by AA or ICP methods, and dilutions are
performed where any analyte concentration exceeds the calibrated
range.
For water samples, a quantitative determination for cyanide is made
by midi-distillation and automated colorimetric analysis by MCAWW
Method 333.2.
28
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b. Soli/Sediment Method
Soil samples for metals analysis are prepared and acid digested and
the digestate filtered to remove insoluble materials prior to analysis.
Samples are analyzed by AA or ICP methods, and dilutions are
performed where any analyte concentration exceeds the calibrated
range.
For soil samples, a quantitative determination for cyanide is made by
midi-distillation and automated colorimetric analysis by MCAWW
Method 335.2.
c. Detection Limits
The detection limits listed on the inorganic data sheets (see Appendix
B) are based on analysis of analytes in pure water. Detection limits
for the sample analyses will be higher, depending on the sample
matrix.
Detection limits for low level water samples can be achieved in the
part-per-billion (ppb) to low part-per-million (ppm) range; detection
limits for medium water and soil samples can be achieved in the low-
ppm to mid-ppm range. Detection limits are significantly affected
by matrix interferences and other sample parameters that vary
considerably depending on the nature and homogeneity of the sample,
interferent contaminants that coextract from the sample, and
analytical method. Lowest detection limits are achieved on low level
water samples in the ppb range, where sample matrix interferences
are minimal
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Exhibit C of the Statement of Work of inorganics 1FB contracts
contains minimum contract-required instrument detection levels
(IDLs) that must be met by ail laboratories for each of the metals and
cyanide in pure water.
Extrapolations from the "pure water" IDLs must be made to estimate
the detection limits for low and medium water and soil samples, since
the detection levels achievable for these samples will be highly
dependent on the inorganic species and matrix of each sample.
Although data is reported down to the "pure water" IOL, results
below the contract-required detection levels should be used with
caution.
5. Contract Quality Control Requirements
The CLP quality control (Q0 program for inorganic RAS laboratory
analysis is structured to provide consistent results of known and
documented quality. The program therefore places stringent quality
control requirements on all laboratories performing sample analysis.
Sample data packages contain documentation of a series of QC operations
that allow an experienced chemist to determine the quality of the data and
its applicability to each investigation. In addition, laboratory contracts
contain provisions for sample re-analysis if and when specified QC criteria
are not met by the contract laboratory. Each CLP laboratory is also
encouraged to develop additional internal QA/QC procedures.
The minimum QC requirements of the inorganic RAS program consist of
both an initial and ongoing demonstration of laboratory capability to
generate acceptable precision and accuracy with the contract methods in
the analysis of water and soil samples* CLP contracts define extensive QA
30
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procedures that must be performed and documented, and criteria that must
be met. These include, but are not limited to, the following:
o iutial calibration and calibration verification.
o Continuing calibration verification.
o ICP interference check sample analysis.
o Preparation blank analysis.
o Matrix spike analysis.
o Duplicate sample analysis.
o Laboratory control sample analysis.
The instrument QC operations include initial and continuing calibration
checks, which are performed daily and/or every ten samples. These checks
determine that the analytical system is meeting contract-required
criteria.
Analytical QC operations include: ICP interference check sample, prepara-
tion blank, spiked sample, and duplicate sample analyses. ICP interference
check sample analyses are performed at least twice per eight-Jnour shift, to
verify intereiement and background correction factors. Preparation blank
analyses are performed for each batch of samples or for each set of 20
samples, to ascertain whether sample concentrations reflect contamina-
tion. Spiked sample analyses and duplicate sample analyses are performed
for each matrix wjthin a Case of samples or for each set of 20 samples of a
similar matrix within a Case, to provide information concerning sample
homogeneity, analytical precision and accuracy, the effect of the sample
matrix on the analytical methodology, and to enable the Agency to
evaluate the long-term precision of the method. The laboratory control
sample is a standard carried through sample preparation and analysis
procedures to document the performance of the entire sample process.
31
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It is the responsibility of the contractor laboratory to document, in each
data package submitted, that both initial and ongoing instrument and
analytical QC criteria have been met The laboratory must demonstrate
that instrument calibration criteria have been met, that interferences from
the analytical system are under control, and that spike recoveries falling
outside contract acceptance windows are attributable to sample matrix
interferences and not to laboratory analytical errors. Any samples
analyzed when contract QC criteria have not been met are re-analyzed by
the laboratory.
32
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C Dioxin Routine Analytical Services (RAS)
1. Sample Matrix and Volume Required
The dioxin RAS contract method applies to analysis of soil/sediment
samples only. Samples for analysis should be single-phase, homogeneous
soil/sediment samples of a similar matrix. Sample matrices other than soil
or sediment are processed through the SAS program.
The dioxin RAS contract method determines the presence of the 2,3,7,8-
tetrachlorodibenzo-p-dioxin isomer in soil/sediment samples. No concen-
tration levels are designated in the dioxin program. All samples suspected
to contain dioxin are considered hazardous and handled accordingly.
The sample volume required to perform RAS dioxin analysis is four ounces
of soil or sediment. Each sample should be collected in one <>-ounce glass
jar or one 8-ounce glass jar filled one-half full The collection of more
than four ounces of sample volume is strongly discouraged due to the
hazardous nature and difficulty of disposing of dioxin-contaminated waste.
Each dioxin sample must be enclosed and sealed in a metal paint can for
shipment.
One or more field blanks should be included with each sample batch (2<* or
less samples). The sampler must designate one field blank for matrix spike
analysis and one field sample for duplicate analysis. A rinsate sample,
consisting of organic solvent used in rinsing sampling equipment, may be
included in a batch. (Rinsates are the only liquid samples analyzed in the
dioxin RAS program.) The four ounce sample volume indicated is sufficient
for duplicate analysis; no additional volume should be collected.
Per program procedures, a QA sample should be included in each sample
batch. Prepared Performance Evaluation (PE) samples are available to
Regions through EMSL/LV for this purpose. PE samples should be included
as part of the sample batch.
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Required sample volume and container types for dioxin RAS analysis of
soil/sediment samples are illustrated in Appendix C. Pre-cleaned sample
bottles are available through the Sample Bottle Repository, as detailed in
Chapter IV.
2. tsomer Identified and puantif ied
The dioxin RAS program identifies and quantifies the 2,3,7,8-tetrachlorodi-
benzo-p-dioxin (2,3,7,8-TCDD) isomer of dioxin in soil/sediment samples.
3. Contract Deliverable Requirements
The dioxin RAS program specifies: completion of sample extraction,
analysis, and data reporting within 15 or 30 days (as specified by the client)
following sample receipt at the laboratory; and automatic re-extraction
and/or additional cleanup and re-analysis of samples where certain criteria
are not met in the initial analysis, reported within 10 days of the initial
data due date. Laboratories are subject to financial penalties for late
delivery and incentives for early delivery of the data package. Illegible
data reports are considered unacceptable, and the laboratory is required to
resubmit readable versions of the illegible pages.
The dioxin RAS 'data package supports independent sample data review by
the client user. Through review of data package components, the client
can determine the quality of the analytical data,
Each dioxin RAS data package includes the following components:
o Completed data reporting sheets with appropriate selected ion current
profiles (SICPs) and spectra attached, indicating instrumental (GC/MS)
operating parameters during data acquisition and including ail rejected
sample runs.
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Results of analyses of multi-level concentration calibration solutions,
including SICPs, calculated response factors, plotted concentration
calibration curves, and computer-generated quantitation reports.
SIC Ps generated during each performance check solution analysis and
each concentration calibration solution analysis.
Documentation of acceptable MS calibration for each confirmatory
analysis.
Chronological list of all analyses performed including labeled peaks for
TCDD isomers and partial scan confirmation spectra.
A summary of RAS dioxin data deliverables and copies of data reporting
forms are contained in Appendix B.
Analytical Protocols
a. Soil/Sediment Method
The standardized dioxin analysis contracts utilize EPA-developed
analytical methods for the analysis of 2,3,7,8-TCDD in soil/sediment
samples. Analyses are performed on a •batch" basis. A sample batch
consists of a shipment of 24 or fewer field samples, and normally
includes an equipment rinse solvent (rinsate) sample, one or more
field blanks, and a QA or PE sample.
Prior to analysis, samples are prepared, homogenized and centrifuged
when necessary. Samples are then solvent extracted with continuous
agitation. Column chroma tog raphic and other cleanup procedures are
applied as necessary to eliminate sample components that may
interfere with detection and quantification of the 2",3,7,8-TCDD
isomer.
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The concentrated extract is analyzed by GC/MS using fused silica
capillary column (FSCC) techniques. The identification and quantif-
ication of 2,3,7,8-TCDD is performed using selected ion monitoring
(SIM) GC/MS instrumentation and data systems with the capability to
acquire, store and retrieve SIM data for six ions.
b. Method Detection Limits
The RAS contract method provides procedures for the detection and
measurement of 2,3,7,8-TCDD in soil/sediment samples at concentra-
tions as low as 1 ug/kg (equivalent to L ppb). Column chromato-
graphy and other cleanup procedures are used to eliminate
coextracted sample components, such as PCBs, which may interfere
with the detection of very low levels of TCDD. Matrix interferences
can also occur, depending on the nature and homogeneity of the
sample, and the lowest MDL may not always be achieved.
5. Contract Quality Control Requirements
The CLP quality control (QC) program for dioxin RAS analysis is structured
to provide consistent, accurate and dependable results of known and
documented quality. The program therefore places stringent quality
control requirements on all laboratories performing sample analysis.
Sample data packages contain documentation of a series of QC operations
that allow an experienced chemist to determine the quality of the data and
its applicability to each investigation. Each CLP laboratory is also
encouraged to develop additional internal QA/QC procedures.
The minimum QC requirements of the dioxin RAS program consist of both
initial and ongoing demonstration of laboratory capability to generate
acceptable precision and accuracy within the contract methods for the
analysis of soil/sediment samples for 2,3,7,8-TCDD. CLP contracts define
36
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extensive QC procedures that must be performed and documented, and
criteria that must be met. These include, but are not limited to, the
following:
o ftutial and continuing calibration and instrument performance checks.
o Reagent blank analysis.
o Field blank analysis.
o Native matrix spike analysis (spiked field blank).
o Rinsate (equipment solvent) sample analysis.
o Duplicate sample analysis.
o Confirmatory partial scan analysis.
o Re-analyses, including re-extraction and/or additional cleanup of the
sample extract, when QC criteria are not met in the initial analysis.
The instrument QC operations include initial and continual calibration and
instrument performance cheks. These checks are performed at least twice
during each 8-hour shift to demonstrate continued acceptable GC/MS
resolution, sensitivity, response factor reproducability, and mass range
calibration, and to validate sample data.
Analytical QC operations include: reagent blank, field blank, spiked field
blank, rinsate, duplicate sample and confirmatory partial scan analyses.
Reagent blank analyses are performed by the laboratory prior to and during
analysis of each batch, to demonstrate that identified compound concen-
trations do not reflect laboratory contamination. Field blank analyses are
performed on one fortified (native matrix spike) and other unfortified
samples of uncontaminated soil/sediment included in each batch of
samples, to provide information on false-positive results, on the matrix
effect of the sample on the analytical methodology, and on the accuracy of
the method. Rinsate sample analysis is routinely performed for each batch
of samples to assure that samples have not been contaminated by sampling
equipment. Duplicate sample analysis is performed on one sample of each
batch to determine precision of the method. Confirmatory partial scan
37
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analysis is performed on the sample extract from each batch containing the
highest concentration of unlabeled 2,3,7,8-TCDD, to confirm identification
of the 2,3,7,8-TCDD isomer.
When certain conditions are not met in the initial sample analysis, the
laboratory is required by contract to re-ex tract the sample and/or perform
additional sample cleanup, and re-analyze the sample. Specific require-
ments for automatic sample reruns are delineated in Exhibit C of the IFB
Statement of Work.
It is the responsibility of the contractor laboratory to document, in each
data package submitted, that both initial and ongoing instrument and
analytical QC criteria have been met. The laboratory must demonstrate
that instrument tuning and calibration criteria have been met, that
interferences from the analytical system are under control, and that spike
and duplicate recoveries failing outside contract acceptance windows are
attributable to sample matrix interferences and not to laboratory
analytical errors. Samples analyzed when contract QC criteria have not
been met are re-analyzed by the laboratory. (Consult the dioxin IFB
Statement of Work, Exhibit C, for detailed re-analysis requirements.)
38
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D. High Hazard Sample Preparation (RAS)
The high hazard (HH) sample preparation RAS program processes high
concentration liquid and solid samples for analysis by CLP organic and inorganic
laboratories or EPA Regional laboratories, to this program, samples are shipped
directly to one of the program's Hazardous Substances Laboratories (HSLs),
either the Regulated Substances Laboratory (RSL) at NE1C or the Containment
Facility (CF) at EMSL/LV, for preparation. The client must Cecily the analysis
to be performed at the time HH sample preparation is scheduled to ensure that
the sample extracts are prepared in a manner to be compatible with the
analytical procedures available through the CLP or the methods to be used by
the Regional laboratory. HH sample analysis and HH sample preparation
services can be obtained through Special Analytical Services, as described in
Section E, following.
1. Sample Matrix, Concentration Level and Volume Required
High hazard (HH) sample preparation RAS methods prepare high
concentration liquid and solid samples for analysis of organic and inorganic
compounds, and may include performance of specified characterization
tests as requested by the client. High concentration samples include
samples collected from drums, surface impoundments, direct discharges
and chemical spills, where there is little or no evidence of environmental
dilution. HH samples are suspected to contain greater than 15 percent
concentration of any individual chemical contaminant.
The sample volume required for HH organic and inorganic preparation for
analysis is six ounces for either a liquid or solid sample. Each sample
should be collected in one 8-ounce clear glass jar, filled one -ha If to three-
fourths fulL Each HH sample must be enclosed and sealed in a metal paint
can for shipment. The six ounce volume of sample is sufficient for all
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organic and inorganic preparations and characterization tests. Collection
of additional volume is strongly discouraged due to the hazardous nature
and difficulty of disposing of HH waste.
Required sample volume and container types for high concentration
samples are illustrated in Appendix C Pre-cleaned sample bottles are
available through the Sample Bottle Repository, as detailed in Chapter IV.
2. Preparation Procedures
a. Organic Preparation
Liquid organic samples are solvent extracted and solid organic
samples are extracted with deionized, distilled water prior to
screening by CC/FID and dilution where necessary. Samples are
prepared for organic analysis of RAS Hazardous Substances List
compounds. Upon request, samples may be characterized by testing
for pH, acidity /alkalinity, conductivity, ignitability /flash point,
oxidants, percent moisture, and percent insoluble residue. The HSL
creates reagent blank, spike, and replicate spike QC samples for each
Case to accompany the organic extracts to the analytical laboratory.
b. Inorganic Preparation
Liquid and solid inorganic samples are prepared by KOH fusion,
extraction, or acid digestion procedures, prior to screening by X-ray/
infrared techniques and dilution when necessary. Samples are
prepared lor analysis of priority pollutant metals (including total
mercury). Upon request, samples may be tested for pH, conductivity,
ignitability/flash point, percent moisture, percent insoluble residue,
strong acid anions, and EP Toxicity. The HSL creates reagent blank,
spike, replicate spike and control QC samples for each Case to
accompany the inorganic extracts to the analytical laboratory.
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E. Special Analytical Services (SAS)
In addition to the standardized analyses provided under the Routine Analytical
Services (RAS) program, the CLP1* Special Analytical Services (SAS) program
provides limited customized or specialized analyses, different from or beyond
the scope of the RAS IPS contract protocols but consistent with program
objectives. Services provided through SAS include: quick turnaround analyses,
verification analyses, analyses requiring lower detection limits than RAS
methods provide, identification and quantification of non-priority pollutant and
non-HSL constituents, general waste characterizations, analysis of non-standard
matrices, and other specific analyses.
SAS functions as an extension of the RAS program, matching unique client needs
with individual laboratory resources to accommodate varied analytical requests,
often in a short or emergency time frame, ^dividual SAS subcontracts are
solicited, awarded and administered by Viar and Company, as part of the
company* contract with the EPA for operation of the Sample Management
Office (SMO). The SAS mechanism, by utilizing the subcontracting process,
allows the CLP to procure specialized services in a timely manner, on an as-
needed basis. The flexibility of the SAS program expands the CLP* capabilities
from standardized RAS organic, inorganic and dioxin contract analyses, to
include a wide variety of additional, non-routine analytical services.
SMO procures SAS services by subcontracting with CLP RAS laboratories or
with other laboratories which have demonstrated the ability to meet program
performance requirements, when RAS laboratories cannot meet the analytical
requirement of the SAS RAS contract laboratories are evaluated for current
performance before they are considered for SAS solicitations, and are not
solicited for SAS work if deficient in this area. SAS organic, inorganic and
dioxin analysis requests are solicited to CLP laboratories with IFB contracts in
the appropriate analytical program, and that are performing in accordance with
all contractual requirements. Other laboratories qualify to perform certain
types of SAS work by successful completion of performance evaluation sample
analyses or by justification of unique analytical capability (e.g., Ames testing).
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3. SampJe Preparation peliverables
The HSLs routinely perform sample preparation and designated waste
characterization tests within 21 days of sample receipt, and ship sample
extracts to designated analysis laboratories. Turnaround time for
preparation may be shortened or lengthened depending on the size o! the
project, the complexity of the parameters requested, and current HSL
sample loading and instrument conditions. Sample preparation documenta-
tion prepared by the HSL accompanies the sample extracts to the
designated analysis laboratory and is included as part of the final organic
or inorganic analytical data package.
ft. Potential Follow-Up Analyses
Following organic and inorganic sample preparation, sample extracts are
shipped by the HSL to a previously designated CLP, Regional or other
analysis laboratory. Shipments of extracts are accompanied by chain-of-
custody forms, sample tracking documentation/ sample preparation and
screening documentation, and HSL-prepared QC samples.
Potential follow -up analyses include organic analysis of HSL compounds,
inorganic analysis of PP metals and cyanide, EP Toxicity testing, and other
specified parameters. CLP analysis of HH organic and inorganic samples is
provided through the SAS program, as described in Section E, following.
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1. SAS Services
a. RAS Plus SAS
(1) Fast Turnaround
A fast turnaround request is defined as a request for routine
(RAS) analyses with analysis or data delivery requirements
which call for performance or delivery in a shorter time frame
than the RAS contracts provide. Fast turnaround requests
require application of existing RAS analytical parameters,
methodologies and detection limits, altering only the time
required for performance of analysis and/or delivery of data.
For information on performance/delivery requirements for RAS
organic*, inorganics and dioxin IFBs, reference Part 3 of
Sections A - C of this chapter.
m responding to fast turnaround requests, SAS procurement is
limited by and dependent upon program sample load, laboratory
capacities and laboratory operating conditions at the time of
the request. Because of constant fluctuations in these factors,
it is not possible to obtain fast turnaround service on an
unlimited basis. Therefore, fast turnaround contracts are
solicited only in situations of demonstrated need, and are used
primarily to support EPA emergency actions and to meet
impending litigation deadlines.
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Once the laboratory universe is determined, SMO initiates solicitation via
telephone, contacting a minimum oi three laboratories (contingent upon
availability of a particular analytical service) and describing the requirement.
Laboratories are asked to bid firm, fixed prices) for the performance of specific
types of analyses on a defined number of samples. Laboratory bids are evaluated
by SMO in terms of bid price and responsiveness to the specified task. The SAS
award is made to the lowest bidding laboratory which responds to the program's
analytical requirement. A written, individual SAS subcontract agreement is then
made between the laboratory and Viar and Company, the SMO contractor, for
laboratory performance of specified analytical work.
A laboratory* ability to bid for SAS work and bid prices vary depending on: the
size or scope of the analytical request; data turnaround requirements and
analytical parameters of a particular task; weekly RAS sample loading; and,
laboratory operating conditions at the time of solicitation. Due to the
fluctuation of these factors on a weekly, and often daily basis, the CLP cannot
accommodate all SAS requests received. Currently, SAS services are provided
on a first-come basis; however, Agency requirements can necessitate that
certain work be given priority. tr\ this event, SMO notifies the involved RSCC
Primary Authorized Requestors, who determine Regional sampling priorities.
An analysis request can be processed through SAS only if the types of samples to
be analyzed or the analysis requirements are different than those of the RAS
program. (Consult earlier sections of this chapter for RAS sample types and
analysis requirements.) SAS requests are separated into two basic categories:
"RAS Plus SAS" and "All SAS". These categories are utilized in defining client
requests and pursuant SAS solicitation and award. Analytical services available
through the SAS program are described in the following sections.
Pre-cleaned sample bottles are available through the Sample Bottle Repository,
as detailed in Chapter IV. In this program, bottles are prepared specifically for
RAS analytical work. However, bottles may be utilized in SAS projects as
appropriate.
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«0 Dioxin - Special Requirements in Addition to RAS
A client may need to access the standardized dioxin RAS
program and add to the contract requirements. Any addition to
the standard dioxin analysis requirements constitutes this type
of SAS request The following examples illustrate "RAS Plus
SAS" dioxin requests, with the SAS portion shown underlined:
o 2,3,7,8-TCDD analysis of soil/sediment samples with a
detection limit lower than 1 ppb.
o 2,3,7,8-TCDD analysis plus analysis of other dioxin isomers
or furans.
b. Ail SAS
CLP clients frequently request types of analyses that are outside the
scope of or not directly applicable to the RAS program. This occurs
most often with samples of difficult or unusual matrices and requests
to measure analytical parameters not provided through the RAS
program. In these situations, requests are met through a second SAS
contracting process referred to as "Ail SAS" Five categories of "All
SAS" requests are described in the following sections.
(1) Organic - Special Requirements Not Provided by RAS
o Seven HSUst PCB arochlors analysis only (with or without
method substitutions).
o Specific pesticides/herbicides analysis only.
o Organic analysis on non-aqueous and non-soil/sediment
samples (e.g., oil, tar or biological tissue).
o Organic analysis by non-RAS methods.
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(2) Organic - Special Requirements in Addition to RAS
A common client request is to access the standardized or RAS
organic program and add to the contract requirements. Any
addition to the standard RAS Hazardous Substances List
(HSUst) organic analysis requirements constitutes this type of
SAS request. The following examples illustrate common WRAS
Pius SAS" organic requests, with the SAS portion shown
underlined:
o HSList B/N/A compound analysis at tow detection limits.
o HSList full organic analysis with additional non-HSUst
pesticide/herbicide compounds.
o HSList pesticide compound analyses with additional cleanup.
(3) tiorganic - Special Requirements in Addition to RAS
As with organ ics, it is common for a client to request the
standardized inorganic RAS program and add to the contract
requirements. Any addition to the standard RAS inorganic
analysis requirements constitutes this type of SAS request. The
following examples illustrate common "RAS Plus SAS" inorganic
requests, with the SAS portion shown underlined.
o Metals and cyanide analyses plus nitrate, sulfate. ammonia,
sulf ide, total organic carbon and chloride.
o Metals and cyanide analyses with sample filtration and
preservation.
o Metals and cyanide analyses with sample homogenization.
o Metals analysis at tew detection limits.
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(5) Special Topics Analysis
The SAS program can also accommodate unusual analytical
requests on an "All SAS" basis, when sufficient toad time is
allowed and complete methodology accompanies the request.
These types of analyses include, but are not limited to:
o Biological samples (e.g., fish, turtle tissue) for specific
organic, inorganic or dioxin analyses.
o Air samples (e.g., tenax, charcoal and flurosil tubes) for
specific organic analyses.
o Wipe samples for specific organic or inorganic analyses.
o Methods comparison studies.
o Asbestos analysis.
o Non-Superfund analytical services of any type.
o Acid deposition parameters.
2. Contract Deliverable Requirements
SAS contracts specify required delivery schedules for sample extraction,
analysis and data reporting, as defined by the client requestor. Deliverable
requirements for "RAS Plus SAS" and "All SAS" requests are per RAS
contract deliverable requirements, as applicable, unless otherwise specified
by the client at the time of request.
3. Contract Quality Control Requirements
SAS contracts require laboratory performance of QC procedures and
reporting of QC parameters, as defined by the client requestor. QC
requirements are as specified in RAS program contracts, as applicable,
unless otherwise specified by the client at the time of request. Clients are
encouraged to maintain a high level of QC in all analysis requests, unless
there is substantial reason for deleting certain QC requirements.
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(2) Inorganic - Special Requirements Not Provided by RAS
o Specified elements from the RAS program metals (e.g.,
cadmium, mercury and selenium only).
o Total organic carbon (TOO analysis only (on water or
soil/sediment samples).
o £P Toxtcity tests (metals, pesticides or herbicides).
o Any inorganic analysis on non-aqueous and non-soil/sediment
samples (e.g., oil, tar or biological tissue).
o Metals analysis by non-RAS methods.
(3) Dioxin - Special Requirements Not Provided by RAS
o 2,3,7,8«TCDD in water or fish tissue.
o 2,3,7,S-TCDF (furan) in any matrix.
o Total tetra through octa dioxin and/or furan classes in
varied matrices.
o Analysis by HRGC/HRMS or GC/MS/MS.
(*) High Hazard Sample Analysis — Organic and Inorganic
The SA5 program provides for analysis of High Hazard (HH)
sample extracts -prepared by the Hazardous Substances
Laboratories. HH analysis services are described below.
o Organic analysis for HSUst compounds by GC/MS and
GC/ECD with tentative identification of 30 non-HSList
compounds of greatest concentration.
o friorgamc analysis for KOH fusion total metals and total
mercury.
*7
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S33IAU3S TYDUATYNV JO NOUVZITLLn
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A. Regional Allocation System
An allocation system has been established to equitably apportion available
laboratory space to the Regions during periods of heavy sampling activity when
analysis capacity (or all requests may not be available. When in effect, all
organics RAS and RAS plus SAS Cases are scheduled under the allocation system.
By the first day of each month, the NPO provides the RSCC with the Region's
monthly allocation of organic sample analyses. The RSCC is responsible for
planning the months sampling activities in accordance with the NPO allocation.
Up to the second Thursday in the month, the RSCC requests sample analyses for
all planned Regional sampling activities for that month, assigning a priority to
each activity requested. (Analysis request procedures are delineated in the following
sections of this chapter.) t\ follow-up, the RSCC submits to SMO confirmation of
verbal requests for sample analyses for the month, using the form entitled,
"Planned Sampling Activity Requiring CLP Analyses." An example of this form is
included in Appendix C Copies are available from SMO.
Upon receiving the Region's sampling requests, SMO makes laboratory
assignments for the month, scheduling requests received up to each
Regions allocation limit. Requests for space in excess of the monthly allocation
will not be processed by SMO until requests from all Regions which fall within
allocations have been placed at a laboratory. At this time, any "excess"
laboratory capacity for the month is determined. The NPO then prioritizes
Regional sampling requests which exceed allocations, on a national basis.
Following NPO prioritization, SMO makes laboratory assignments for sampling
activities as prioritized by the NPO, utilizing available laboratory capacity.
For additional information concerning the allocation system, contact SMO* Group
Leader for Analytical Services (see Appendix A).
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CHAPTER HI
UTILIZATION OF ANALYTICAL SERVICES
The CLP provides clients with prompt access to laboratory services through a
documented system of sample scheduling and coordination in which the client plays a
key role. The purpose of this chapter is to familiarize clients with the proper use of
program services. Specific procedures and required documentation are reviewed for
each program, providing complete step-by-step information on how to properly access
the program's analytical resources.
CLP procedures are based on two fundamental requirements: (1) the maintenance of
ongoing communication among Regional Sample Control Center (RSCC), field sampler,
SMO and laboratory personnel; and, (2) the correct use of sample scheduling and
tracking documents by RSCC, field sampler and laboratory personnel The Sample
Management Office (SMO) provides centralized direction and coordination in
scheduling sample analyses through the CLP, and tracks the progress of samples from
the point of collection through final data production. To effectively match the
analytical needs of program clients with the capabilities of appropriate contractor
laboratories, SMO maintains ongoing records which document for each
program: current utilization, availability of resources, and laboratory performance
limitations.
SMO is authorized to accept analytical requests only through the RSCC, centered in
the Region's Environmental Services Division. The RSCC, established by the EPA
Regional Administrator, is responsible for defining the Region's analytical priorities
and placing analytical requests for CLP services through SMO. The RSCC consists of
three or more identified Authorized Requestors (AR), who routinely place analytical
requests through SMO and coordinate with SMO throughout sample shipment and
analysis. The RSCC is responsible for ensuring Regional compliance with the CLP*s
allocation system, as described in the following section. The Primary AR determines
analytical priorities for the Region when conflicts occur.
ftidividuals interested in obtaining CLP analytical support are instructed to contact
their Regional EPA office* Regional Sample Control Center (see Appendix A).
50
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Overestimation of the number of samples to be collected and/or
miscalculation of shipment dates unnecessarily ties up available
laboratory capacity, preventing the efficient management of CLP
analytical resources and rendering the program less than maximally
responsive to all clients. Underestimation of the numbers and types
of samples to be collected may mean that adequate services will not
be available for any additional analyses needed.
b. Lead Time Requirement
When planning for a sampling activity has been completed and at
least one week prior to the scheduled start of sampling, the AR
telephones SMO and places the specific request for RAS services. A
minimum of one week lead time is essential to facilitate laboratory
scheduling and resolution of questions concerning sampling and
analysis procedures, and to allow the sampler adequate time to
prepare the required sample documentation. Advance scheduling is
available through the Regional Allocation System and should be
utilized whenever possible.
c. Case Number Assignment and Laboratory Scheduling
At the time of request, SMO assigns a sequential Case number to
each individual RAS sampling activity. The RSCC records the Case
number and uses it in referencing that request throughout sampling
and analysis. A Case number designates a single group of samples
,i
collected at one site or geographical location during a predetermined
and finite time period and is used to identify a particular RAS
sampling event throughout sample tracking and data production.
SMO then schedules the requested analyses through an appropriate
RAS laboratory. This selection is determined by the types of
analyses, number of samples, program contract capacity, sample
53
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ft. Analysis friitiatjon/Request Procedures
1. RAS Initiation Process
User ^formation Required
To initiate a RAS request, the RSCC Authorized Requestor contacts
the appropriate SMO Controller by telephone and provides a complete
description of the analytical requirement. (SMO personnel are
identified in the CLP Directory, Appendix A.)
SMO requires the following information to initiate a RAS request:
o Name of RSCC Authorized Requestor
o Namets), association, and telephone numbeKs) of
sampling personnel.
o Name and location of the site to be sampled.
o Number and matrix of samples to be collected.
o Type of analyses required; i.e., organic*, inorganics,
dioxin.
o Cyanide analysis requirement (inorganics only).
o Scheduled sample collection and shipment dates.
o Nature of sampling event (i.e., investigation, monitoring,
enforcement, remedial, drilling project).
o Other pertinent information which may effect sample
scheduling or shipment (Le., anticipated delays due
to site access, weather conditions, sampling equipment).
o Name(s) of Regional or contractor contacts for
immediate problem resolution.
The Authorized Requestor is responsible for applying professional
judgment in accurately estimating the numbers and types of samples
and the sample shipment dates of the analytical request.
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and quality control requirements. In addition to the summary
information contained in this User's Guide, the RAS Statement of
Work should be consulted by program users to confirm that the RAS
program is suited to an analytical request. Analytical requirements
differing from RAS parameters are processed through the SAS
program, as described in Section E, Chapter IL
2. SAS Initiation Process
a. User Information Required
To initiate a SAS request, the RSCC Authorized Requestor contacts
the appropriate SMO Controller by telephone and provides a complete
description of the analytical requirement. (SMO personnel are
identified in the CLP Directory, Appendix A.)
SMO requires the following information to initiate a SAS request:
o Name of RSCC Authorized Requestor
o Name(s), association, and telephone numbeKs) of
sampling personnel.
o Name and location of the site to be sampled.
o Number and matrix of samples to be collected.
o Specific analyses required and appropriate protocols.
o Required detection limits.
o Matrix spike and duplicate frequency.
o Justification for fast turnaround request, if appropriate.
o Scheduled sample collection and shipment dates.
o Nature of sampling event (Le., investigation, monitoring,
enforcement, remedial, drilling project).
o Other pertinent information which may affect sample
scheduling or shipment (i.e., anticipated delays due
to site access, weather condition, sampling equipment).
o Name(s) of Regional or contractor contacts for immediate
problem resolution.
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balance among the various laboratories, and laboratory loading and
instrument conditions. When possible, the nearest available labora-
tory is assigned to minimize sample shipping costs.
Once RAS laboratory assignments are made, SMO contacts the AR to
confirm the field investigation plans, identify the laboratories to be
used for the Case, and answer any further questions the sampler may
have regarding program procedures or documentation. At that point,
the AR must indicate all known or anticipated sample scheduling
changes. Any other changes occurring after this time should be
communicated to SMO immediately upon identification to ensure the
timely resolution of conflicts and the optimal allocation of program
resources.
After the initial placement of the RAS request, the RSCC may
choose to assign a logistical contact, such as the team leader in the
sampling effort, to follow up with SMO in finalizing sampling
requirements, initiating changes, and coordinating sample shipment.
d. User Knowledge of Analytical Protocols
It is the responsibility of each RSCC Authorized Requestor to acquire
and maintain a working knowledge of current RAS protocols and
analytical services. SMO provides each Region with Master Copy
notebooks of each RAS program IFB Statement of Work (SOW), which
are periodically updated to reflect program protocol changes. The
SOW represents the standardized requirements which each individual
RAS laboratory is contractually bound to follow. Regional DPOs (see
Appendix A) maintain the Region's Master Copy SOW notebooks.
The analytical SOWs contain specific information on sample types
suited to RAS analysis, compounds identified and quantified, analy-
tical methods, protocols, detection limits, deliverable requirements,
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The AR should consider the above-outlined criteria in determining
the lead time required to schedule a particular SAS effort. As a
general rule, due to protocol diversity and laboratory procurement
procedures, accessing SAS demands greater advance planning and
more lead time than that required for the standardized RAS
programs. The AR should contact SMO several weeks in advance, if
there is a question regarding the advance time needed to schedule a
particular SAS.
c. SAS Number Assignment and Laboratory Scheduling
At the time of request, SMO assigns a sequential SAS number for
each individual SAS sampling activity. If SAS services are being
provided in association with RAS services, SMO also designates the
assigned Case number. The AR records the SAS number and Case
number (if applicable) and uses these numbers in referencing the
request throughout sampling and analysis. Like the Case identifica-
tion, the SAS number designates a single group of samples collected
at one site or geographical location during a predetermined and finite
time period, and is used to identify a particular SAS sampling event
throughout sample tracking and data production.
SAS laboratory selection is based on a telephone solicitation process
for each individual request, which results in a written SAS award to
the lowest qualified bidder. Once SAS laboratory assignments are
made, SMO notifies the AR of the laboratories that will be
performing the analyses.
As indicated, the nature of the SAS laboratory solicitation process
requires the Authorized Requestor to be as exact as possible with all
elements of a request at the time of request. It is understood that
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ti follow-up to the verbal request, the AR must submit a completed
SAS Client Request form to SMO. This form serves as the written
record to clarify and confirm the client's requirement for specialized
analysis work. A copy of the SAS Client Request form is included in
Appendix C.
The Authorized Requestor is responsible for applying professional
judgment in accurately estimating the numbers and types of samples
and the sample shipment dates of the SAS request. Overestimation
of the number of samples to be collected and/or miscalculation of
shipment dates unnecessarily ties up available laboratory capacity,
preventing the efficient management of CLP analytical resources and
rendering the program less than maximally responsive to all clients.
Underestimation of the numbers and types of samples to be collected
may mean that adequate services will not be available for any
additional analyses needed. Depending on the scope of the mis-
calculation, it may require that the entire request be resolicited, and
sampling plans postponed accordingly.
b. Lead Time Requirements
When planning for a sampling activity has been completed, the AR
telephones SMO and places the specific request for SAS services.
Because SAS services are individually procured on a competitive
basis, a minimum lead time of one week is required to process a SAS
request. A two-week lead time is strongly recommended whenever
possible.
Certain types of SAS requests require a longer lead time, as follows.
A minimum lead time of two weeks is required for SAS requests
which involve distribution of protocols (reference item d., this
section). A minimum lead time of three to four weeks is required for
large-scale, analytically complex and/or non-Superfund SAS requests.
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SAS requests which cite the application of well-known analytical
publications do not require additional lead time for distribution, since
laboratories have immediate access to this information. Examples of
such frequently-utilized method manuals are listed below. Additional
analytical references are supplied in Appendix E.
o Methods for Chemical Analysis of Water and Waste. USEPA, 1983.
o Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods, SW-846, USEPA Office of Water and Waste Manage-
ment, 1983.
o Standard Methods for the Examination of Water and Waste Water,
APHA, AWWA, WPCF, Current Edition.
The RSCC should contact SMO several weeks in advance if there is a
question as to whether a particular method will require additional
lead time for distribution.
Initiation of RAS High Hazard Sample Preparation
a. User Information Required
To initiate a request for routine High Hazard (HH) sample prepara-
tion, the RSCC Authorized Requestor contacts the appropriate SMO
Controller by telephone and provides a complete description of the
requirement. (SMO personnel are identified in the CLP Directory,
Appendix A.)
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actual site conditions can vary considerably from expected conditions
and necessitate changes in the sampling plan. However, the AR has
the responsibility to notify SMO immediately of any changes to allow
sufficient time to amend the SAS contract(s) to meet the changed
needs. If an original request is changed significantly, the original
SAS contract will be voided and the entire analysis effort will be
resolicited, requiring an additional week of time before sample
shipment can take place.
d. User-Provided Analytical Protocol
It is the responsibility of the RSCC Authorized Requestor to provide
the applicable analytical protocol and associated Q€ procedures to be
utilized for each SAS request. The analytical methodology and QC
requirements to be applied under a particular SAS must be provided
or referenced at the time of request.
For SAS requests that are based on the use of amended RAS protocols
the AR must specify modifications or additions to these protocols at
the time of request. If such changes are extensive, the AR must
submit changes in written form two weeks in advance of scheduled
sample shipment under the SAS. This additional lead time is required
for protocol distribution and review by solicited laboratories.
For SAS requests which require use of a non-RAS method that is not
commonly available, the AR must submit the method to SMO two
weeks in advance of sample shipment, to allow time for protocol
distribution and review by solicited laboratories.
58
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b. Lead Time Requirement
A minimum lead time of one week is required to schedule RAS HH
sample preparation. Longer lead time is required for a request
involving large numbers of samples or a long-term request.
c. SAS Number Assignment and Laboratory Scheduling
At the time of request, SMO assigns a SAS number to the individual
sampling event and designates the HSL that will perform the sample
preparation, either the Regulated Substances Laboratory at NEIC or
the Containment Facility at EMSL/LV. (It should be noted that HH
sample preparation involves assignment of a SAS number to identify
the sampling event, rather than using a Case number as in other RAS
programs.) The AR records the assigned SAS number, and uses this
number in identifying the HH preparation request throughout sample
tracking and HSL preparation.
d. Sample Preparation and Shipment to Analysis Laboratory
Samples are sent directly to the designated HSL for sample prepara-
tion and characterization tests, if requested. Following the comple-
tion of sample preparation, the HH extracts are shipped by the HSL
to the assigned CLP or non-CLP analysis laboratory. If the analysis
is being performed by a non-CLP laboratory, the client must make
arrangements directly with the HSL for shipment of the extracts to
the appropriate analysis facility.
61
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SMO requires the following information to initiate a High Hazard
RAS request:
o Name of RSCC Authorized Requestor
o Name(s), association, and telephone numbeKs) of
sampling personnel
o Name and location of the site to be sampled.
o Number and matrix of samples to be collected.
o Type of preparation and analyses required.
o Scheduled sample collection and shipment dates.
o Nature of sampling event (Le., investigation, monitoring,
enforcement, remedial, drilling project).
o Suspected hazards associated with the site.
o Other pertinent information which may affect sample
scheduling or shipment (Le., anticipated delays due
to site access, weather conditions, sampling equipment).
o Name(s) of Regional or contractor contacts for
immediate problem resolution.
It is the responsibility of the RSCC Authorized Requestor to provide
information concerning the target analyses for which the samples are
being prepared and to designate the analytical facility (CLP or
Regional) that will be performing the foitownip analyses at the time
of request. Specific- HH sample preparation procedures are then
employed by the Hazardous Substances Laboratory (HSU to render
sample extracts compatible with the specific analytical protocols to
be used by the analysis laboratory.
If the analysis will be performed through the CLP, the AR should
schedule the HH SAS analyses when placing the RAS HH preparation
request. (Consult part 2., preceding for applicable SAS request
procedures.) If the analysis will be performed by a non-CLP
laboratory, it is the client's responsibility to make the necessary
analytical arrangements with the selected laboratory.
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C. Sample Documentation
Each sample processed by the CLP must be properly documented to ensure
timely, correct and complete analysis lor all parameters requested, and most
importantly, to support use of sample data in potential enforcement actions
concerning a site. The CLP documentation system provides the means to
individually identify, track, and monitor each sample from the point of collection
through final data reporting. As used herein, a sample is defined as a
representative specimen collected at a specific location of a waste site at a
particular point in time for a specific analysis, and may reference field samples,
duplicates, replicates, splits, spikes, or blanks, that are shipped from the field to
a laboratory. Specific CLP sample documentation requirements are described in
the following sections.
Whenever questions arise, samplers should contact SMO for direction and
clarification concerning the proper completion and distribution of Case and/or
SAS paperwork for a sampling effort.
1. Sample Traffic Report (TR)
The sample documentation system for the RAS organic, inorganic and HH
sample preparation programs is based on the use of the sample Traffic
Report, a four-part carbonless form printed with a unique sample
identification number. One Traffic Report and its preprinted identification
number is assigned by the sampler to each sample collected. The three
types of TRs currently in use include: Organic, horganic and High Hazard
Traffic Reports. Copies of the three types of TRs are included in Appendix
B, along with examples of properly completed TR forms.
To provide a permanent record for each sample collected, the sampler
completes the appropriate TR, recording the Case Number, site name or
code and location, analysis laboratory, sampling office, dates of sample
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4. Procedures for Making Changes to Analytical Requests
The RSCC Authorized Requestor is responsible lor immediately notifying
the appropriate SMO Controller of all changes in sampling plans as they are
identified. This includes any changes in sample matrices, numbers of
samples, analyses requested, detection limits, shipping dates, postpone-
ments or cancellations. The RSCC Authorized Requestor must maintain
this communication at all stages of the request — before, during and after
shipment of samples to the laboratories. Likewise, the AR-designated
logistical contact must notify the appropriate SMO Controller of any
changes in sampling before and during the on-site sampling event and after
shipment of samples to laboratories.
Failure to notify SMO of such changes can result in: delay in sampling to
Accommodate scheduling changes, delay in start of analysis due to
conflicts, unsuitability of a particular sample to an analytical program,
and/or analysis data inappropriate for client purposes.
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2- Dioxin Shipment Record (DSR)
Sample documentation lor the RAS dioxin program utilizes the CLP Dioxin
Shipment Record, a four-part carbonless form. The OSR provides a
record for one shipment batch of dioxin samples (up to 24 samples).
Samples are individually numbered using the pre-printed labels provided by
SMO with the supply of DSRs, and each sample number is entered on the
DSR by the sampler. A copy of the DSR is included in Appendix C, along
with an example of a properly completed DSR form.
To provide a permanent record of each sample collected, the sampler
completes the DSR, first recording the appropriate CLP Case number and
Batch /Shipment number. Header information pertinent to all samples is
then entered, including: site name/code, tier designation, data turnaround
(15 or 30 days), sampling office, sampling contact, sampling date, date of
shipment, and analysis laboratory. Sample matrix and description
information (e.g., soil/sediment field sample, solvent rinsate) is recorded
for each sample by checking the appropriate box following each sample
number.
After completion of the DSR, the sampler includes the bottom two copies
with the sample shipment to the laboratory. Following sample shipment,
the sampler returns the top copy of the DSR to SMO, The second copy is
the sampler^ file copy. Upon receipt of the sample shipment, the
laboratory documents sample condition and signs the DSR, returning a copy
to SMO and keeping a file copy. Copies of the laboratory-signed DSRs are
provided to the RSCC as part of the data package.
As indicated, two strips of adhesive sample labels pre-printed with unique
sample numbers are provided with the DSR for the sampler's use in labeling
both the sample bottle and the outside of the paint can in which the sample
is packed, in order to protect the labels from water and solvent attack,
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collection and shipment, and sample concentration and matrix. Numbers oi
sample containers and volumes are entered by the sampler beside the
analytical parameters) requested for particular sample portions.
Alter completing the TR, the sampler includes the bottom two copies in
the sample shipment to the laboratory. Following sample shipment, the
sampler returns the top copy of the completed TR to SMO. The second
copy is the sampler's file copy. Upon receipt of samples, the analysis
laboratory documents sample condition and signs the TR, returning the
signed copy to SMO and keeping a laboratory file copy, to the Organics
RAS program, copies of the laboratory signed TRs are provided to the
RSCC as part of the data package, h the Inorganics and High Hazard RAS
programs, SMO provides copies of the TRs to the RSCC separately.
A strip of adhesive sample labels each printed -with the TR sample number
come attached to the TR, for the sampler* use in labeling sample bottles.
The sampler affixes one of these numbered labels to each container making
up the sample. In order to protect the label from water and solvent attack,
each label must be covered with clear waterproof tape. The sample labels,
which bear the TR identification number, permanently identify each
sample collected and link each sample component throughout the analytical
process.
Where a RAS request is associated with an additional SAS request
(described in Chapter n as "RAS Plus SAS" request), TR forms are used for
both RAS and SAS samples. Both the RAS Case number and the SAS
number must be entered on the TR line requesting "Case Number." Both
numbers are required in order to clearly identify and track the sampling
event. Additionally, the sampler must document a brief description of the
SAS requirement on each TR. For example, "VOA - 1 ppb detection limit".
Traffic Report forms are provided by SMO to each Region through the
RSCC One of the RSCC ARs should contact SMO two or more weeks in
advance to order additional TRs for the Region.
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Adhesive sample labels must be provided by the sampler and marked with
the appropriate SAS sample numbers using indelible ink. Labels are
secured to each sample container, and covered with clear waterproof tape
to protect the label from water and solvent attack. The sample label
permanently identifies each sample collected and links each sample
component throughout the analytical process.
SAS Packing Lists are provided by SMO to each Region through the RSCC
One of the RSCC ARs should contact SMO two or more weeks in advance
to order additional SAS PLs.
Sample Tag
To render sample data valid for Agency enforcement uses, individual
samples must be traceable continuously from the time of collection until
the time of introduction as evidence during litigation. One mechanism
utilized in the CLP to comply with this enforcement requirement is the use
of the "sample tag". Each sample removed from a wastesite and
transferred to a laboratory for analysis is identified by a sample tag
containing specific information regarding the sample, as defined by the
EPA National Enforcement Investigations Center (NEIC). Following
sample analysis, sample tags are retained by the laboratory as physical
evidence of sample receipt and analysis, and may later be introduced as
evidence in Agency litigation proceedings. Sample tags can be obtained
through the Regional office.
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libels on both the sample container and the paint can are covered with
clear, waterproof tape. The sample labels permanently identify each
sample collected throughout the analytical process.
Oioxin Shipment Record forms are provided by SMO to each Region
through the RSCC One of the RSCC ARs should contact SMO two or more
weeks in advance to order additional DSRs.
SAS Packing List (PL)
For an "All SAS" type of request (as described in Chapter ID, samplers
utilize the SAS Packing List, a four-part carbonless form. The PL
provides space to list up to 20 samples on one form. SAS samples are
numbered using the SAS number followed by a hyphen and progressive
numerical designation, starting with 1 (e.g., SOOE-1, SOOE-2, SOOE-3, etc.)
If the sampling activity extends over several days and more than one PL is
used, care must be taken not to repeat sample numbers. A copy of the SAS
Packing List is included in Appendix C, along with an example of a properly
completed PL form.
To provide a permanent record of each sample collected, the sampler
completes the PL, recording the SAS number, site name and location,
sampling date, shipment date, analysis laboratory, sampling office, sampler
name and telephone number, individual SAS sample numbers, sample
description and analytical parameters requested.
After completing the PL, the sampler includes the bottom two copies with
the sample shipment to the analysis laboratory. Following sample
shipment, the sampler sends the top copy to SMO. The second copy is the
sampler^ file copy. Upon receipt of samples, the analysis laboratory
documents sample condition and signs the PL, returning a copy to SMO and
keeping a laboratory file copy. Copies of the laboratory-signed PLs are
provided to the RSCC as part of the SAS data package.
66
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Each sample tag is completed and securely attached to the sample
container. Samples are then shipped under chain-of-custody procedures as
described in the following section.
Chain-of-Custody Record
Official custody of samples must be maintained and documented from the
time of sample collection up to introduction as evidence in court, in
accordance with Agency enforcement requirements. The following custody
documentation procedure was developed by NEIC and is used in conjunction
with CLP sample documentation (Le., Traffic Report, Dioxin Shipment
Record and SAS Packing List) for ail samples processed through the CLP.
A sample is considered to be in an individual's custody if the following
criteria are met: it is in your possession or it is in your view after being in
your possession; it was in your possession and then locked up or transferred
to a designated secure area. Under this definition, the team member
actually performing the sampling is personally responsible for the care and
custody of the samples collected until they are transferred or dispatched
properly. fri follow-up, the sampling team leader reviews all field
activities to confirm that proper custody procedures were followed during
the field work.
The Chain-of-Custody Record is employed as physical evidence of sample
custody. Chain-of-Custody Record forms can be obtained through the
Regional office. The sampler completes a Chain-of-Custody Record to
accompany each sample shipment from the field to the laboratory.
Similar information to that entered on the sample tag is recorded on the
Chain-of-Custody Record. Header information includes the project number
and name, samplers' signatures and the CLP Case/SAS number (entered on
the upper right of the form). For each station number, the sampler
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The information recorded on an EPA sample tag includes:
o CLP Case/SAS No(s). - The unique numbers) assigned by
SMO to identify the sampling event. (Entered under
"Remarks" heading.)
o CLP Sample No. — The unique identification number
(from the TR, OSR or PL) used to document that sample.
(Entered under "Remarks" heading.)
o Project Code — The number assigned by EPA to the
sampling project.
o Station No. — A two-digit number assigned by the
sampling team coordinator.
o Date — A six-dig it number indicating the month, day and
year of collection.
o Time — A four-digit number indicating the military time
of collection.
o Station Location — The sampling station description as
specified in the project plan.
o Samplers — Signatures of samplers on the project team.
o Remarks — Case/SAS and sample numbers are entered
here, and any pertinent comments indicated.
o Tag No. - A unique serial number preprinted or stamped
on the tag.
o Lab Sample No. — Reserved for laboratory use.
Additionally, the sample tag contains appropriate spaces for noting that
the sample has been preserved and indicating the analytical parameter(s)
for which the sample will be analyzed. An example of a properly
completed sample tag is included in Appendix C.
68
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D» Sample Packaging and Siipment
1. Packaging Requirements
Samples processed through the CLP must be packaged for shipment in
compliance with current U.S. Department of Transportation (DOT) and
commercial carrier regulations. All required government and commercial
carrier shipping papers must be filled out and shipment classifications
made according to current DOT regulations. (Consult Appendix E for
shipping references.)
Traffic Reports, Dioxin Shipment Records, SAS Packing Lists, Chain-of-
Custody Records, and any other shipping/sample documentation
accompanying the shipment, must be enclosed in a waterproof plastic bag
and taped to the underside of the cooler lid.
Coolers must be sealed with custody seals in such a manner that the
custody seal would be broken if the cooler were opened.
Shipping coolers should have clearly visible return address labels on the
outside. Shipping coolers that are labeled in this manner will be returned
to the sampler by the laboratory within 14 days following laboratory
sample receipt.
hside the cooler, sample containers must be enclosed in clear plastic bags
through which sample tags and labels are visible. For dioxin samples and
water and soil samples suspected to be of medium or high concentration,
each sample must be enclosed in a metal can with a clipped or scalable lid
(paint cans are normally used for this purpose) and surrounded by packing
material such as vermiculite. The outer metal can must be labeled with
the number of the sample contained inside.
71
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indicates: date, time, whether the sample is a composite or grab, station
location, number of containers, analytical parameters, CLP sample
numbers) (from TR, DSR or PL), and sample tag number(s). When
relinquishing the samples for shipment, the sampler signs in the space
indicated at the bottom of the form, entering the date and time the
samples are relinquished. The sampler enters shipper name and airbill
number under the "Remarks" section on the bottom right of the form. An
example of a properly completed Chain-of-Custody Record is included in
Appendix C.
The custody record is completed using waterproof ink. Any corrections are
made by drawing a line through and initialing the error, then entering the
correct information. Erasures are not permissable.
The top, original signature copy of the Chains-Custody Record is
enclosed in plastic (with CLP sample documentation) and secured to the
inside of the cooler lid. A copy of the custody record is retained for the
sampler's files.
Shipping coolers are secured and custody seals are placed across cooler
openings (see Section C., following). As long as custody forms are sealed
inside the sample cooler and custody seals remain intact, commercial
carriers are not required to sign off on the custody form.
Whenever samples are split with a source or government agency, a separate
Chain-of-Custody Record should be prepared for those samples, indicating
with whom the samples are being split and sample tag serial numbers from
splits.
The laboratory representative who accepts the incoming sample shipment
signs and dates the Chain-of-Custody Record to acknowledge receipt of the
samples, completing the sample transfer process. It is then the
laboratory's responsibility to maintain internal log books and records that
provide a custody record throughout sample preparation and analysis.
70
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All samples should be shipped through a reliable commercial carrier, such
as Federal Express, Emory, Pur o la tor, or equivalent. Sampling offices are
responsible for sample shipping charges.
The NEIC/Denver and the ERT/Cincinnati hazardous waste site manuals
(references provided in Appendix E), provide extensive information on
EP ^-approved sample packaging and shipment techniques, fti addition,
questions concerning sample packaging and shipment may be directed to
SMQ.
3. Shipment Coordination
To enable SMO to track the shipment of samples from the field to the
laboratory and ensure timely laboratory receipt of samples, the sampler
must notify SMO immediately following all sample shipments* At that
time, the sampler should provide the following information:
o Sampler name
o Case Number and/or SAS Number of the project.
o Batch numbers (dioxin only)
o Exact numbers) and type(s) of samples shipped.
o Laboratory(s) samples were shipped to.
o Carrier and airbill number(s) for the shipment.
o Method of shipment (e.g., overnight, two-day)
o Date of shipment.
o Any irregularities or anticipated problems with the samples,
including special handling instructions, or deviations from
established sampling procedures.
o States of the sampling project (e.g., final shipment, update
of future shipping schedule).
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Low level water samples for organics analysis must be shipped cooled to
ii°C with ice. No ice should be used in shipping: dioxin samples; inorganic
low level water samples; or, organic/inorganic medium/high level water or
soil samples. Ice is not required in shipping low level soil samples, but may
be utilized at the option of the sampler.
Low and medium level water samples for inorganic analysis require
chemical preservation (reference Chapter II, Section B, for preservation
techniques).
Waterproof, metal ice chests or coolers are the only acceptable type of
sample shipping container. Shipping containers should be packed with non-
combustible, absorbent packing material (vermiculite is recommended)
surrounding the plastic-enclosed sample bottles (or metal cans containing
samples) to avoid sample breakage in transport. Sufficient packing
material should be used so that sample containers will not make contact
during shipment. Earth or ice should never be used to pack samples. Earth
is a contaminant, and ice melts resulting in container breakage.
Unless the sampler requests otherwise through SMO in advance, the
laboratory disposes of unused sample volume, sample bottles and packing
materials 90 days following sample receipt.
A summary of correct sample packaging is illustrated in Appendix C.
2. Shipping Instructions
Samples for organics analysis must be shipped "Priority One/Overnight." If
shipment requires more than a 24-hour period, sample holding times can be
exceeded compromising the integrity of the sample analyses.
Samples for inorganics analysis should be held until sampling for the Case
is complete and shipped "Standard Air" for two-day delivery. In the RAS
inorganic program, three days is the recommended period for collection of
a Case of samples.
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Procedures for Problem Resolution
!• Resolving Problems Concerning Sample Shipment and Analysis
Program laboratories routinely notify SMO upon encountering problems
with sample receipt or during sample analysis. (Examples of these types of
problems are listed in Appendix C) In response, SMO immediately
contacts the RSCC to relay the problem and to assist in formulating a
solution. SMO then contacts the laboratory involved to communicate the
recommended action and to authorize processing of the sample(s) in
question. The key to this type of problem resolution is timeliness, since
delays impact sample holding times, contractual time requirements lor
sample extraction and analysis, and if extreme, could invalidate the
analyses.
General questions a user may have regarding sample shipment, sample
analyses, laboratory contracts, or the status of data deliverable; on a
particular Case or SAS should be referred to the appropriate SMO
personnel. Questions of a technical nature regarding contract analytical
procedures should be referred to the appropriate NPO official or to the
appropriate Regional Deputy Project Officer through the NPO. (Reference
Appendix A, CLP Directory.)
2. Resolving Problems Concerning Analytical Data
In the CLP* Regional/Laboratory Communication System, authorized
Regional personnel can contact specified laboratory personnel, after
laboratory data submission only, to resolve questions regarding the final
data package. This system may never be used to initiate additional
analytical work to resolve data questions. All communications between
laboratories and Regional contacts are recorded by each party on a
Telephone Record Log, indicating the number of the Case and/or SAS
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Sample shipments made after 5:00 PM EST should be called in to SMO at
the start of business the next day (8:00 AM EST). SMO must be notified by
3:00 PM EST Friday concerning information on sample shipments going out
Friday intended for Saturday delivery/pickup. CLP laboratories remain
open to receive or pick-up Saturday shipments only upon advance notifica-
tion by SMO and only when shipment airbill numbers have been provided to
SMO by the sampler.
The success of sample shipment coordination depends on the proper use and
handling of the sample tracking forms and on timely and complete
communication among the RSCC, samplers, SMO, and laboratories. Any
postponements or cancellations, changes in the number or type of samples
to be collected or shipping dates must be communicated to SMO as soon as
this information is known, to facilitate this process. Appendix C contains a
checklist for coordinating sample shipment.
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concerned, the individuals making contact, the subject of the discussion
and its resolution. In follow-up, copies of completed telephone logs are
sent to SMO by both the Regional and laboratory parties and become a
permanent part of the Case/$AS file. An example of the Telephone Record
Log is included in Appendix C. Copies are available from SMO.
Prior to the laboratory's submission of the final data package, client
queries regarding those analyses or data are handled through SMO.
Depending on the nature of the question, SMO will respond or will direct
the client to the appropriate NPO official for resolution. Comments
regarding laboratory performance, whether positive or negative, should be
directed in writing to the appropriate Regional DPO, with a copy provided
to the NPO.
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CHAPTER IV
AUXILIARY SUPPORT SERVICES
77
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CHAPTER IV
AUXILIARY SUPPORT SERVICES
to addition to its analytical programs, the CLP provides several supplementary
services. These activities have developed as a natural adjunct to the program's
analytical services. The purpose of this chapter is to provide the user with a
description of each auxiliary program service and how the service may be accessed.
A, Sample Bottle Repository Program
1. Types and Quantities of Bottles Available
Under the Sample Bottle Repository operation, nine types of sample
containers are available to CLP clients for use in hazardous waste sampling
activities of the Superfund Program. Bottles provided through this
program are precleaned and QC-tested according to prescribed procedures
to ensure that no contamination exists that might affect sample data
results.
Clean, empty bottles and closures are shipped to users in protective
cardboard cartons. (Sample coolers and sample preserving agents are not
supplied through the Repository program.)
The following chart lists the types of bottles provided through this
program, the case sizes in which bottles are shipped, and the type{s) of
samples appropriate for collection in each bottle type. Each bottle type is
cleaned and QC tested by procedures directly related to the specific
analyses that may be performed on samples collected in the bottle.
Therefore, to ensure appropriate quality control, users are instructed to
utilize bottles only to collect sample types as listed on the following chart.
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SAMPLE BOTTLE REPOSITORY SERVICES
Container
Type
Description
Used for RAS
Sample Type*
1 80 ounce amber glass bottle 6
with teflon-lined black
phenolic cap
2 40-ml glass vial 72
with teflon-backed silicon
septum cap
3 1 -liter high-density 42
polyethylene bottle
with poly cap
4 120-ml wide-mouth glass vial 72
with poly cap (white)
16-oz wide-mouth glass jar 48
with teflon-lined black
phenolic cap
8-oz wide-mouth glass jar 96
with teflon-lined black
phenolic cap
Extractable Organic*
Low Concentration
Water Samples
Volatile Organics
Low ft Medium Concentration
Water Samples
Metals, Cyanide
Low Concentration
Water Samples
Volatile Organics
Low & Medium Concentration
Soil Samples
Metals, Cyanide
Medium Concentration
Water Samples
Extr actable Organics
Low & Medium Concentration
Soil Samples
-and-
Metals, Cyanide
Low & Medium Concentration
Soil Samples
-and-
Dioxin
Soil Simples
-and-
Organics & Inorganics
High Concentration
Liquid & Solid Samples
*This column specifies the only type(s) of samples that should be collected in each
container.
(continued
79
Rev: 10/84
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SAMPLE BOTTLE REPOSITORY SERVICES (continued)
Container
Type
Description
Used lor
Sample Type*
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2. Ordering Procedures
The Sample Bottle Repository program may be used by any organization
scheduling samples through the CLP, and is commonly accessed by
Regional and remedial contractor clients. Two individuals from each
organization are designated by SMO as Repository Authorized Requestors
(RARs) and only these individuals may place bottle orders through the
program. State personnel should access the bottle program through their
EPA Regional office.
Users should contact SMO initially to become authorized to order from the
Repository and to obtain a supply of Delivery Order forms. Thereafter,
the RAR orders bottles directly from the Repository. Since the Repository
can respond only to orders submitted by a SMO-designated RAR, users
must notify SMO of any change in RAR designations.
There are three types ol bottle orders, defined by the amount of ti
between the date the order is placed and the requested delivery date:
o Routine Order
o Fast-Turnaround Order —
o Emergency Order
Ten or more working days lead time for
delivery.
More than three days, but less than ten
days lead time for delivery.
Less than three days lead time for
delivery.
Routine orders are mailed to the Repository utilizing the Delivery Order
(DO), a four-part carbonless form. The DO must be signed by an RAR.
The first two copies of the completed DO are sent to the Repository at the
address indicated on the form, the third copy is sent to SMO, and the
fourth copy is retained for the user's file.
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Fast-turnaround and emergency orders should be called in to the Reposi-
tory, at the telephone number provided on the form, and the written
Delivery Order distributed as outlined above, to confirm the order. When
placing a telephone order, the RAR must give the Repository the DO
number for the order and provide the corresponding written DO in
folio wup.
Users should submit orders a minimum of two weeks in advance of the
required delivery date, whenever possible, to ensure timely and complete
delivery of bottles. Emergency and fast-turnaround orders are filled on an
"as available" basis from the Repository* emergency inventory stock. It
may not be possible to respond to all emergency and fast-turnaround
orders, as response depends on Repository inventory and in-process orders.
In the event that an order is cancelled, the user must immediately contact
the Repository to verbally cancel the order, and follow up with a
cancellation memo to the Repository, sending a copy of the memo to SMO.
Cancellation memos, as well as all other project-related correspondence,
should cite the appropriate DO number.
3. Shipment Information
Upon receipt of the Delivery Order, Repository personnel schedule ship-
ment and begin preparing the order. Repository personnel immediately
notify the RAR if for any reason the order cannot be met in full by the
requested delivery date. Often, partial shipments can be arranged over
several days to meet the client's requirement. If concurrent orders are
received at the Repository that cannot be filled in a timely manner and if
partial shipments cannot be satisfactorily arranged, the Repository
immediately notifies SMO, which coordinates with the involved Regional
Sample Control Centers) in determining the priority of bottle orders based
on the Regions sampling needs.
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Each carton in a Repository shipment is marked "Box ___ of ," and a
Repository Packing List (PL) is included in Box I of each shipment, so that
the designee can verify that the entire shipment has been received. In
addition, the Repository sends two copies of the shipping PL to the RAR at
the time of shipment. The RAR confirms with the designee that the entire
shipment was received in good condition, then enters the date of receipt
and signs the packing list in the space indicated to confirm receipt. The
RAR must return a copy of the signed packing list to SMO within seven
days of shipment receipt.
Procedures for Problem Resolution
a. Resolving Problems Concerning Bottle Shipment
If there are problems relating to shipment (Le., shipment does not
arrive by scheduled date, shipment is incomplete or contents are
damaged), the shipment designee or RAR (as appropriate to the
situation) should contact the Repository immediately to resolve the
problem. If the problem is not satisfactorily handled in this manner,
the RAR should then contact SMO for resolution.
*
b. Resolving Problems Concerning Bottle Contamination
If a user has definitive cause to suspect that container contamination
may have affected sample analysis results, the concerned RSCC
should notify SMO by telephone and follow up with an explanatory
memorandum directed to the appropriate NPO Project Officer (PO).
The memorandum should include the following information:
description of the problem, rationale for suspecting bottle
contamination, supporting documentation (if available), and lot
numbers) for all bottles concerned. Bottle lot numbers must be
provided before any corrective action can be taken. Prior to
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requesting corrective action, the user should verify to the extent
possible that the contamination encountered is not a result of either
improper field procedures (e.g., use of contaminated water for field
blanks) or poor laboratory practice (e.g., background contamination)
and include this information as part of the rationale in the
memorandum submitted to the NPO.
After review of submitted information, the PO notifies SMO to
initiate appropriate follow-up action. Upon notification by SMO, the
Repository will first check the QC analysis record for the concerned
lot(s) of containers and verify that contract procedures were
correctly followed and that the lot passed the QC analysis. Should an
error be identified in this process, the Repository will notify SMO
immediately.
As a second step, following PO authorization the Repository will pull
the QC storage container for the bottle lot(s) and analyze the
containers) for suspected contaminants. SMO will notify the RSCC
concerning the analysis results, so that if there is a contamination
problem, analysis data from samples collected in other containers in
that lot can be appropriately flagged. Should contamination be
confirmed by analysis of the QC storage container, the Repository
will immediately identify the problem and correct procedures as
necessary to resolve it. Should a wide-spread problem be identified
at any time, RARs would be notified in a timely manner so that
bottles could be pulled before use in the field.
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3. Summary of Bottle Cleaning and Quality Control Procedures
Containers provided under this program are prepared in batches or lots of
approximately 100 containers. (Exact lot sizes for each bottle type are
determined, so that a bottle lot is not split between cases.) Bottles are
cleaned in lot groups, utilizing procedures specifically designed to remove
any possible contaminants. Different cleaning procedures are employed
according to the container material and the type(s) of samples that will be
collected in the container.
Each bottle lot is assigned a unique identifying number. This lot number is
permanently affixed to each bottle in the lot, recorded in the Repository
logbook, and entered on the shipment Packing List when bottles from that
lot are shipped. For QA purposes, it is vital that each container's lot
number be permanently associated with the sample collected in that
particular container. Therefore, it is recommended that samplers record
each container lot number and associated CLP sample numbers in their
field records at the time that samples are collected.
The Repository routinely performs QC analyses on one percent of the
number of containers per lot. No lot is released for shipment until
acceptable QC results are verified. QC analyses are performed by
equivalent methods to those utilized in CLP RAS programs, and are
specific to the types of samples that may be collected in the container. U
a container fails to pass the QC check, the associated lot of bottles is
pulled and reprocessed through the system.
A QC release number is assigned to each lot of bottles that passes QC
analysis, and is marked on both the analysis and storage QC containers for
each tot. The QC release number is cross-referenced with the lot number
in Repository records, so that all QC records can be accessed based on the
lot number identification.
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In addition to the QC analysis check, an additional bottle is removed from
each lot and stored for QC purposes. QC storage containers are kept in a
contaminant-free area of the Repository which is monitored for volatile
compounds. The QC storage containers are retained as a backup to
recheck for cleanliness, should possible contamination of a tot of bottles
come into questions at a later date.
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Information Services
1. Regional Sample List Report
On a monthly basis, SMO distributes a Regional Sample List Report to each
Regional Sample Control Center (RSCC). This computerized report
provides a summary of the Regions use of CLP resources during the
previous month. The following information is included in the Sample List
Report:
o Case number
o Sample number
o Laboratory name and contract number
o Laboratory sample receipt date
o Sample weight and components analyzed
o Sample type
o Data due date
o Days late/early calculations for contractually required deliverabies
(i.e., extraction, VOA analysis and sample data package).
This report is provided to the Region for use as a management and resource
planning tool, as well as for verification of monthly sample receipts and
analyses performed. While client activity is reported on a monthly basis,
information covering other time periods can be provided upon RSCC
request to SMO. An example of the Regional Sample Ust is contained in
Appendix D.
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2. Sample Status Information
In its sample management role, SMO schedules sample analysis and tracks
samples from shipment through data reporting, maintaining manual and
computerized tracking systems. SMO maintains ongoing communication
with the RSCC regarding sample status, and responds to inquiries from
concerned parties as appropriate.
3. General Program ^formation
Under the direction of CLP management, SMO serves as the program's
information center for both incoming calls, correspondence and dissemina-
tion of information. Upon request, SMO provides program participants and
interested parties with information and material on program services and
procedures, and refers callers to the proper sources for additional
information as appropriate.
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C. Enforcement Support
1. Generation of Enforcement Quality Data
One major objective of Super fund is to recover from responsible parties
costs incurred in the investigation and cleanup of hazardous waste sites.
The process by which these parties are identified and determined to be
responsible often involves litigation, and frequently the Agency's case is
based upon CLP analytical data generated from samples collected at a
given site. The CLP supports these and other enforcement requirements of
Superfund by ensuring that CLP-generated analytical data is admissable
and defensible in court. The CLP, in cooperation with the EPA National
Enforcement frwestigations Center (NEIC), has established detailed
procedures and documentation to ensure that CLP sample data meets
Agency enforcement standards.
a. Chain-of-Custody and Document Control
Each CLP analysis contract requires the laboratory contractor to
implement a comprehensive document control system and to employ
strict chain-of-custody procedures in the receipt and handling of
samples throughout the analysis and data reporting process. The
laboratory must have written Standard Operating Procedures (SOPs)
for: receipt and log-in of samples, maintenance of sample security
after log-in, tracking the sample through all steps of preparation and
analysis, and organization and assembly of all sample-related
documentation on a Case-specific basis. Required document control
and chain-of -custody records include, at a minimum} sample tags,
custody records, sample tracking records, analyst logbook pages,
bench sheets, chromatographic charts, computer printouts, raw data
summaries, instrument logbook pages, correspondence and the
document inventory.
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Before a laboratory is awarded a CLP contract and continuing
periodically throughout the life of the contract, each laboratory
facility is audited by NE1C to ensure compliance with these require-
ments, it addition to facility audits, laboratory data and evidence
documentation are reviewed by NEIC on a regular basis, as described
below.
b. NEIC Evidence Audits
Laboratories are contractually required to purge their files of all
evidence and other documentation relating to sample analysis, and to
submit a complete Case file purge package (as detailed in the
previous section) to NEIC six months after submission of analysis
data. The Contractor Evidence Audit Team (CEAT) reviews all
document control packages to verify that the documentation is
complete and conforms to contractual requirements, and routinely
audits a selected number of packages for document accuracy and
suitability for enforcement uses. A list of Case file purge materials
is included in Appendix D.
NEIC evidence audits involve production of sample profiles. A
sample profile traces the path and handling of specific samples from
the point of collection through shipping, laboratory receipt, chemical
analysis and data reporting. This process identifies any gaps or lapses
in the chain-of-custody so that measures may be taken before
enforcement case preparation either to correct the problem or
eliminate the data from consideration in enforcement action.
Examples of NEIC sample profiles for organic and inorganic Cases are
incuded in Appendix D.
Following review and/or audit, NEIC returns laboratory Case file
purge packages to the originating Region, where the packages are
filed with the analysis data and may be subject to additional Regional
review. In addition to the routine generation of sample profiles in
evidence audits, authorized Regional personnel and enforcement
attorneys may request NEIC to prepare sample profiles for Cases to
support enforcement activities.
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2. Additional CLP Enforcement Support
Enforcement activities frequently require direct CLP support. Court
appearances and other mandated deadlines often do not allow sufficient
time for completion of the normal Case file purge package submission,
review and audit process, h this event, CLP assistance may be required.
Also, data package evaluation and/or testimony from laboratory or CLP
personnel may be needed.
The CLP has established procedures to meet these short-term requirements
through SMO, which coordinates and responds to enforcement-related
requests. This process is described in the following sections.
a. Request Procedures
Requests are originated by a Regional counsel, NEIC or other
appropriately designated EPA personnel, and are submitted in a
memorandum to the NPO Program Manager (PM). The PM reviews
the memorandum, determines necessary CLP action and forwards the
request along with his directions for action to SMO. If a request
requires immediate response, the requestor should contact SMO
directly by telephone and relay the request, following up with the
written request memorandum to the PM.
b. Requestor Information Required
The following information must be provided by the requestor to
initiate CLP action:
o Name and telephone number of Regional contact coordinating the
enforcement activity
o Case numbeKs) of specific site sampling(s)
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o Sample numbeKs)
o Date(s) of sample collection
o Laboratory(ies) that performed the analysis
o Type of support needed
Most requests can be met quickly, however a two-week lead time is
strongly recommended.
c. Documentaton/Support Provided by CLP
In responding to enforcement support requests, SMO provides the
following support:
o Arranges for the timely delivery of all laboratory and evidence
documentation relating to specific sample analyses (within a
minimum of seven days of request, if designated).
o Obtains information relating to sample analysis or handling not
specifically required under laboratory contracts.
o Arranges for expert testimony by laboratory or CLP personnel.
o Augments Regional resources for analytical data review.
o Supplies replacement copies of analytical data.
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D. Cost Recovery Substantiation
The CLP provides documentation concerning program analytical costs to the
EPA1* Office of Waste Programs Enforcement (OWPE) in support of Super fund
cost recovery efforts. Formal procedures have been developed to respond to
Agency requests for this information. Site-specific cost data, the information
required to initiate this process, and cost documentation provided by CLP are
described in the following sections.
1. Request Procedures
Requests for cost recovery (CR) documentation on a site must be made
through OWPE, using the Cost Recovery Checklist. This checklist is
designed to provide basic site information needed to compile cost
documentation from the CLP and other sources. A copy of the OWPE Cost
Recovery Checklist is included in Appendix D. Each requesting office must
complete the CR Checklist, providing all information requested, and mail
the completed checklist to OWPE.
In response to requests, OWPE collects and organizes cost-related
documentation from the CLP and several other sources, such as the EPA
Financial Management Division, the EPA Office of Emergency and
Remedial Response, and REM/FIT, TAT and other Agency contractors. In
case of conflicts, OWPE is responsible for prioritizing incoming requests.
A minimum lead time of four to six weeks is required to complete this
process and provide the requestor with a full site cost recovery report.
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2. Requestor Information Required
Requestors are asked to supply the following information items on the CR
Checklist to enable the CLP to prepare its cost documentation package.
(Complete checklist information is required to obtain a full OWPE cost
report, which contains information from other sources in addition to the
CLP.)
o Identification number
The appropriate CLP Case or SAS number must be entered here. If the
Case or SAS number refers to more than one site, the specific sample
numbers (from the Case Traffic Reports or SAS Packing List) related to
the sites in question must be provided.
o Name and location of site
o Date the cost report is needed
A minimum of four weeks from the date of request must be given. Six week
lead time is recommended whenever possible.
3. Documentation Provided by CLP
The CLP provides an information package to OWPE which is part of
OWPES full cost recovery report to the requestor. The CLP provides the
following information to OWPE:
o Financial Summary for Cost Analysis
This summary lists analytical and sample management costs on a Case
and/or SAS basis, showing total expenses for a particular site. Informa-
tion on how sample management costs are computed is included.
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o Summary of Invoices, Vouchers, and Cancelled Checks
This report lists all SAS laboratory invoice numbers and includes SAS
cancelled check numbers. The summary is organized by SAS number
and laboratory name.
o Routine Analytical Services (RAS) Cost Report
This computerized report is organized by Case number and laboratory
contract. It includes laboratory invoice numbers, net analysis costs,
total of adjustments for late/early deliverables, and sample
management costs; and lists total costs on a sample-by-sample,
laboratory contract, and Case basis.
o Special Analytical Services (SAS) Cost Report
This computerized report provides a brief description of the service
provided, including the number of samples analyzed, data turnaround
time, contract start date, laboratory receipt date, unit costs, sample
management costs, and contract status; and lists total contract costs on
SAS and laboratory bases.
o Copies of art SAS-Related Cancelled Checks and Laboratory tivoices
CLP documentation, as described above, is assembled by SMO and
submitted to OWPE. OWPE provides this CLP information, along with
documentation gathered from other sources, to the Regional case
development team in the full cost recovery package.
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Data Review Services
In its program support role, SMO has developed systems of quality assurance and
quality control evaluation, working under the guidance of EPA personnel most
directly concerned with hazardous waste site data quality assessment. These
systems can be applied to CLP data generated from IFB laboratory analysis
contracts, upon client request.
The objectives of the data review program are:
o To provide systematic and standardized data quality assessment at the
Case, sample and sample fraction levels.
o To increase the amount of useable data by resolving or proposing solutions
to analytical or quality control problems.
o To determine the useabifity and limitations of the data given particular
field or policy assessment questions.
The purpose of the CLP* data review service program is to assist, supplement
and/or extend Regional capabilities in evaluating the quality and applicability of
data for intended uses. The program's application of standardized data
evaluation techniques and procedures to given Cases and samples of interest
ensures the Regional client a degree of confidence when using the data for
enforcement or remedial action planning. Several different types of data review
may be conducted depending upon Regional needs and service availability.
1- Types of Review Provided
Four basic types of data review are provided in this program. One or more
types of review may be requested for a given Case, and review may be
requested for more than one Case. As indicated, these data review
services are intended to supplement or extend, but not to replace, Regional
data review.
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The four types of data review currently provided through this program are
summarized below:
o QA/QC Compliance Review
A technical and administrative review of each Case, sample, and
sample fraction for compliance with contractually-required ranges on
measures of precision and accuracy.
o Problem Case Review
A technical evaluation of a Case which has failed a Regional or SMO
QA/QC Compliance Review in order to resolve or propose solutions to
analytical or quality assurance problems.
o Applications Review
A technical evaluation of the validity and limitations of the data given
particukr field or policy assessment questions requiring actual
measures of precision and accuracy.
o Consulting Review
A technical second opinion of the data from a previous review. Serves
an appeal function in determining data useability.
Each type of review is further characterized below.
In the QA/QC Compliance Review, the following areas are examined: data
completeness, spectra matching quality, surrogate spike results, matrix
spike results, duplicate sample analysis results, blank analysis results,
instrument tuning and performance results, chromatography checks, and
calibration results. Criteria from each area of performance are applied in
the evaluation of each fraction. Acceptability or unacceplability is
determined separately for volatiles, semi-volatiles, pesticides and dioxins,
using contract ranges as guidance.
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The purpose of the Problem Case Review is to increase the amount of
useable data by resolving or proposing solutions to analytical or quality
assurance problems. Data which have failed the QA/QC Compliance
Review may be adequate for the intended purpose, even when laboratory
problems cannot be resolved.
The Applications Review attempts to determine the actual quality of the
data and relate this assessment to particular field or policy assessment
questions. The confidence limits set by compliance to the contractually-
determined basic data quality measures are further examined. Additional
statistical measures are calculated and reported, and the new confidence
levels are related to the Regional client's intended use (e.g., enforcement,
site screening, remedial design, site monitoring).
The Consulting Review allows the user to obtain a second opinion of the
data quality in problematic situations where the assessment of data quality
is either complex, critical or very dependent upon field conditions.
2. Request Procedures
Requests for Data Review Services should be directed to the Regional
Deputy Project Officer (DPO), with a copy submitted to SMO,
Attention: Data Review Team, and a copy provided to the Regional
Sample Control Center. In follow-up, the DPO must notify SMO that the
request is authorized, or the DPO may choose to initiate all requests for
the Region.
Upon authorization by the DPO, SMO schedules the review and notifies the
requestor of the date the review is scheduled for completion. It should be
noted that review cannot be initiated until all deliverables for the subject
Case(s) have been received from the laboratory.
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All requests should be placed using the SMO Data Review Request
memorandum. An example of the request memorandum is provided in
Appendix O. Copies are available from SMO on request.
3. Requestor Information Required
In completing the Data Review Request form, the client must provide the
following information for each Case for which review is requested:
o SMO Case number
o Site name
o Analytical laboratory name(s)
o Number of samples
o Sample list
o Type(s) of review requested
o Requested date for review completion
o User name and contact
o Intended use of data
A minimum lead time of two weeks is required for data review. However,
review time is variable depending upon the number of samples involved and
the nature of the review. If conflicts occur, the appropriate DPO(s) will be
notified and asked to prioritize requests.
. Documentation Provided by CLP
An evaluation report, including supporting statistics and documentation, is
produced with each type of review.
The QA/QC Compliance Review report indicates for each sample fraction
whether the data are considered: acceptable, acceptable given
qualifications noted, or unacceptable. Reasons for the designation are
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discussed and completed data review forms for each of the areas of
performance are included in the report to the client. Examples of data
review forms used in the QA/QC Compliance Report are included in
Appendix EX
The contents and format of reports for Problem Case, Applications and
Consulting Reviews are determined by the nature of the data probiem(s)
being examined and/or the purpose for which the data will be used. Any
statistical measures used to define data quality and the raw data
supporting conclusions are appended to these reports.
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CHAPTER V
PROGRAM QUALITY ASSURANCE
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CHAPTER V
PROGRAM QUALITY ASSURANCE
The purpose of this chapter is to present a summary oi the different aspects of quality
assurance (QA) and to show their interrelationship within the overall structure of the
program. This information is included to familiarize users with the program's basic
QA principles and their application, and to facilitate a more complete understanding
of the quality of CLP analytical data in terms of potential utilization.
A. Interface with Agency Quality Assurance
The primary role of the CLP is to support the Agency's Superfund investigation
and cleanup efforts by producing analytical data of known and documented
quality useable for Agency enforcement actions keyed to identification of
pollutant sources and recovery of cleanup costs. Therefore, a comprehensive
quality assurance program that reflects Agency QA objectives has been
incorporated into all aspects of CLP operations. The CLP links two primary
aspects of quality assurance (QA): field QA, which includes field sampling
operations and QA project planning; and laboratory QA, which is comprised of
analytical method QC and external or program QA.
Field operations include sampling activities performed by the EPA Regions and
National Remedial Action/Field Investigation Team (REM/F1T) and Technical
Assistance Team (TAT) contractors, which result in samples being processed
through the CLP for analysis. The CLP NPO coordinates closely with these and
other Agency sampling groups and Agency QA teams, in the development and
application of quality-controlled Program Plans and site-specific Project Plans.
These plans include the consistent use of Agency-specif led containers, sampling
techniques, sample preservation, sample tags and chain of-custody documents,
and adherence to DOT regulations in sample shipment. The CLP strongly
supports the use of consistent field sampling, and sample packaging and shipment
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techniques, and specifies types of sample containers and required sample
volumes for appropriate target analyses. Through its Sample Bottle Repository
system, the CLP provides Super fund samplers with the prec leaned sampling
bottles for use in the field.
The CLP is directly involved in all aspects of laboratory QA, Analytical methods
require extensive Agency-specified quality control (QC) procedures and
documentation to ensure a complete data product that will withstand legal
scrutiny. The CLP operates an extensive external QA program, which includes:
pre-award and post-award laboratory performance evaluation sample analyses
and laboratory facility evaluations, required submission of laboratory Standard
Operating Procedures (SOPs) for analytical operations and documentation,
continuous monitoring of lab performance by Headquarters contract POs and
Regional DPOs, and a multi-level data review process to evaluate the validity of
the data product*
The CLP, through a variety of mechanisms, continuously strives to improve the
quality of program data by maintaining state-of-the-art analytical methods,
refining the structure and requirements of analytical contracts, and strengthen-
ing lab operations. CLP QA activities are coordinated through the NPO QA
Officer, to ensure that the CLP is operating in accordance with overall Agency
QA mandates.
The application of field QA is addressed in Chapters II and III, where sample
volume, container, preservation, packaging, shipment and documentation
requirements are discussed. Analysis or method QC is addressed for each
analytical program in Chapter II, which contains a description of contract
analytical methods and QC requirements for each program. The following
sections of this chapter describe the program^ external laboratory QA activities.
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B. Laboratory Selection Process
1. Bid Price
The first criterion for laboratory selection is bid price. Following bid
opening, bid abstracts are reviewed and evaluated by NPO and EPA
contract officials. The lowest competitive bidders are selected to
participate in pre-award bid confirmation, the process through which
bidder responsiveness and responsibility for award are demonstrated and
evaluated.
2. Pre-Award Bid Confirmation
Pre-award bid confirmation may include three activities: (1) bidder
analysis of performance evaluation (PE) samples; (2) bidder submission of
Standard Operating Procedures (SOPs); and (3) site evaluation of the
bidder's facility, performed by EPA program management and contracts
personnel.
a. Performance Evaluation Sample Analysis
Laboratories chosen to participate in the pre-award process are sent
a set of PE samples for analysis. The PE samples are prepared by
EM5L/LV and are representative of the types of field samples that
the contractor would routinely be analyzing under the subject
procurement. The laboratory is required to analyze PE samples
according to contract procedures set forth in the IFB, and to report
PE sample data according to IFB requirements, within a time period
of 21 days. Bidders' PE sample data are evaluated by NPO and
EMSL/LV personnel, in terms of compliance with contract require-
ments and accuracy of determination of compounds at the levels
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known to be in the PE samples. Analysis results are rated by a
scoresheet developed by EMSL/LV. The PE sample score is a primary
consideration in determining bidder responsiveness/responsibility for
contract award.
b. Standard Operating Procedures
Bidders are required to submit copies of all laboratory Standard
Operating Procedures (SOPs) at the time of submission of PE sample
data. SOPs are not required to coincide with each specific detail of
the contract requirement, but must be representative of good
laboratory practices and must demonstrate that the laboratory has a
facility-wide quality assurance program in place and operating.
Bidder SOPs are reviewed by NPO and EMSL/LV personnel and are
utilized by EPA in performance of the site evaluation.
c. Laboratory Evaluation
EPA NPO and EMSL/LV personnel participate in site evaluations of
laboratory facilities of bidders which scored acceptably on the PE
sample analyses. EPA personnel perform a walk-through of the
facility and complete a site evaluation questionnaire. The results of
the site evaluation are considered in final determination of bidder
responsiveness/responsibility for contract award.
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C. Laboratory Start-Ut> Process
Laboratories entering the program undergo a learning curve process during which
they become fulty familiarized and obtain expertise in application of program
methodologies and quality control procedures. To reduce the teaming curve
period and bring laboratories "up to speed" in a timely manner, CLP management
employs a series of laboratory start-up procedures which are utilized during the
laboratory's initial contract operations and whenever laboratory problems are
identified during contract performance.
1. Provision of Standards to Laboratory
Immediately following contract award, EMSL/LV arranges for the provision
of standard materials (SMs) to the contractor, through the Agency's
contractor-operated QA Materials Bank. These SMs are utilized by the
laboratory in performing initial instrument calibrations and as reference
standards throughout contract performance.
2. PO Review of First Data Packages
Initial data packages are targeted for immediate review and evaluation by
the NPO Project Officer (PO), EMSL/LV and the Region. This review is
intensive and focuses on any problems the laboratory has, either in applying
methodologies or in reporting the data. The PO then supplies feedback to
the laboratory concerning the status of the data and works with the
laboratory in identifying and remedying problems.
3. PO/DPO Laboratory Visits
Depending on the extent of the problems found during the review of an
initial data package, the PO may visit the laboratory facility and work on-
site with laboratory personnel in rectifying problems. This process also
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occurs on an ongoing basis during the life of the contract. Site evaluations
are performed yearly by EPA staff, and the PO and/or Deputy Project
Officer (OPO) visit the laboratory on an as-needed basis to resolve
performance problems.
*. Pp/DPO/SMO/Laboratory Communication
Telephone communication is the most widely applied method for problem
solving and maintaining efficient laboratory operations, both during the
laboratory start-up phase and throughout the performance of the contract.
During the start-up period, communication links are established and the
laboratory becomes familiarized with the communication process. In
general, the laboratory notifies 5MO immediately upon identification of
any problem regarding the samples (e.g., insufficient sample volume) or any
difficulties encountered in analysis. SMO routinely resolves sample-related
problems in coordination with the Regional client, and refers technical
problems to the contract PO, who contacts the laboratory and resolves the
problem. The resolution and any specific actions taken are reported to
SMO which records this information as part of the permanent Case record.
The laboratory also records the problem and resolution on the sample data
report, so that the Region considers this information in association with
evaluating and using the data. With the appointment of Regional DPOs to
assist in the monitoring of contractor performance, the DPO will play a
major role in ongoing laboratory problem resolution in coordination with
the PO.
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D. Laboratory Performance Evaluation
l« Performance Evaluation Sample Analysis
Performance Evaluation (PE) samples are prepared by ORD EMSL/LV and
sent to contractor laboratories for analysis, normally on a quarterly basis.
PE samples are typically shipped as Double blind" samples, ue., the PE
samples are not discernable from routine field samples, to ensure that the
laboratory processes the samples in a routine manner. Evalution of PE
sample data is performed by EMSL/LV and is used by the NPO in formally
evaluating laboratory contract performance. Additionally, PE sample QC
data are entered by EMSL/LV into the program's QA Data Base, and are
utilized, along with other laboratory data, in trend analyses, and evaluation
and revision of contract QC criteria.
2. Laboratory Site Evaluation
At least once a year, EPA NPO, Regional and EMSL/LV personnel visit
each laboratory facility and evaluate laboratory procedures. The evalua-
tion reports which result from these site visits are utilized by the NPO in
identifying and remedying laboratory performance problems. Repeat site
visits by EPA NPO, Regional and EMSL/LV personnel are made on an as-
needed basis throughout the year, to resolve laboratory problems.
3. Corrective Action
Upon identification of laboratory performance problems, the PO and DPO
work closely with the laboratory to effect correction of the problems.
Depending on the scope of the problems, the laboratory may be placed on
temporary hold, whereby the laboratory does not receive additional
samples for analysis until the problem has been corrected.
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Should the contractor's non-compliance to contract performance or
deliverable requirements continue, the EPA Contracting Officer is
requested by the NPO to issue a Show Cause Notice to the contractor.
This document requires the contractor, within a ten-day period of time, to
present the government with any facts bearing on the issue, to be used in
the government's determination regarding whether the contractor's failure
to perform arose out of causes beyond the laboratory's control and without
fault or negligence on the part of the contractor, the contractor, in
response, must submit substantial evidence to demonstrate that the
contract should not be terminated for default
A recovery plan is generally included as part of the contractor's response
to the Show Cause Notice. EPA Contracts and NPO officials review the
contractor's response and proposed recovery plan, and determine whether
the contractor has presented sufficient evidence to demonstrate timely
remedy of the noncompliance. Following this review, if the contractor has
presented acceptable evidence toward recovery, the government issues a
Cure Notice to the contractor which delineates the government-accepted
recovery plan that the contractor must follow to avoid contract termina-
tion. The government's recovery plan includes actions and time schedules
for completion of each step of the recovery process, and specifies an
overall time period acceptable for completion of recovery.
Should the contractor not comply with the recovery schedule, the next and
final step may be contract termination by the government for default. In
addition to terminating the laboratory's contract, this action impacts on
evaluation of the contractors responsiveness/responsibility for award under
future CLP solicitations.
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Sample Data Evaluation
!• frtercomparison Check Sample Studies
tttercomparison check sample studies are initiated by the EPA Regions on
a periodic basis and involve simultaneous shipment of known samples to
two or more CLP and/or Regional laboratories for analysis. Check samples
are routinely shipped as "single blind" sample, Le., the laboratory is aware
samples are check samples but does not know sample composition.
Analytical data from study participants are compiled by the Region and
used in comparative data evaluation. The Region provides intercomparison
sample study results to the NPO and EMSL/LV for use in programmatic
applications. These studies differ from the PE sample program in that
check sample data do not result in contractual evaluation of individual
laboratory performance.
2. Regional Sample Split/Spike Programs
This Regionally ^directed program involves simultaneous sample analysis by
two or more CLP and/or Regional laboratory facilities, and provides the
Region with comparative data utilized in evaluating application of
methods. In the sample split program, the Regions arrange to have field
samples split and sent to different contractor and Regional laboratories for
analysis. In the sample spike program, a known sample volume is prepared
and divided into two or more equivalent portions. Each sample portion is
then spiked with known levels of contaminants, and sent to different
contractor and/or Regional laboratories for analysis. Results of split/spike
sample analyses performed by CLP laboratories are provided to the NPO
and EMSL/LV by the Region.
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F. Analytical Data Review
Upon completion of analysis and data reporting, the laboratory simultaneously
sends a copy oi the complete data package to the CLP SMO, EMSL/LV and the
Regional client. Each oi these groups performs complementary aspects of data
review.
1. EMSL/LV Data Review
On a routine basis, EMSL/LV performs a comprehensive QA audit on CLP
sample data packages using MiL Standard 105D. Based on this review,
EMSL/LV prepares a detailed report on the data packages, which is
provided to the NPO and to Regional clients by SMO. This review package
is valuable to both program management and users in evaluating the
suitability of the contract methods to the types of samples analyzed, the
quality of the analytical data, and the performance of the contractor
laboratories.
In addition, EMSL/LV enters surrogate and spike recovery information into
the program* QA Data Base. These data are then statistically evaluated
and utilized to determine and revise contract QC acceptance windows ior
CLP-generated data and to characterize laboratory performance.
2. Regional Data Review
The Regional client reviews ail data packages resulting from Regional
sampling efforts. It is the responsibility of the Region, as the data user, to
determine the applicability of each data package to its intended use, e.g.,
site investigation support, cleanup activities and/or enforcement actions.
In this review, the Region applies its standard CLP data review procedures
and references the requirements of the contract Statement of Work under
which the analyses were performed.
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SMO Data Check for Completeness
Each CLP-generated data package is checked for completeness by SMO
upon receipt. SMO reviews the data package verifying that ail
contractually-required forms are included and that forms are completed
according to contract specifications. Should SMO identify any missing
information, incomplete forms or other problems with the data package,
SMO immediately notifies the NPO PO, EMSL/LV and the Regional client.
At this time, the laboratory is contacted and instructed to submit the
missing or incorrect portions of the data package.
SMO Data Review Services
Under direction of CLP management, SMO may perform additional data
review, checking the data for compliance to contract QC procedures and
parameters and for applicability to its intended uses, this review is
provided on a limited basis in response to specific Regional request.
Consult Chapter IV, Section E, for a complete description of the data
review services provided and appropriate request procedures.
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C. Analytical Methodology Improvement/Development
1. Protocol Standardization and Improvement
Refining and improving analytical protocols to maintain state-of-the-art
status and to reflect newly-de fined or changed requirements of the
Super fund effort, is an ongoing activity for all CLP participants. This
effort is accomplished through an established system of information
transfer coordinated through the NPO. All program participants submit
comments or recommendations to the NPO on an ongoing basis. The NPO
reviews all submitted information and considers recommendations for
program application, on a periodic basis.
Since 1982, input on protocol improvements has come primarily through the
CLP Technical Caucuses which involve NPO, EMSL/LV, EMSL/Cincinnati,
EPA Region, SMO, laboratory and other program support contractor
personneL Analytical methods and data reporting formats are reviewed
and discussed in detail at the caucus sessions. EPA personnel then review
caucus discussions and compile concensus recommendations for protocol
changes. Following NPO approval of recommended changes, laboratory
contracts are modified by the Contracting Officer to include recommended
revisions, through contract change order actions. Ail laboratory contracts
within an analytical .program are changed concurrently to maintain
consistency across the program.
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2. Method Development
Development of new analytical methods may be initiated by a newly
identified or redefined Agency analysis requirement, such as dioxin
analysis. Analytical methods utilized in the CLP are based on EPA-
devetoped and approved methodologies. The NPO, EMSL/LV, EMSL/Cin-
cinnati, and/or EPA Regions have historically contributed to development
of new program analytical methodologies. Regardless of the group
responsible for method development, methods are reviewed by several
sources and are tested prior to implementation, to the extent possible to
meet program requirements.
11*
-------
-------
APPENDICES TO
CLP USER'S GUIDE
-------
-------
APPENDIX A
CLP DIRECTORY
A-l
-------
-------
EPA HEADQUARTERS AND NATIONAL LABORATORIES
CLP National Program Of lice (NPO)
USEPA Office of Emergency and Remedial Response
Hazardous Response Support Division (Mail Code: WH-508A)
Support Services Branch
tO I M Street, S.W. (Mall - Room 5213)
Washington, DC 20460
Stanley Kovell, National Program Manager
Mary Mahsetky, NPO Secretary
202/382-7906 FTS 382-7906
Duane Geuder, QA Officer
202/382-7903 FTS 382-79*3
Fred Haeberer, Organic Technical Officer
202/382-79*2 FTS 382-7902
3oan Fisk, Organic Technical Officer
202/382-3115 FTS 382-3115
Gary Ward, Inorganic Technical Officer
202/382-0619 FTS 382-4619
USEPA Office of Administration
Procurement and Contracts Management Division
(Mail Code: PM-210)
001 M Street, S.W.
Washington, DC 20060
Street Address:
099 South Capitol Street
Fairchild Building, 3rd Floor
Washington, DC
Marian Bernd
Contracting Officer
202/382-3195 FTS 382-3195
Dave Stutz
Contract Specialist
202/382-2357 FTS 382-2357
A-2
-------
EPA Headquarters and National Laboratories (cont)
USEPA Office of Research and Development
Environmental Monitoring Systems Laboratory (EMSL/LV)
P. a Box 15027
Us Vegas, Nevada 89114
Street Address:
944 East Harmon Avenue
Las Vegas, Nevada 89109
Ross Robeson, Acting Director
QA Division
702/798-2103 FTS 5*5-2103
Gareth Pearson, Chief
Toxics
-------
REGIONAL DEPUTY PROJECT OFFICERS
Region I
Region II
Region III
Region IV
Region V
Region VI
Region VII
Region VIII
Region IX
Region X
Edward Taylor
617/861-6700 FTS 828-6700
William Coakley
201/321-6702 FTS 3*0-6702
Patricia Krantz
301/224-2740 FTS 922-3752
Tom Bennett, Jr.
404/546-3112 FTS 250-3112
Charles Elly
312/353-8370 FTS 353-8370
William Langley
713/954-1766 FTS 526-1766
Robert Kleopfer
913/236-3881 FTS 926-3881
John Tilstra
303/234-3263 FTS 234-3263
Harold Takenaka
415/974-7*84 FTS 454-7484
Arnold Gahler
206/442-0370 FTS 399-0370
A-4
-------
REGIONAL SAMPLE CONTROL CENTERS
Authorized Requestor*
Edward Fitzpatrick, ESD Director
FTS 828-6700
Thomas Spittler, Chief
Technical Support Branch
FTS 828-6700
•Edward Taylor, CLP DPO
FTS 828-6700
Region 11
•Richard Spear, Chief
Surveillance It Monitoring Branch
FTS 3*0-6685
Doug Stout
FTS 3*0-6717
Carol Price
FTS 3*0-671«
Region HI
•Daniel Donnelly, Laboratory Chemist
Annapolis Field Office
FTS 922-3752
Ramona Trovato, Chemist
FTS 922-3752
John Austin, Chemist
FTS 922-3752
Region IV
•Tom Bennett, Chief
Chemistry Section
FTS 250-3112
Myron Stephenson
Chemistry Section
FTS 250.3165
Bobby Carol, Chief
Analytical Support Branch
FTS 250-3111
• Primary Authorized Requestor
A-5
-------
RSCC*(conO
Region V
Curtis Ross, CRL Director
FT5 353-8370
•Charles Elly, CLP DPO
FTS 353-8370
(RAS only)
EJcE:
Kathy Getty
Cindy Bacunas
312/663-9*15
CH2M Hill:
3erry Bills
Lin Klann
414/272-2426
Roy F. Weston:
Kurt Stimpson
Geoff Watkms
Tom DeFouw
312/V98-9090
Region VI
•Keith BradJey
FTS 729-9770
Minnie Rojo
FTS 727-9990
Dave Peters, Chief
Hazardous Waste Section
FTS 729-9783
-------
RSCCsCcont.)
Region VII
•Charles HensJey, Chief
Laboratory Branch
FTS 926-3831
Joyce Woods
FTS 926-3881
Bob Kleopfer, CLP OPO
FTS 926-3881
Region VIII
•Keith Schwab, Assc. ESO Director
FTS 327-0935
Tom Staible
FTS 234-3678
Region IX
•Harold Takenaka, CLP DPO
FTS «5«-748»
Laura Tom
FTS 45*-8379
Frank Day
FTS 054-8200
Region X
•Gary O'Neal, ESD Director
FTS 399-1295
John Osborn, Regional PO
FTS 399-0837
Joyce Crosson
FTS 399-4562
* Primary Authorized Requestor
A-7
-------
SAMPLE MANAGEMENT OFFICE
CLP Sample Management Office (SMO)
P. a Box 818
Alexandria, Virginia 22313
Street Address:
300 N. Lee Street
Alexandria, Virginia 22314
703/557-2*90 FTS 557-2*90
David Stewart,
Project Manager
Dick Thacker,
Deputy Project Manager
Tina DeYoung, Croup Leader
Management Information Systems, Invoice Processing
and Cost Recovery
Linda Haas, Croup Leader
Analytical Services
Leslie Braun, RAS Sampling Controller
EPA Regions I - IV, Zones 1 and 2
Eileen O'Connor, RAS Sampling Controller
EPA Regions V - X
Maka Grogard, SAS Sampling Controller
Dioxin and EPA Region V
Roch Mongeon, SAS Sampling Controller
EPA Regions I - IV, Zone 1
Paula Ausserer, SAS Sampling Controller
EPA Regions VI - X, Zone 2
Deborah Miller, Croup Leader, Special Projects
1FB Development, User's Guide and Communication System
Steve Manzo, Special Projects Coordinator
Bottle Repository Services and Meeting Planning
Rob Pritchard, Head
Enforcement Support
Don Trees, Head
Data Review and QA Support -:
Paul Friedman,
QA Chemist
Bill Eckel,
QA Support
A-8
-------
-------
APPENDIX D
RAS DEUVERABLES AND DATA REPORTING FORMS
B-l
-------
-------
RAS ORGANIC
DELIVERABLES INDEX
I. Case Narrative
The Case narrative must contain: Case number, Contract number,
of any QC, sample, shipment and analytical problems, and documentation of all
imternal decision tree processes used. Outline problems encountered and final
solutions. Be as specific and detailed as necessary.
__ QC Summary
A. Surrogate Percent Recovery Summary (Form II)
B. Matrix Spike/Matrix Spike Duplicate Summary (Form III)
C. Reagent Blank Summary (Form IV)
(If more than a single form is necessary, it must be arranged In
chronological order.)
D. CC/MS Tuning and Calibration Standard (Form V)
1. DFTPF in chronological order; by instrument.
2. BFB in chronological order; by instrument.
XII. Sample Data Package
A. Sample data in Increasing SMO Number order:
1. HSL Results - Organic Analysis Data Sheet (Form I)
2. CC/MS tentative ID (Form I, Part B) - Must be included even
if no compounds are found; if so, Indicate on form: "no
volatile compounds found" and/or "no semi-volatile compounds
found."
3. Rav data - in order: VOA, BNA, Pesticide
a. Reconstructed ion chromatogram(s) (CC/MS), chromatogram(s)
(CC)
b. Data System Printout
* Quant1tat ion report or legible facsimile (CC/MS)
* Integration report or data system printout (CC)
c. HSL spectra with lab generated standard (Dual Display)
* data systems incepablc of dual display shall provide
spectra In order:
B-2
-------
- raw HSL compound spectra
- enhanced or background subtracted spectra
- laboratory generated HSL standard
d. GC/MS library search spectra for Tentatively Identified
Compound(s) (TIC)
e. Quantltation/Caleulatlon of tentative ID concentratioa(s)
IvTStandards Data Package
A. Current list of laboratory calculated Instrument detection limits
for all HSL compounds.
B. Initial Calibration Data (Form VI) - In order: VOA. BNA; by
instrument if more than one Instrument used.
1. When more than one initial calibration Is performed, the data
must be put in chronological order. All initial calibration data must be
included even for a specific Case.
C. Continuing Calibration (Form VII) - in order: VOA, BNA; by
instrument if more than one Instrument used.
1. When more than one Continuing Calibration it performed, forms
must be in chronological order.
D. Pesticide forms in the following order:
1. Form VIII - Pesticide Evaluation Standards Summary
2. Form IX - Pcstlclde/PCB Standards Summary
3. Form X - Festieide/FCB Identification (only required for
positive results)
E. VOA standard(s) chromatograms and data system printouts (or legible
facsimile). Spectra are not required.
F. BNA standard(s) chromatograms and data system printouts (or legible
facsimile). Spectra are not required.
G. All pesticide evaluation standard(s) (A, B, and C) chromatograms and
data system printouts la chronological order.
R. All pesticide Individual Standard Mix (A or B) chromatograms and data
system printouts.
B-3
-------
X. Pesticide Quant itation stsndard(s) chroaatograas and date systea
printouts .
A. DFTPP
1. Bar graph spectrua
2. Mass listing
B. BFB
1. Bar graph sp«ctru*
2. Mass listing
C. Blank Data
1. Tabulated results (Fora I)
2. CC/MS tentative ID sheet (Form I, Pert B) even if none found
3. Raw Data - in order: VGA, BNA, Pesticide
a. Reconstructed ion ehroaatogram(a) and quant i tat ion
report (s) or legible facsimile (CC/MS)
b. ChrooatograB(s) and data system prlntout(s) (GC)
c. HSL spectra with lab generated standard (duel display)
* data systems which are incapable of dual display shall
provide spectra in order:
- raw HSL compound spectra
- enhanced or background subtracted spectre
- laboratory generated HSL standard spectre
d. CC/MS library search spectra for Tentatively Identified
Compounds (TIC)
e. Quentitat Ion/Calculation of Tentative ID concentrations
D. Matrix Spike Data
1. Tabulated results (Fora I) of non-spiked compounds
2. lew Data - In order: VGA, BNA. Pesticide
-------
•. Reconstructed Ion chroaato|raa(s) and quantitation report(s)
or legible facsimile (CC/HS)
• apectra not raqulrad .
b. Chro«atograa)(s) and data syste* printout(•) (CC)
E. Matrix Spike Duplicate Data
1. Tabulated results (For* I) of non-spiked compounds
2. Kav Data - la order: VGA, INA, Pesticide
a. Reconstructed ion chroMtofraa(s) and quantitation report(s)
or legible facaiaile (CC/MS)
- spectra not required
b. Chro«atofra>(s) and data syste* prlntout(s) (GC)
B-5
-------
RAS ORGANIC DATA REPORTING FORMS
B-6
-------
-------
Oft
0 *»•<•.
i. v»'p»«« mn
Analysis Data Sheet
0*u ftoiMM AtHMim** tv
Urn M**um (CM* On*)
Ovtt famcwd/Mvpmd ^^__^^^__
Cmc/DM'mr
WpfGQAt MCMMUfV (DOCAAWtf)
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B-7
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B-9
-------
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ai .
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Worm I. (continued).
B-10
-------
DATA REPORTING QUALIFIERS
For reporting results to EPA. the following results qualifiers are used.
Additional flags or footnotes explaining results are encouraged. However, the
definition of such flags Bust be explicit.
Value - If the result is a value greater than or equal to the detection
limit, report the value.
U - Indicates compound was analyzed for but not detected. Report
the minimum detection limit for the sample with the U (e.g., 10U)
based on necessary concentration/dilution actions. (This is not
necessarily the Instrument detection limit.) The footnote should
read: U-Coapound was analyzed for but not detected. The number
is the minimum attainable detection limit for the sample.
J * Indicates an estimated value. This flag Is used either when
estimating a concentration for tentatively identified compounds
where a 1:1 response !• ••tuned or when the mass spectral data
Indicates the presence of a compound that meets the identification
criteria but the result is less than the specified detection limit
but greater than zero, (e.g., 10J)
C - This flag applies to pesticide parameters where the identification
has been confirmed by CC/MS. Single component pesticides MO ng/ul
in the final extract should be confirmed by GC/MS.
B - This flag is used when the analyte is found in the blank as well
as a sample. It Indicates possible/probable blank contamination
and warns the data user to take appropriate action.
Other - Other specific flags and footnotes may be required to properly
define the results. If used, they must be fully described and
such description attached to the data summary report.
Form I.
(continued)•
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B-13
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B-15
-------
(A
111
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B-16
-------
OC/MS TUNING AND MASS CALIBRATION
D«caflueretriph«nylpho»phifM (DFTPP)
hwVtM
Ub It
m*
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THIS Pf MO«MANCf TUM( AWbUS TO TNI POLlOWIMC
CAW^LtS. (LANKI AND fTANOMDl
10
OATI OF ANAkTOt | TNit Of ANALYSIS
ronu v
Form V. DFTPP Tuning and Mait Calibration.
B-17
-------
QC/MS TUNING AND MASS CALIBRATION
Bromofluorobtni«n« (BF8)
10,
Conflict No.
Tim*
Ub ID.
Dm
Auttariad ly:
•ft tOtt AtUNOANCt CMITIIMA
WILATIVI ABUNOANCI
•0
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M
ITS
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177
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Orwiir «Mfi M.0% of a* to« RNk
LO • t.0% •« ••• 174
Ormi Mn H 0». M IM 1»tn 101.0% •* MM 174
10 t«K •« m*> I7«
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( )'
V*M m (v«mMM it % ««* 174.
'VMM •» JJ>IBI>»M M % mm 17$.
THIS Ff DFOHMANCI TUNI AFTUIS TO TNC FOLLOWING
SAMPLtl. tLANKS ANO STANOANOt
•AMPLf 10
LA* 10
PA7I OF ANALYSIS
TIMI OF ANALYSIS
4/M
FOJtU V
Pom V. BFE Tuning and Man Calibration.
B-18
-------
Initial Calibration Data
Volatile HSL Compound.
CM* No _
Contractor .
Contract No
mamimant ID -
Calibration Data
Minimum IF for SFCCfcO.MO Maximum % USD tor CCC fc 10%
%MO
c*
t»nf.1.
.1. t -Tr
-------
Initial Calibration Data
•emivQlatila HSL Compounds
CM* No
tootrumant B: _
Calibration Data:
Contract No:
Minimum ftpfor SPCCw 0.0*0 Manmum % USD for CCC to 90%
•'10
%MO
1 J
2. 4-T
!. 4.
1 4 }-T'«til«rMn«n«l
«• •manni «f
Mce
t -nm 4MMM« 20 «•
CCC
(..)
4/O4
Fora VI. Initial Calibration - Seal-Volatile HSL Compounda
B-20
-------
MttolCaNbmionOau
Swnivotetilc HSL Compounds
Cm No:
Instrument Or _
CalibrttiOfl Don
ComrwiNe:
Minimum ftF tor SPCC to O.OSO Maiimum « USD for CCC * 30%
*MD
MCC-
t^CMorae*
4-NitrMnrim*
J -«Mor«b*flii*n«
itfl -f «r>v«twtvi i^mntwtt
%HtB •»««
CCC -C*M»>
f»CC-S*i«*l
t -KM ««nn»ii >i 10 m
(••t
II.)
Form VI. Initial Calibration - S««l-Volatll« HSL Coapouadt
&-2J
-------
Continuing Calibration Cnocli
Volatile HSL Compounds
CtMNo: _
Contractor:
Contract No:
Calibration Data.
Tim*:
laboratory ID: -
Initial Calibration Omt:
Minimum «f for S*CC ia 0.100 ftUiimum %D for CCC * 21%
IIP
%O
ccc
Vinyl C*+f
1 1 •DiC1IOr**Tl*'i*
1 1 2.Trcniaro»in«nt
1 122 Ttl«K'0*tn»n«
Mt n M ••'
SO AtrM*
ccc c**»
I..I
Fora VII. Continuing C*libration Data - Volatile**
B-22
-------
Continuing Calibration Choc*
Samivolatilk HSl Compound!
CM* Mo
Co-
CalibrMion DM*:
Tim*: —
Contract No _
Inatrumcm R>:
Laboratory!):
Initial Calibration Dot*
Minimum MF tor SPCC to O.OM Maximum %0 tor CCC to 2t%
%D
CCC
toM 2-CMorwmtHlf in*
JC«'C' •*'«•"*
t 2
2 «
•cn«o<«t>M«tn*nt
2 * 0*»l0'oe'»«noi
1 2 4 Ti
-------
Continuing Calibration Chock
SomivoUtito HSL Compounds
CT— "•• .„
Gantrfe""-
dn»tn ••*• ..
AAtaMltaJMI '
C«mp*un4
2. «-Otmf«*y«fw
2. 4-0»«itr««tw«"«
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C-ar*i*>«ontn«i -i»«B»mh>f
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l*«aif luonniMn*
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l*
iration Oota: .
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ll Calibration D
imum%DforC
%b
•••• _ r ,
CCialiU
4cc
•
•
•
•
•
•PCC
• •
crc
I.I
Fora VII. Continuing Calibration Data - S«*l-VolatlUa
B-24
-------
Pattlclda Evaluation Standards Summary
Caao Mo. _^___^_^_
Coatract No.
Oato of *•••?•!«
•VALUATION CHECK POR LINEARITY
Laboratory
Cohmn _«_
taatrMont •>,
LASORATOKr
KtTlClK
ALBMM
BOH*
4.4'-OOT
CH.OKCNOATE
EV»L. MIX A
%MO
EVALUATION CHECK POM 4.4*-OOT/8ND«lN •HEAKOOWN
CNMM
4,«*-DOT
LAIOKATOMT
ID
TMEOF
AMALtSB
PERCENT (KEtKOOWN CxniESSEO AS TOTAL DE0UD1TCN
evAt. u« •
EVAL.MKI
EVAL. MIX •
EVfcL. MK I
EVALUATION OP METENTION TIME SHIFT FOft OWUTYLCHLOMENDATE
8MO
SAMPLE NO.
LAS
B
TMEOF
ANALTSB
PERCENT
OtFF. •
SMO
SAMPLE NO.
LAS
0
TMEOF
ANALYStt
PERCENT
wrr.«
•«8» PACKED.«O.S% CAPILLARY
FORM Vllt
For* VIII. Peitlclde Evaluation Standards Data.
4/S4
B-25
-------
PESTICIDE/PCB STANDARDS SUMMARY
OC
•C Ht«tr«M»ot 0
CO*OUNO
•i**-aHC
toU-BHC
Mu-BHC
fMMB-SHC
MMUCfttor
AMIM
M»tacM*r Iftntl
t»**X»*l
0«Mn«
4.4--OOC
fc*M
EMCtrffM I
4.4'-000
tmrm AMrtf*
CM»»l«*
|i*«Ml»CM«rMi^
T«S*»hWM
Arwltr* IOI«
ftnctor -1221
AmMr- lt»
Arwtor- 1242
Am*- 1241
Artttar- (254
*rwlv- 12*0
DATE OF AN
TMC V AM
LABOMATOM^
NT
ALYfUl
L^TUf
r «
MCTENTCN
TMC
WMOOW
CALttNATtON
fACTOH
C»F.
QUANT.
*KCCXN«lTi.FMT7
DATE « AIM
TMCOT AJU
LAtORATOK)
HT
•• COM
OUAJ
kLYM
IVU«
re
MJMATION
FACTOH
COIF.
OUANT.
KMCEN7
OTF.«»
|
J
1
n
"-"-
. xCONTmUATlON (-20* OiFPEMCNCCI
WT.aOUANTlTATlON («IO% NTFEIICNCC)
POftMIX
Ferv IX. P««tlcld«/PCB Standards Suaaary.
B-26
-------
£••• * •. _
Centred Ml
ftugU
MIHMT
COLUMN
PCITICIOC/
N*
HT4BT
TtMTATlvC
V WMOMiATC
•TMMAD
Likvrs
EOMfMIHlTIOH
CCLUMN
lary
«»%.?«.*
COLUMM
n»Moa*or
•RKRtf1
•C/MI
COfMUCP
-------
RAS INORGANIC DATA DELFVERABLES SUMMARY
TABULATED RESULTS FOR;
o PRIORITY POLLUTANT METALS AND CYANIDE
o INSTRUMENT DETECTION LIMITS
ANALYTICAL RESULTS FOR;
o MATRIX SPIKE RECOVERIES AND DUPLICATES
o CALIBRATION FREQUENCIES AND VERIFICATIONS
o PREPARATION BLANKS
o ICP INTERFERENCE CHECKS
o STANDARD ADDITION RESULTS
o LABORATORY CONTROL SAMPLES
RAW DATA SYSTEM PRINTOUTS FOR;
o SAMPLES
o CALIBRATION STANDARDS AND BLANKS
o MATRIX SPIKE AND DUPLICATES
o METHOD BLANKS
o INSTRUMENT ADJUSTMENTS
B-28
-------
RAS INORGANIC DATA REPORTING FORMS
B-29
-------
-------
U.S. EPA Contract Laboratory Program
Sample Management Office
P.O. Box Bib - Alexandria, VA 22313
703/557-2A90 FTS: 8-557-2490
Date
COVER PAGE
INORGANIC ANALYSES DATA PACKAGE
Lab hame
SOW No.
EPA No.
Case No.
Q.C. Report No.
Sample Numbers
Lab ID No. EPA No. Lab ID No.
I
Comments:
ICP Interelement and background corrections applied? Yes ^__ No .
If yes, corrections applied before _ or after _ generation of raw data.
Footnotes :
NR - not required by contract at this tine
Fora I:
Value - If the result Is a value greater than or equal to Che Instrument
detection limit but less than the contract required detection limit,
report the value in brackets (i.e., [10]). Indicate the analytical
method used with P (for ICP/Flame AA) or P (for furnace).
- Indicates element was analyzed for but not detected. Report with the
detection Halt value (e.g., 10U).
- Indicates a value estimated or not reported due Co Che presence of
interference. Explanatory note -Included on cover p«ge.
* Indicates value determined by Method of Standard Addition.
- Indicates spike sample recovery is not within control Halts.
- Indicates duplicate analysis Is not within control limits.
- Indicates the correlation coefficient for method of standard addition is
less than 0.995
U
B-30
-------
For* I
U.S. EPA Conerace Laboratory Program
Sample Management Office
P.O. Box 818 - Alexandria, VA 22313
7U3/557-2490 FTS: 8-557-2490
|EPA Sample No.
LAB NAME
SOU NO.
LAB SAMPLE ID. NO.
I
Date
INORGANIC ANALYSIS DATA SHEET
CASE NO.
QC REPORT NO.
Elements Identified and Measured
Concentration:
Matrix: Water
1. Aluminum
2. Antimony
3. Arsenic
4. Barium
5. Beryllium
6. Cadmium
7. Calcium
8. Chromium
9. Cobalt
10. Copper
1 I . Iron
12. Lead
Cyanide
Footnotes: For
Low
Soil
ug/L or mg/kg dry
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
Medium
Sludge Other
weight (Circle One)
Magnesium
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Tin
Vanadium
Zinc
Percent Solids (I)
reporting results to EPA,
standard result qualifiers are usi
as defined on Cover Pag*. Additional flags or footnotes explaining
results are encouraged. Definition of such flags must be explicit
and contained on Cover Page, however*
Comments:
Lab Manager
B-31
-------
Fora II
Q. C. Report No.
LAB NAME
DATE
INITIAL AND CONTINUING CALIBRATION VERIFICATION3
CASE NO.
SOW NO.
UNITS
Compound
Metals:
1. Aluminum
2. Antimony
3. Arsenic
4. Barium
5. Beryllium
6. Cadmium
7. Calcium
8. Chromium
9. Cobalt
10. Copper
11. Iron
12. Lead
13. Magnesium
14. Manganese
IS. Mercury
16. Nickel
17. Potassium
18. Selenium
19. Silver
20. Sodium
21. Thallium
22. Tin
23. Vanadium
24. Zinc
Other:
Cyanide
Initial Calib.1 Continuing Calibration2
True Value
Found
1
1
j XR
1
|
•
True Value
Found
ZR
Found
1
u|
|
|
|
|
|
Method4
1
1 Initial Calibration Source 2 Continuing Calibration Source
3 Control Limits: Mercury and Tin 80-120; All Other Compounds 90-110
4 Indicate Analytical Method Used: P - ICP/Flane AA; F - Furnace
B-32
-------
LAB NAME
DATE
Form III
Q. C* Report Mo.
BLANKS
CASE NO.
UNITS
Matrix
Preparation
Compound
Metals:
1. Aluminum
2. Antimony
3. Arsenic
4. Barium
5. Beryllium
6. Cadmium
7. Calcium
8. Chromium
9. Cobalt
10. Copper
11. Iron
12. Lead
13. -Magnesium
14. Manganese
IS. Mercury
16. Nickel
17. Potassium
18* Selenium
19. Silver
20. Sodium
21. Thallium
22. Tla
23. Vanadium
24. Zinc
Other :
Cyanide
Initial
Calibration
Blank Value
Continuing Calibration
1
Blank Value
2 3
*
4
Preparation Blank)
j
1 2
k
J
B-33
-------
Fora IV
Q. C. Report No.
ICP INTERFERENCE CHECK SAMPLE
LAB NAME
DATE
CASE NO.
Check Sample I.D.
Check Sample Source
Units
Compound
Metal* :
i . Aluminum
2. Antimony
3. Arsenic
4. Barium
5. Beryllium
6. Cadmium
7 . Calcium
8. Chromium
9. Cobalt
10. Copper
1 1 . Iron
12. Lead J
13. Magnesium
14. Manganese
15. Mercury
16. Nickel
17. Potassium
18. Selenium
19. Silver
20. Sodium
21. Thallium
22. Tin
23. Vanadium
24. Zinc
Other:
Control Limits1
Mean
Std. Dev.
j
True* |
Initial
1 Observed
1
ZR
| Final
Observed ZR |
II
j!
1
1
11
it
It
1
Mean value based on n »
2 True value of EPA ICP Interference Check Sample or contractor standard.
B-34
-------
Fora V
Q. C. Report No.
SPIKE SAMPLE RECOVERY
LAB NAME
DATE
CASE NO.
EPA Sample No.
Ub Saaple ID No.
Units
Matrix
Compound
Metala:
1 . Aluminum
2. Antimony
3. Arsenic
4. Barium
5. Beryllium
6. Cadmium
7. Calcium
8. Chromium
9. Cobalt
10. Copper
11. Iron
12. Lead
13. Magnesium
14. Manganese
IS. Mercury
16. Nickel
17. Potassium
18. Selenium
19. Silver
20. Sodium
21. Thallium
22. Tin
23. Vanadium
24. Zinc
Other:
Cyanide
Control Limit
ZR
75-125
M
-
-
!
••
•M
ft
ft
.
*
M
"
M
•»
M
M
M
M
N
m
*•
M
•*
-
Spiked Sample
Result (SSR)
Sample
Result (SR)
Spiked
Added (SA)
ZRl
1 ZR - ((SSR - SR)/SAJ x 100
Comaents:
"R"- out of control
"505"
-------
LAB NAME
DATE
Fora VI
Q. C. Report No.
DUPLICATES
CASK NO.
EPA Sample No.
Lab Sample ID No.
Units
Matrix
Compound
Metals:
1. Aluminum
2. Antimony
3. Arsenic
4. Barium
5. Beryllium
6. Cadmium
7. Calcium
B. Chroeium
9. Cobalt
10. Copper
11. Iron
12. Lead
13. Magnesium
14. Manganese
15. Mercury
16. Nickel
17. Potassium
18. Selenium
19. Silver
20. Sodium
21. Thallium
22. Tin
23. Vanadium
24. Zinc
Other:
Cyanide
Control Limit1
Sample(S)
Duplicate(D) RPD2
* Out of Control
1 To be added at a later date. 2 RPD - [|S - D|/((S + D)/2)] x 100
NC - Non calculable RPD due to value(s) less than CRDL
B-36
-------
Fora VII
Q.C. Report No.
LAB NAME
DATE
INSTRUMENT DETECTION LIMITS AND
LABORATORY CONTROL SAMPLE
CASE NO.
LCS UNITS
ug/L
•8/kg
(Circle One)
Compound
Metals :
1 . Aluminum
2. Antimony
3. Arsenic
4, Barium
5. Beryllium
6. Cadmium
7. Calcium
8. Chromium
9. Cobalt
10. Copper
11. Iron
12. Lead
Required Detection
Limits (CRDLJ-ug/1
Instrument Detection
Limits (IDD-ug/1
ICP/AA Furnace
200 | j |
60 |i
10
200
5
5
5000
10
50
25
100
5
13. Magnesium | 5000
14. Manganese) 15
IS. Mercury 0.2
16. Nickel 40
17. Potassium) 5000
18. Selenium 5
19. Silver
10
20. Sodlua 5000
21. Thallium 10
22. Tin
23. Vanadium
24. Zinc
Other:
Cyanide
40
SO
20
10
'
Lab Control Sample
True Found ZR
1
II
J
1
II
11
-------
Fora VIII
Q.C. Report No. _
STANDARD ADDITION RESULTS
LAB NAME
DATE
CASE NO.
UNITS
1
j Sample f
Element
0 ADD
ABS.
1 ADD
CON. /ABS.1
'
2 ADD
CON. /ABS.1
3 ADD
CON. /ABS.1
FINAL
CON.2
1
r* 1
|
1 CON ift the concentration added, ABS. is the Instrument readout in absorbance or
concentration.
^ Concentration as determined by MSA
*"r" is the correlation coefficient.
+ - correlation coefficient is outside of control window of 0.995.
B-38
-------
Form IX (Quarterly)
Instrument Detection Limits
Laboratory Nama.
Data.
, ICP/Flama AA (Circla Ont) Modal Numbar,
Furnaea AA Numbar.
Element
1. Aluminum
2. Antimony
3. Araanic
4. Barium
f . Baryllium
•. Cadmium
7. CaJeium
•. Chromium
9. Cobalt
10. Copper
11. Iron
12, laad
Wavelength
jnm)
CRDL
IWO/U
200
60
10
200
6
5
5000
10
BO
29
100
B
IDL
(ug/D
Elamant
13. Magnesium
14. Manganece
IB. Marcury
16. Niekal
17. Potauium
IB. Salanium
If. SHvar
20. Sodium
21. Thallium
22. Tin
23. Vanadium
24. Zinc
Wavalangth
(nmj
CRDL
lug/U
5000
1B
C.2
40
5000
B
10
5000
10
40
50
20
IDl i
(wg/U
!
*
i
I
Footnotaa:
_ Indieata tha inttrumant for which tha IDL appliaa with a P (for ICP/Flama AA} or •
F (for Furnaca AA) bahind tha IDL vaKta.
m Indieata alamantt commonly run with background corraction (A At with a B bahind tha
analytical wavalongth.
9 If more than ana ICP/Flama or Fumaca AA ia uaad. aubmit aaparata Forma IX-XI for
each inatrumant.
Commanta:
Lab Managar.
B-39
-------
Form X (Quarterly)
ICP Interelement Correction Factors
*t. _
-------
Form X (Quarterly)
ICP Interelement Correction Factors
laboratory,
Date,
ICP Model Number.
Analyte
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Cobalt
Copper
Lead
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Theilium
Tin
Vanadium
Zing
A alyte
Wavelength
(run)
lnt*r»l«ment Correction Factors
for
•
. \
^_
_
M1V
Comments:
B-41
-------
Form XI (Quarterly)
ICP Linear Ranges
Laboratory Name.
Date.
ICP Model Number.
Upper ICP Linearity Limits
Anelyte
1. Aluminum
2. Antimony
3. Araenic
4. Sarium
(. ieryllium
6. Cadmium
7. Calcium
•. CKromium
9, Cobalt
10. Copper
1 1 . Iron
12 Lead
Integration
Time (Second!)
Concentration
(Mfl'L)
Analyte
13. Magneiium
14. MenganeM
IS. Mercury
U. Nickel
17. Potaaaium
1|. Selenium
19. Silver
20. Sodium
21 . Thallium
22 Tin
23 Vanadium
24 Zinc
Integration
Time (Second*)
Concentration
tee a)
Footnote*.
• Indicate element* not analysed fay tCP with the notation NA.
Comments:
Lab Manafer.
-------
HAS OIOXIN DATA DELIVERABLE* SUMMARY
SAMPLE DATA PACKAGE, INCLUDING:
o TABULATED RESULTS OF 2,3,7,8-TCDD ANALYSES
o SELECTED ION CURRENT PROFILES (SICP) AND SPECTRA FOR
TCDD ANALYSES
o TABULATED RESULTS OF INITIAL CALIBRATION ANALYSES
o SICPs, RESPONSE FACTORS, CALIBRATION CURVES, AND
QUANTITATION REPORTS FOR INITIAL CALIBRATION ANALYSES
o SICPs FOR PERFORMANCE CHECK SOLUTION ANALYSES
o SICPs FOR CONTINUING CALIBRATION SOLUTION ANALYSES
o MS DOCUMENTATION FOR CONFIRMATORY ANALYSES
o CHRONOLOGICAL LIST BY INSTRUMENT OF ALL ANALYSES
PERFORMED
&-4J
-------
RAS D10XIN DATA REPORTING FORMS
-------
-------
!i ?:
M. B ^1" .
w
i
«*
^
i
at
§
^
^
i
i
t
• "
5
*)
• ;/
|i~
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fc r
]'l
if
)^« ?
-li ' - ^
"= ti3 2
i |
= n '
• • V > •»
— , — T a w ~
T 4
•i] _ | > . • *
Sis' *** I
I1"
f;
r
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i? *
1; :
s - "i S " *
It 1 1 5 !
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:f ||J 1
* *2
^ ^1
1 I "
I I i*
S«jf. ;
|f!t i
• •> • • *
*.
:.,. !
-------
FORM B-2. INITIAL CALIBRATION SUMMARY
Instr. Sol.
ID Date Tins ID
Peak Area (or Height)
320 322 323 328 332 334
Meas. Mean Neas. Mean TCDL
RF RF RF RF Iscrors
Native Native Surr. Surr. Resolut'r,
Solution ID Codes;
PC
OC1
CC2
CCJ
OC4
CCS
torforntance check eolution
Concentration calibration eolution tl • 0.2 ng/U
Concentration calibration solution f2 » 1.0 ng/U
Concentration calibration solution §3 « 5.0 ng/U
Concentration calibration solution 14 • 20.0 ny/tal
Concentration calibration solution IS • 40.0 ng/WL
B-46
ftw: 5/84
-------
FORM B-3. CONTINUING CALIBRATION SUMMARY
ID
SOl.
Date Time ID
Peak Area (or Height)
320 322 323 328
32 334
Meas. Mean Meas. Mean TCDD
RF RF RF RF Isorers
Native Native Surr. Surr. Resolut'r?
Solution ID Codes:
PC
OC1
CC2
CC3
CC4
CCS
Performance check solution
Concentration calibration solution fl «
Concentration calibration solution t2 *
Concentration calibration solution 13 *
Concentration calibration solution 14 *
Concentration calibration solution tS «
U.2 ny/tnl
1.0 na/ml
S.O ng/ml
20.0 ng/ml
40.0 ny/ml
B-47
Itev: 5/84
-------
FORM B-4. TCDO DATA REPORT - PARTIAL SCAN CONFIRMATION
Response Ratios i Relative Abundances
(relative to iVe 322)
320/322 320/324 257/322 257/259 194/196 160 161 194 196 257 259 320 322 3;
QUALITY CONTROL SUMMARY
Mean Accuracy, Surrogate Measurement*:
Accuracy, Fortified/Spike Field Blanks
Relative Differenced), Duplicate Analysis!
No. of Osta Points:
-------
APPENDIX C
SAMPLE INFORMATION AND DOCUMENTATION
C-l
-------
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C-S
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
CLP Sample Management Office
P.O. Box SIS - Akxandria, Virginia 22313
~ 703/557-2*90 - FTS/557-2WO
SPECIAL ANALYTICAL SERVICES
Client Request
SAS Number
D
Regional Transmittal
D
Telephone Request
A.
B.
C.
D.
EPA Region/Client:
Representative:
Telephone Number:
Date of Request:
Please provide below description of your request for Special Analytical Services
under the Contract Laboratory Program. In order to most efficiently obtain
laboratory capability for your request, please address the following considerations,
if applicable. Incomplete or erroneous information may result in a delay in the
processing of your request. Please continue response on additional sheets, or
attach supplementary information as needed.
1. General description of analytical service requested:
2. Definition and number of work units involved (specify whether whole samples
or fractions; whether organics or inorganics; whether aqueous or soil and
sediments; and whether low, medium or high concentration):
3. Purpose of analysis (specify whether enforcement, remedial action, etc.):
*. Estimated date(s) of collection:
5. Estimated date(s) and method of shipment:
C-9
-------
6. Approximate number of days results required after lab receipt of samples:
7. Analytical protocol required (attach copy if other than a protocol currently
used in this program): _____^_^^^_^____^__^_____^_^^_____^
8. Special technical instructions (if outside protocol requirements, specify
compound names, CAS numbers, detection limits, etc.):
9. Analytical results required (if known, specify format for data sheets, QA/QC
reports, Chain of Custody documentation, etc.) If not completed, format of
results will be left to program discretion.
10. Other (use additional sheets or attach supplementary information, as needed):
11. Name of sampling/shipping contact:
Phones
Please return this request to the Sample Management Office as soon as possible to
expedite processing of your request for special analytical services. Should you
have any questions or need any assistance, please call us at the Sample Manage-
ment Office.
C-10
-------
SAMPLE DOCUMENTATION
C-ll
-------
(&'!
USEKVIBONMDfTAi.P«CmXTIONA^*CY HW1 Sompfc- Man
;\~> K • - - A »i- r ; v- - i 'j • . v .' • tjp* ~f^ v. i-c
ORGANICS TRAITIC BEPORT
CD C«* Number:
Swnplt Sit* N*im/Cod«:
Svnplmg Personnel
Nvn*
-------
U SEKVIRONMENTALraOTtCnCW AGENCY HW1 SornjJr M™i^jcnwi< Oboe
ORGAN1CS TRAFnC RO»ORT
CM* Number.
Sample Sit* Name/Code:
©Regional Otter
Sampling Penonnel
(Phon*
Sampling Date:
(End
0 Shipping Iniormatien
Name of Cams:
Date Shipped
AvbtS Nunbvr
SAMPLE CONCENTRATION
Medium Cc
ratM
SAMPLE MATRIX
(CteckOM)
Soil/SediiM*
3> Ship To;
&>f F.
K/TSTC/v
PA
Ann
Per each »ample ooUeeted tpeah
of oontainenuMd and mark volume leral
on each bottle.
Number of
Conumcrc
Watv
(EietraetabU)
Water
(VOA>
Soil/Sadinvnt
Wafer
(Tat/VOA)
Oth-i
© SunpUDMcnptaon
Sample Location
UCLt- *
-^ Ground W.ter
__ LMchate
_ Solids
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INORGANICS TRAFFIC REPORT
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USDlVWONMaflAL PROTECTION AGENCY
INORGANICS TRAFFIC REPORT
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C-15
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HIGH HAZARD TRAFHC
FIELD SAMPLE RECORD
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HIGH HAZARD TRAFFIC REPORT
FIELD SAMPLE RECORD
CM* Number
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USEPA Contract Laoorato»y Program
CASE NO:
PO Bot8<8 Mianona Virginia 22313
FTS • 557 2490 703 557-2490 CL«, O,OX|N $M»MJENT RECORD
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CLP DIOXIN SHIPMENT RECORD
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U.S. ENVIRONMENTAL PROTECTION AGENCY
CLP Sample Mana|*T>*M Oflicc
P.O. 601 111 - Aleianana, Virginia 22)1)
Phone: 70J/5V-2*»0 • FTS/«7-2*»0
SPECIAL ANALYTICAL SERVICE
PACKING LIST
SAS Number
Sampling Of lice:
Sampling Contact:
(name)
(phone)
Sampling Dated): Snip Tot
Date Shipped:
Site Name/Code:
Atm
For Ub Uie Only
Date Samples Rec'd:
Received fty:
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2.
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9.
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Sample Condition on
Receipt at L*b
PerUkUeeOnty
White - SMO Copy, Yellow - Region Copy, Pink - Ub Copy for return to SMO, Gold - Lab Copy
C-20
-------
ENVIRONMENTAL PROTECTION AGENCY
CUP Sample MaTtgemeM OlJice
P.O. fcoitll - AJ*«»-wJMa, Vtrgmi* 2231)
Phone: 703/537-2*?: -
SPECIAL ANALYTICAL SERVICE
PACKING LIST
Number
S7C-F
Sampling Oiiice:
£1 /)*//& 5
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(name)
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(phone 1
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C-21
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SAMPLE PACKAGING AND SHIPMENT
C-25
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Contract Liberator^ Pfocrvn
REGIONAL/LABORATORY COMMUNICATION SYSTEM
Telephone Record Lof
D*te of Call:
Laboratory Name:
Lab Contact:
Region:
Regional Contact:
Call Initiated By: __ Laboratory
In reference to data tor the following sample
_ _ Region
Summary ol Quettieru/liiuei Ditcusted:
Summary of Re»olutioru
Sijrvatufe
Distribution: (1) Lab Copy, (2) Region Copy, (3) SMO Copy
Date
C-29
-------
APPENDIX D
AUXILIARY SUPPORT SERVICES DOCUMENTATION
D-l
-------
-------
SUPERFUND SAMPLE BOTTLE REPOSITORY
DELIVERY ORDER
Date of Order:.
Type of Order:
Routine
Fast Turnaround
Emergency
ORDER NO.
FROM (Name):
Affiliation:
Telephone:
AR Signature:
TO:
order
I-CHEM Research Corporation
237J7-F Eichler St. - Hay ward, CA
Telephone:
-------
SUPERFUND SAMPLE BOTTLE REPOSITORY
PACKING LIST
REPOSITORY
1-CHEM Research.
23717-F Eichler St.
Hayward, CA 9d305
Telephone: <* 15/712.3903
DESTINATION (Irom Delivery Order)
Name:
Address:
Delivery Order No.
Type of Order:
Time:
remergency only)
The materials listed below have been
shipped as requested.
Date Shipped:
Mode of Shipment:
To be delivered by:
Telephone No:
Type of Shipment: Q Partial Q
No. of
hem Cases
No. Description Shipped
1 tO oz. ftlass
2 *0-mL class
3 UL poly
* 120-mL class
5 • 16-oz (lass
6 t-oz (lass
7 »-«r (lass
t 1-L ^lass
t 32 -oz f lass
UPS, BOL, A/B No:
Signature:
Complete Q P*rti*l/Completes Order
Lot
NumbeKs)
QC
Ckarance
NumbeKs)
AUTHORIZED REQUESTOR USE ONLY
Sign below and forward the pink copy to SMO within 7 days of shipment receipt. Keep the
gold copy for your file.
The above order was received by the desfcnee, inspected, and accepted.
Date of Receipt: _ Requestor Si(naturti _
Send pink PL copy to:
USEPA Sample Manafcment Office (SMO)
P.O. Box til
Alexandria, Virginia 22313
Distribution: White - Repository Copy
Yellow . Designee Copy
Pink - Requestor Copy for Return to SMO
Cold - Requestor File Copy
D-3
Rev:10/84
-------
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-------
CASE FILE PURGE MATERIALS
Include, but are not limited tot
Sample Tags
Chain-of-Custody Records
Sample Shipment Records
Sample Receipt Logbook Pages
Copies of Internal Sample Tracking Records
Organic/^organic/High Hazard Traffic Reports
Dioxin Shipment Records
SAS Packing Lists
Extraction/Preparation Notes
Analysts1 Logbook Pages
instrument Logbook Pages
Bench Sheets
Organic /Inorganic /Dioxin/S AS Analysis Data Sheets
Standards Analysis Data
Calibration Worksheets
Chromatograms/Spectra
horganic Raw Data Printouts
Raw Data Summaries
Correspondence Memos
Document Inventory
-------
or
fOUH't l«n*IU
(MB) MM *: 1000
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MP.) •'•. t»4?t, f 147?
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C*i«x-of-Cuttod> Record
CH«in-or.Cuttoor Record
HSU 1 ItTALS
T!(M/mC»
4.12-82
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-------
OWPE COST RECOVERY CHECKLIST
1. Site Name:
J. Site No.:
a. Status: (Check One)
__JTrial Date Set - 11 yes, please give date:_
Filed
Referred to DOJ
Referred to HQ
In Preparation Stage in Region
Statute of Limitations Problem
5. Name of OSC or Regional Contact
6. Telephone Number of OSC or Regional Contact
2. State:
7. Which, if any, of the following FIT contractors were used?
(Circle One)
a. E&E Yes No Dates EAcE worked on site:
b. CHjM Hill Yes No Dates CHjM Hill worked on site:
NUS
Yes No
Dates NUS worked on site:
S. Which, if any, of the following TAT contractors were used?
(Circle One)
a. E&E Yes No Dates E&E worked on site:
b. Weston Yes No Dates Weston worked on site:
9. Were any contract laboratories used for analysis work? (Circle One) Yes No
a. Was work done through the Contract Laboratory Program (CLP)? (Circle One) Yes
No
b. If yes, list applicable Case/SAS numbers and/or CLP sample numbers below.
c. If not, who did work? List name of lab(s) and date(s) of work below.
d. Please list any other names or acronyms ever used in identifying this site:
D-8
-------
10.
11.
12.
13.
15.
Which, if any, of the following REM contractors were used?
(Circle One)
Yes No
Yes No
Yes No
Yes No
Yes No
a. Black & Veatch
b. COM
c. Weston
d. CHjM Hill
e. NUS
Dates work was done:
Dates work was done:
Dates work was done:
Dates work was done:
Dates work was done:
Please provide the following information about any contractors let by OSC:
d. Invoice Nos:
e. Invoice Dates:
^ f. Invoice Amounts:
Aa. Contractor:
b. Contract No:
c. Dates work was done:
Ba.
b.
c.
Contractor:
Contract No:
Dates work was done:
d. invoice Nos:
e. Invoice Dates:
f. Invoice Amounts:
Were any expert witnesses hired? (Circle One) Yes No
a. If yes, were these witnesses hired through either of the following contracts:
(Circle One)
TES Yes No Dates of work:
Life Systems Yes No Dates of work:
Were any overflights done? (Circle One) Yes No
a. If yes, give approximate dates of overflights: _
Was any work (e.g., evidence audits, sampling) done by NEIC? (Circle One) Yes No
a. If yes, give approximate dates of work: ..__._.
Was any work done by Tech Law, Inc. (bitera)? (Circle One) Yes No
*• K yes, give approximate dates of work: —_________________
16. Was any work done by TES? (Circle One) Yes No
a. If yes, give approximate dates ol work: _
17. Was any work done by IT (emergency response) contract? (Circle One) Yes No
a. If yes, five approximate dates ol work: _
D-9
-------
12. Please provide the following information about any other agencies that may have worked
on this site:
Approximate Dates
of Work
IAG
Number
Contact Person
at Agencv
Telephone
Number
HHS
DOI
usoc
NOAA
USGS
Corps
FEMA
DOD
D03
Contract
Number
Cooperative
Agreement No.
State
-------
-------
MEMORANDUM
DATEs
TO: Data Review Team
Sample Management Office
ROM:
USEPA Region
SUBJECT: Data Review Request
COPIES:
Please review the data from the following SMO Case:
SMO Case No.:
Site Name:
Lab Name(s):
1. Sample Information:
A. Number of Samples in Case:
B. Number of Samples to be Reviewed:
(List Numbers if Not All)
C. Organic! to be Reviewed? Yes No
D. Inorganics to be Reviewed? Yes No
-------
H. User Information:
A. User Organization:
Contact for Questions:
Name:
C.
Type{») of Review Requested:
Check All
That Apply
QA/QC Compliance
Problem Case
Applications
Consulting
Other
Specify: ______^
|~"1
| _ j
( I
| _ j
D. Additional Issues to Address in Review:
Enforcement I j
Preliminary Assessment I I
Site Investigation
Remedial Action
Site Monitoring
Undetermined
Other
Specify: ____^^_L.
D
D
D
D
D
Telephone:
Date
Needed
Intended Use of Data:
Check All
That Apply
D-12
-------
F. Comments:
D-13
-------
-------
QA/QC COMPLIANCE REPORT
D-l*
-------
-------
MEMORANDUM
DATE:
TO:
PROM:
SUBJECT:
COPIES:
USEPA Region
SMO Data Review Team
QA/QC Compliance Review Summary for a
Contract Laboratory Organic Data Package: Case No.
As requested, quality control and performance measure for the data packages
noted have been examined and compared to EPA standards for compliance.
Measures for the following general areas were evaluated:
L Data Completeness
IL Spectra Matching Quality
!IL Surrogate Spikes
IV. Matrix Spikes
V. Duplicates
VL Blanks
VIL DFTPP and BFB Tuning
VIIL Chromatography
IX. Holding times
Any statistical measures used to support the following conclusions are attached so
that the review may be reviewed by others.
Correspondence Dates;
A. Review Requested
B. Review Authorized
C, Results Available
D. Review Mailed
Action Items;
D-15
-------
Data Reviewed
(Use Number:
Site Name:
Laboratory Name(s):
Intended Use:
Conclusions
Compared to existing contract standards, each fraction is found to be acceptable,
acceptable but qualified as noted, preliminary pending verification or unacceptable.
Qualified Prelimi- Un-
Acceptable Acceptable nary Acceptable
Fractions:
A. Volatites
B. Base/Neutrals
C Acids
D. Pestkides/PCBs
E, TCDD
Comments and Qualifications: See Text.
Data Prepared Byt
Reviewer* Name:
Reviewer* Signature!
Telephone NO.S
FTSUnet
Date:
Date:
Appendices
A. Sample List
B. Summary of Compounds Found
C Glossary and Data Qualifiers
6/27/S*
D-16
-------
SUt Imhjf LT
EXAMPLE
UTtKBlt. 1: IIMUKT Or COXPOIiKH ro««t>
-------
D. SPECTRA MATCHING QUALITY
Spectra Were Examined and Found to be of Good Matching Quality
Some Spectra Were Examined and Found to be of Poor Matching Quality
Remarks:
D-1S
-------
I
*
D-19
-------
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Fhe matrix spike results
vith the MSR guidelines
Compound
Volatile*
1,1-Djchloroethylene
Trlchloroethylene
Chlorobenzene
Toluene
Benzene
Base/Neutrals
i,2,*-trichlorobenzene
Acenephthene
2,%-dinitrotoluene
Di-n-butylphthalate
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N-nitrosodi-n-propylam
1 , *»dichlorobenzene
Acids
Pentachlorophenol
Phenol
2-chlorophenol
p-chlofo-m-cr«ol
*-nitrophenol
-------
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V. DUPLICATE ANALYSIS RESULTS
The relative percent difference (RPD) for each parameter group was evaluated. The
delicate analysis RPD acceptance criteria should be:
Maximum Acceptable
Fraction Percent Difference
Volatile 15%
Base/Neutral 30%
Acid *0%
Pesticide 40%
The RPDs exceeding the maximum acceptable percent difference were:
Concentration
Compound Actual RPD Sample Duplicate
Fraction:
Volatile ]
Base/Neutral rj
Acid
Each duplicate analysis was examined in reference to compounds detected in each
analysis. Those compounds which were not common to each analysis for the duplicate
sample are listed below:
Sample
Fraction Number Compound Concentration
Remarks:
D-25
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VL BLANK ANALYSIS RESULTS
The blank analysis was reviewed. The contarmnents in the blank are listed below:
Fraction
Compound
Significant
Yes
Yes
Yes
No,
No
No
Remarks:
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ITU. DFTPP AND BFB TUNING RESULTS
___ The DFTPP tuning results were reviewed and found to be within the q»ecif ied
criteria.
The BFB tuning results were reveiwed and found to be within the specified
criteria.
The (DFTPP/BFB) tuning results were reviewed and the following abundances were
found to fail outside the specified criteria:
Required Actual
Compound m/z Abundance Abundance
The (DFTPP/BFB) performance results which were found to be outside the
contractually-required tuning requirements do not have an adverse technical impact on
the data.
No adverse technical impact.
Adverse impact on data.
Remarks:
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CHROMATOCRAPHY CHECKS
Resolution and Sensitivity
Type of Columns Packed Column Fused Silica Capillary Column (FSCC)_
Packed Column Chromatography Check)
Tailing
Factors
Benzidine
Pentachlorophenol
FSCC Chromatography Check:
50-ng benzidine detectable?
Acceptance
Windows
Less Than 3
Less Than 5
Yes
Actual
No
Pentachlorophenol response factor? Yes No
General shape of the total ion chromatograrm
Acids
Base/
Neutrals
Voiatiles
Pesticides
Peak Shape
Interferences _ .
Background . ._
Standards
General shape of the total ion chromatographyi
Base/
Neutrals
Acids
Voiatiles
Pesticides
Peak Shape
Interferences
Background
Remarks:
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MEMORANDUM
DATE:
TO:
USEPA Region
FROM:
SMO Data Review Team
SUBJECT: QA/QC Compliance Review Summary for a
Contract Laboratory Inorganic Data Package: Case No.
COPIES:
As requested, quality control and performance measure for the data packages
noted have been examined and compared to EPA standards ior compliance.
Measures for the following general areas were evaluated:
L Data Completeness IV. Blanks
1L Matrix Spikes V. 1CP Interference Check
IIL Duplicates VL Calibrations
Any statistical measures used to support the following conclusions are attached so
that the review may be reviewed by others.
CorrespondenceDates;
A. Review Requested
B. Review Authorized ^_
C, Results Available
D. Review Mailed
Action Items;
I .
D-29
-------
Data Reviewed
Case Number:
Site Name:
Laboratory Name(s):
Intended Use;
Conclusions
Compared to existing contract standards, each fraction is found to be acceptable,
acceptable but qualified as noted, preliminary pending verification or unacceptable.
Qualified Prelimi- Un-
Acceptable Acceptable nary Acceptable
Fractions:
A, Taskl(ICP)
B. Task II (AA)
C Task HI (CN)
Comments and Qualifications: See Text.
Data Prepared Byi _
Reviewer's Name: _
Reviewer's Signature: . . ._
Telephone No:
FTSUnet
Date:
Date:
Appendices
A. Sample List
Summary of Elements Pound
Glossary and Data Qualifiers
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ic-a
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APPENDIX E
REFERENCES
NOTE: The references in this Appendix are supplied for
general information purposes and do not necessarily
represent methods or procedures utilized in the CLP.
\
\
E-l
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ANALYTICAL REFERENCES
American Public Health Association, A-nerican Water Works Association, Water Pollution
Control Federation, Standard Methods lor Examination of Water and Wastewater,
l*th Ed., (1975).
American Society lor Testing and Materials, Annual Book of ASTM Standards, Part 31,
"Water", Standard D3223-73, p. 343 U976JI
Bishop, IN., Mercury in Sediments, Ontario Water Resources Comm., Toronto, Ontario,
Canada, 1971.
Brandenberger, H. and Bader, H., "The Determinatin of Nanogram Levels of Mercury in
Solution by a Flameless Atomic Absorption Technique," Atomic Absorption News-
letter 6. 101, (1967).
EPA, Environmental Monitoring and Support Laboratory, Cincinnati, Ohio, Interim
Methods for the Sampling and Analysis of Priority Pollutants in Sediments and Fish
Tissue. Aug. 1977. Revised October 1980.
EPA, Handbook for Analytical Quality Control in Water and Wastewater Laboratories,
USEPA-600/W9-019.
EPA, Handbook for Monitoring Industrial Wastewater. USER A Technology Transfer, 1973.
EPA, Methods for Chemical Analysis of Water and Wastewater, USEPA Technology
Transfer, 197*.
EPA, Methods for Chemical Analysis of Water "and Wastes. EPA Pub. 600/0-79-02, March
1979.
EPA Office of Solid Waste and Emergency Response, Modification (By Committee) of
Method 3050, 5W-S46, 2nd Ed., Test Methods for Evaluating Solid Waste. July 1982.
EPA, Procedures Manual lor Croundwater Monitoring at Solid Waste Disposal Facilities,
EPA930/SW-611, 1977.
EPA EMSL, Users Guide for the Continuous Flow Analyzer Automation System.
Cincinnati, Ohio, 1981.
Garbarino, 3.R. and Taylor, HE., "An Muctively-Coupled Plasma Atomic Emission
Spectrometric Method for Routine Water Quality Testing," Applied Spectroscopy 33.
No. 3, 1979.
Goulden, P.D. and Afghan, B.K., An Automated Method for Determining Mercury in
Water, Technicon, Adv. in Auto. Analy. 2, p. 317 (1970).
Hatch, W.R. and Ott, W.L., "Determination of Sub-Microgram Quantities of Mercury by
Atomic Absorption Spectrophotometry.* Analytical Chemistry »0. 2085 (1968).
-------
ANALYTICAL REFERENCES
(continued)
Kopp, IF., Longbottom, M.C, and Lobring, L.B., "Cold Vapor Method for Determining
Mercury," AWWA, VoL 64, p. 20, Jan. 1972.
Martin, T.D., Kopp, 3. F., and Ediger, R.D., "Determining Selenium in Water, Wastewater,
Sediment and Sludge by Flameless Atomic Absorption Spectroscopy", Atomic
Absorption Newsletter 14, 109, 1973.
Organochlorine Pesticides and PCBs, Method 60S; 2,3,7,8-TCDO, Method 613; Purgeabies
(Volatiles), Method 624; Base/Neutrals, Acids and Pesticides, Method 625; Federal
Register. VoL 44, No. 233, Monday, December 3, 1979, pp. 69501, 69526, 69532 and
69540.
Owerbach, Daniel, "The Use of Cyanogen iodide (CND as a Stabilizing Agent lor Silver in
Photographic Processing Effluent Sample," Photographic Technology Division,
Eastman Kodak Company, Rochester, New York, 14650.
Technicon Industrial Systems, Operation Manual for Technicon Auto Analyzer 11C System,
Technical Pub. #TA9-0460-00, Tarry town, New York, 10591, 1980.
Martin, Theodore D., EMSL/Cincinnati, Inductively Coupled Plasma - Atomic Emission
Spectrometric Method of Trace Elements Analysis of Water and Waste, Method
200.7, Modified by CLP ^organic Data/Protocol Review Committee.
Winefordner, ID., "Trace Analysis: Spectroscopic Methods for Elements," Chemical
Analysis. VoL 46, pp. 41-42.
Winge, R.K., Peterson, V.3., and Fassel, V.A., Inductively Coupled Plasma - Atomic
Emission Spectroscopy Prominent Lines, EPA-600/4-79-017.
Wise, R.H., Bishop, D.F., Williams, R.T.', and Austern, B.M., Gel Permeation Chroma-
tography in the GC/MS Analysis of Organic* in Sludges. USEPA. Municipal
Environmental Research Laboratory; Cincinnati, Ohio 43268.
SAFETY REFERENCES
Committee on Chemical Safety, Safety in Academic Chemistry Laboratories, American
Chemical Society Publications, 3rd Ed,, 1979.
Department of Health, Education and Welfare, Public Health Service, Center for Disease
Control, National Institute for Occupational Safety and Health, Carcinogens -
Working with Carcinogens. Pub. No. 77-206, Aug. 1977.
Occupational Safety and Health Administration (OSHA), OSHA Safety and Health
Standards. General Industry. (29 CFR 1910), OSHA 2206, (Revised January 1976).
Wallace, R.A., Fulkerson, W., Shults, W.D., and Lyon, W.S., Mercury in the Environment -
The Human Element, Oak Ridge National Laboratory, ORNL/NSF-EP-1, p.
31 (January 1971).
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SAMPLING REFERENCES
EPA Environmental Response Team, Field Monitoring and Analysis of Hazardous
Materials, EPA Training Manual, Course NO. ite.*, Cincinnati, Qruo, i w>.
Hiibregtse, K.R., and Moser, 1H>, Handbook for Sampling and Sample Preservation of
Water and Wastewater. USEPA-*00/4-76«0<»9, 1976.
Municipal Environmental Research Laboratory, USEPA, Samplers and Sampling Procedu-
res for Hazardous Waste Streams. EPA-600/280-OU, Cincinnati, Ohio, 1980.
National Enforcement tivestigations Center, Enforcement Considerations lor Evaluation
of Uncontrolled Hazardous Waste Sites by Contractors, EPA Office of Enforcement,
Denver, Colorado, 19SO.
Olson, D.M., Berg, E.L., Christensen, R., Otto, ri, Ciancia, 1, Bryant, G., Lair, M.D.,
Birch, M., Keffer, W., Dahl, T. and Wehner, T., Compliance Sampling Manual. EPA
Enforcement Division, Office of Water Enforcement, Compliance Branch, 1977.
Weber, C.L, Biological Field and Laboratory Methods for Measuring the Quality of Surface
Waters and Eif luents. USEPA-670/<*-73-001, 1973.
SHIPPING REFERENCES
Federal Express Corporation, Hazardous Materials Department, Telephone: 1-400-238-
5592.
U.S. Department of Transportation, A Guide to the Federal Hazardous Materials
Transportation Regulatory Program, 1983.
U.S> Department of Transportation, U.S. Department of Transportation Regulations, *9
CFR Parts 100 - 199, October 1, 1978.
E-4
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