User's 6mdc h> 1U Gmtocf- Uhombt^ Pto^tam
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 require-
ments and analytical procedures of the new/ CLP protocols developed from technical
caucus recommendations. These protocols were implemented into CLP analysis
contracts in 1985. Other analytical programs, procedures and documentation
described herein reflect the status of the program as of July 1986. Critical
information for CLP samplers and user groups is contained in Chapter III and Appendix
C. This information should be distributed to all contractors collecting samples for the
CLP and to each user group of the EPA and of the States.
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.
Third Printing
Issued: December 1986
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CLP USER'S GUIDE
TABLE OF CONTENTS
Pace
CHAPTER I BACKGROUND AND INTRODUCTION
A. CLP Objectives and Orientation 2
B. CLP Structure 3
1. Program Management 3
a. National Program Office (NPO) 3
b. Sample Management Office (SMO) 5
c. USEPA Office of Research and Development (ORD), Environmental
Monitoring Systems Laboratory/Las Vegas (EMSL/LV) 6
d. National Enforcement Investigations Center (NEIC) 7
2. Regional Program Support 7
a. Contract Deputy Project Officers 7
b. Regional Sample Control Centers 7
c. Technical Caucuses 8
d. Regional/Laboratory Communication System 8
3. Clients/Users 9
a. EPA Regions 9
b. States 9
c. Non-Superfund Clients 9
i- t. • • ,
4. Analytical and Support Contractors 10
'Analytical Laboratories 10
b. Sample Bottle Repository 10
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Page
CHAPTER H DESCRIPTION OF ANALYTICAL SERVICES 11
Menu of Routine Analytical Services (RAS) 13
Menu of Special Analytical Services (SAS) 1 b
A. Organic Routine Analytical Services (RAS) 15
1. Sample Matrices, Concentration Levels and Volumes Required 15
2. Compounds Identified and Quantified 17
3. Contract Deliverable Requirements 18
k. Analytical Protocols 19
a. Water Method 19
b. Soil Method 20
c. Contract Required Detection Limits (CRDLs) 20
5. Contract Quality Control Requirements 21
B. Inorganic Routine Analytical Services (RAS) 23
1. Sample Matrices, Concentration Levels, Volumes Required
and Preservation Techniques 23
2. Constituents Identified and Quantified 26
3. Contract Deliverable Requirements 26
U. Analytical Protocols 27
a. Water Method 27
b. Soil/Sediment Method 28
c. Contract Required Detection Limits (CRDLs) 28
5. Contract Quality Control Requirements 29
C. Dioxin Routine Analytical Services (RAS) 32
1. Sample Matrix and Volume Required 32
2. Isomer Identified and Quantified 33
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Page
C. (Dioxin RAS - continued)
3. Contract Deliverable Requirements 33
4. Analytical Protocols 34
a. Soil/Sediment Method 34
b. Contract Required Detection Limits (CRDLs) 35
5. Contract Quality Control Requirements 35
D. Special Analytical Services (SAS) 37
1. SAS Services 39
a. RAS Plus SAS 39
(1) Fast Turnaround 39
(2) Organic - Special Requirements in Addition to RAS 40
(3) Inorganic - Special Requirements in Addition to RAS 40
(4) Dioxin - Special Requirements in Addition to RAS 41
b. All SAS 41
(1) Organic - Special Requirements Not Provided by RAS 41
(2) Inorganic - Special Requirements Not Provided by RAS 42
(3) Dioxin - Special Requirements Not Provided by RAS 42
(4) High Concentration Sample Analysis - Organic and Inorganic 42
(5) Special Topics Analysis 43
2. Contract Deliverable Requirements 43
3. Contract Quality Control Requirements 43
iv
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Page
CHAPTER HI UTILIZATION OF ANALYTICAL SERVICES 45
A. Analysis Initation/Request Procedures 46
1.
RAS Initiation Process
46
a. User Information Required
46
b. Lead-Time Requirement
47
c. Case Number Assignment and Laboratory Scheduling
47
d. User Knowledge of Analytical Protocols
48
2.
SAS Initiation Process
49
a. User Information Required
49
b. Lead-Time Requirements
50
c. SAS Number Assignment and Laboratory Scheduling
51
d. User Provided Analytical Protocol
52
3.
Procedures for Making Changes to Analytical Requests
53
Regional Organic Allocation System
55
Sample Documentation
56
1.
Sample Traffic Report (TR)/Usage, Distribution, Ordering
56
2.
Dioxin Shipment Record (DSR)/Usage, Distribution, Ordering
58
3.
SAS Packing List (PL)/Usage, Distribution, Ordering
59
4.
Sample Tag
60
5.
Chain-of-Custody Record
61
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Page
D. Sample Packaging and Shipment 6ft
1. Packaging Requirements 6ft
2. Shipping Instructions 65
3. . Shipment Coordination 66
E. Procedures for Problem Resolution 68
1. Resolving Problems Concerning Sample Shipment and Analysis 68
2. Resolving Problems Concerning Analytical Data 68
CHAPTER IV AUXILIARY SUPPORT SERVICES 70
A. Sample Bottle Repository Program 70
1. Types and Quantities of Containers Available 71
2. Ordering Procedures 72
3. Shipment Information 75
ft. Procedures for Problem Resolution 76
a. Resolving Problems Concerning Container Shipment 76
b. Resolving Problems Concerning Container Contamination 76
5. Summary of Container Cleaning and Quality Control Procedures 77
B. Information Services 79
1. Regional Sample List Report 79
2. Sample Status Information 79
3. General Program Information 80
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Page
C. Enforcement Support 81
1. Generation of Enforcement Quality Data SI
a. Chain-of-Custody and Document Control 81
b. NEIC Evidence Audits 82
2. Additional CLP Enforcement Support 83
a. Request Procedures 83
b. Requestor Information Required 83
c. Documentation/Support Provided by CLP 84
D. Cost Recovery Substantiation 85
1. Request Procedures 85
2. Requestor Information Required 85
3. Documentation Provided by CLP 86
E. Contract Compliance Screening 88
F. Data Review Services 89
h Requestor Information Required 90
2. Documentation Provided by CLP 91
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Page
CHAPTER V PROGRAM QUALITY ASSURANCE 92
A. Interface with Agency Quality Assurance 93
B. Laboratory Selection Process 95
1. Prebid Conference 95
2. Preaward PE Sample Analysis 95
3. Bid Price 96
k. Preaward Bid Confirmations 96
a. Standard Operating Procedures 96
b. On-Site Laboratory Evaluation 97
C. Laboratory Start-Up Process 98
1. Provision of Standards to Laboratory 98
2. PO Review of First Data Packages 98
3. PO/DPO Laboratory Visits 98
U. PO/DPO/SMO/Laboratory Communication 99
D. Laboratory Performance Evaluation 100
1. Performance Evaluation Sample Analysis 100
2. On-Site Laboratory Evaluation 100
3. Corrective Action 100
E. Sample Data Evaluation 102
1. Intercomparison Check Sample Studies 102
2. Regional Sample Split/Spike Programs 102
viii
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Page
F. Analytical Data Review 103
1. EMSL/LV Data Review 103
2. Regional Data Review 104
3. Contract Compliance Screening (CCS) 104
4. SMO Data Review Services 104
G. Analytical Methodology Improvement/Development 105
1. Protocol Standardization and Improvement 105
2. Method Development 105
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CLP USER'S GUIDE
INDEX TO APPENDICES
Page
APPENDIX A: CLP DIRECTORY
A-l
CLP National Program Offices
A-2
USEPA Regions
A-8
Sample Management Office
A-21
Regional Deputy Project Officers
A-23
Regional Sample Control Centers
A-24
CLP Regional/Laboratory Communication System
A-27
APPENDIX B: RAS DELIVERABLES AND DATA REPORTING FORMS B-l
RAS Organics Deliverables Index B-2
RAS Organic Data Reporting Forms B-6
RAS Inorganic Deliverables Index B-2S
RAS Inorganic Data Reporting Forms B-32
RAS Dioxin Deliverables Index B-48
RAS Dioxin Data Reporting Forms B-49
APPENDIX C: SAMPLE INFORMATION AND DOCUMENTATION C-l
Organic Sample Collection Requirements C-2
Inorganic Sample Collection Requirements C-3
Dioxin and High Hazard Sample Collection Requirements C-4
Special Analytical Services Client Request Form C-5
RAS Re-Analysis Request/Approval Record C-8
SAS Re-Analysis Request/Approval Record C-9
Sample Documentation: C-10
Organic Traffic Report and Completed Example C-ll
Inorganic Traffic Report and Completed Example C-13
Dioxin Shipment Record and Completed Example C-15
High Hazard Traffic Report and Completed Example C-17
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Index to Appendices (continued)
Pagp
SAS Packing List arid Completed Example C-19
Examples of Sample Tag and Custody Seal C-21
Chain of Custody Record and Completed Example C-22
Sample Packaging and Shipment: C-24
Sample Packaging Summary C-25
Sample Shipment Coordination Checklist C-26
Potential Problems with Sample Shipment and Analysis C-27
Regional/Laboratory Communication System - Telephone Record Log C-28
Deputy Project Officer Communication Summary C-29
Request for Corrective Action Form C-30
APPENDIX D: AUXILIARY SUPPORT SERVICES DOCUMENTATION D-1
Sample Bottle Repository Superfund Delivery Request D-2
Sample Bottle Repository Superfund Packing List D-3
Example of Regional Sample List D-4
Case File Purge Materials D-5
QA/QC Compliance Report: D-6
SMO QA/QC Compliance Review Summary Memorandum D-7
Case Narrative Form D-8
Review Matrix Forms D-12
Contract Compliance Screening: D-16
Organic Screens D-17
Inorganic Screens D-21
APPENDIXES REFERENCES E-l
Analytical References E-2
Safety References E-3
Sampling References E-^
Shipping References E-4
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CHAPTER I
BACKGROUND AND INTRODUCTION
I
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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's Superfund effort, originally under the 1980
Comprehensive Environmental Response, Compensation, and Liability Act
(CERCLA) and presently under the 1986 Superfund Amendment and Re-
authorization Act (SARA) 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 legally-defensible analytical results for
use in supporting Agency enforcement actions. Therefore, a high level of quality
assurance and documentation 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 Superfund 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, as well as states and other EPA
programs, such as RCRA, which have become part of the CLP user community.
The CLP is a service program designed to provide a wide range of enforcement-
quality 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 all CLP services and responses.
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B. CLP Structure
The CLP effort involves numerous Agency, contractor and other groups through-
out the country. These organizations are identified and their role 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.
1. Program Management
a. National Program Office (NPO)
The CLP is directed by the National Program Office, in EPA
Headquarter's Analytical Support Branch (ASB), 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, Inorganic and Dioxin Technical
Project Officers (PO); the Sample Management Office Project
Officer; and a Quality Assurance (QA) Officer.
NPO responsibilities includes 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 special analytical
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.
The National Program Manager (NPM), in addition to directing
program staff, is responsible for the formulation of program policies
3
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INTERRELATIONSHIP OF PROGRAM PRINCIPALS
CLP CLIENT/USERS
RSCC
• SCHEDULING
ANALYSES
• ANALYSES
PRIORITIZATION
• PROBLEM RESOLUTION
• CONTRACT MONITORING
• PROTOCOL DEVELOPMENT
• STANDARDS
• OA DATA BASE
AUDIT REPORTS
LAB/METHOD PERFORMANCE REPORTS
CONTRACT PROCUREMENT
CONTRACT MODIFICATIONS
• CONTRACT EVIDENCE AUDIT TEAM
• DOCUMENT AUDIT CONTRACTOR
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and direction; communicates with the Regional and Agency communi-
ties on a continuing basis, keeping all parties apprised of program
activities and receiving input on program effectiveness.
The Technical Project Officers (POs) are responsible for technical
program decisions, contract administration and contractor perform-
ance 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 techni-
cal caucuses for purposes of CLP data and protocol review.
The Sample Management Office (SMO) Project Officer is responsible
for the administration of the SMO contract as well as overseeing the
overall supply/demand balance between CLP contracts and client
needs. This PO is also responsible for the administration of the
Sample Bottle Repository contract.
The Quality Assurance (QA) Officer coordinates all aspects of
program application of QC 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 QC 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
scheduling and tracking; (2) Contract Compliance Screening;
(3) Special Analytical Services subcontracting; (4) laboratory invoice
5
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processing; (5) maintenance of CLP records and management report-
ing; and (6) NPO management, technical and administrative support.
SMO routinely receives analytical requests from the Regions, coordi-
nates and schedules sample analyses, tracks sample shipment and
analyses, receives and checks data for completeness and compliance,
processes laboratory invoices, and maintains a repository of sampling
records and program dat&. In response to client requests for non-
routine types of analyses, SMO subcontracts for Special Analytical
Services (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 ORD 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 on-site
laboratory evaluations; prepares performance evaluation (PE) samples
for pre-award and post-award 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 reference standards to program
laboratories through the contractor-operated 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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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; which 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's
evidence audit process appears in Chapter IV, Section C.
2. Regional Program Support
The Regions play 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 participates in laboratory on-site evaluations.
b. Regional Sample Control Centers
In January, 1984, each Region established a Regional Sample Control
Center (RSCC) to centralize ordering of CLP sample analyses within
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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,
where applicable. The Primary AR makes final determinations
regarding Regional analysis priorities when conflicts occur. RSCC
ARs routinely place all Regional requests for CLP analyses, coordi-
nate 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.
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 method-
ologies and data reporting requirements. Technical caucuses are held
on a periodic basis and involve participation of the following groups:
EPA Regions, EMSL/LV, EMSL/Cincinnati, NEIC, contract labora-
tories, 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.
Regional/Laboratory Communication System
In January 1983, the NPO established a system of direct communica-
tion 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 most timely and direct
manner possible. In this system, designated Regional communi-cation
contacts call designated laboratory communication contacts as
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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 an
RSCC, which schedules all CLP analyses requests for the Region,
coordinating Regional sampling to balance with allocated numbers of
CLP sample analyses available each month, and prioritizing the
Region's 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 that arise. In this role, the RSCC also processes
analytical requests from state or other program users that are
located in the Region's geographical area.
b. States
Under RCRA - CERCLA Cooperative Agreements, any state
undertaking initial site investigations and entering into cooperative
agreements with the government for cleanup of local waste sites, can
utilize CLP services. States must access CLP analytical services
th ough the RSCC and data packages are distributed to states
through the RSCC.
c. Non-Superfund Clients
Program services are available to support non-Superfund clients on a
"noninterfering" basis. Non-Superfund analyses and other CLP
support are provided by the CLP through transfer of funds from the
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non-Superfund program to the CLP. Non-Superfund clients currently
include other government agencies and other EPA programs, such as
Office of Acid Disposition, Office of Solid Waste, and the National
Dioxin Study.
k. Analytical and Support Contractors
a. Contract Analytical Laboratories
The CLP's 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 must 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. Sample Bottle Repository
The Superfund 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 repositories serve as a central source for several
types of pre-cleaned sample bottles which are routinely utilized by
Regional and contract personnel performing Superfund sampling
activities. Repository services are detailed in Chapter IV.
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CHAPTER D
DESCRIPTION OF ANALYTICAL SERVICES
11
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CHAPTER H
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. In response to the increasing analyti-
cal demands of its client base, the CLP has continually expanded its analytical
capacity for standardized analyses through frequent IFB solicitations. On the average,
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 four separate analytical programs:
o Organic Routine Analytical Services (RAS),
o Inorganic RAS,
o Dioxin 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, which provide
analytical services to Superfund clients. The SAS program provides unique, non-
standardized analytical services to Superfund and non-Superfund clients for organic,
inorganic, dioxin and other 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.
The two tables which follow outline the menu of services available under the CLP'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 Contract deliverable requirements.
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Table 2
MENU OF ROUTINE ANALYTICAL SERVICES
ts
Category
Sample
Matrices
Compounds
Identified
&
Quantified
Deliverables
Analytical
Procedures
QA/QC
RAS
Organic
Analysis
Low Sc. Medium Concentration
Water & Soil/Sediment Samples
HSL Compounds &
Library Matches of
30 Highest Compounds
(In the ppb Range)
Extraction in 5 Days for H^O
& 10 Days for Soil Samples
VOA Analysis in 10 Days for h^O
& 10 Days for Soil Samples
Data Delivery in
30,
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Table 3
MENU OF SPECIAL ANALYTICAL SERVICES (SAS)
RAS Plus SAS Category
Examples of Services Available:
o Fast Turnaround Analysis by RAS Organic,
Inorganic or Dioxin IFB Protocol
o RAS/Organic Analysis with Additions/Adjustments
to IFB Protocols.
o RAS Inorganic Analysis with Additions/Adjustments
to IFB Protocol
o RAS Dioxin Analysis with Additions/Adjustments
to IFB Protocol
All SAS Category
Examples of Services Available:
o Organic Analysis Per Non-RAS Protocols, Matrices,
Com pounds
o Inorganic Analysis Per Non-RAS Protocols, Matrices,
Com pounds
o Dioxin Analysis Per Non-RAS Protocols, Matrices,
Com pounds
o Organic and Inorganic High Concentration
Sample Preparation and Analysis
o Special Topics Analysis (As Requested)
NOTE: The client requestor is responsible for designating IFB method adjustments in RAS Plus SAS
work and for supplying suitable analytical protocols for All SAS work. Additionally, the
client must provide QA/QC procedures and criteria, and must specify analysis and data
reporting delivery schedules. This information must accompany the client's request for SAS
services.
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o Description of analytical protocols and detection limits,
o Contract quality control requirements.
The organics and inorganics RAS sections present the caucus-revised protocols
implemented in 1985.
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 this Guide, Regional DPOs maintain a Master Copy notebook of each
Statement of Work (SOW) under which CLP RAS laboratory contractors operate.
Users are instructed to consult the Region's Master Copy SOWs for detailed analytical
information.
A. Organic Routine Analytical Services (RAS)
1. Sample 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 single-phase, homo-
geneous 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 com-
pounds 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
only. Low and medium level analysis designations are performed within the
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laboratory to determine the appropriate analytical protocol to be used.
For soil/sediment samples only, there are separate procedures for semi-
volatiles organics analysis depending upon whether the samples are
determined to be low ( >20 ppm) or medium (>20 ppm) concentration.
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 low
level, one gallon sample volume is required for extractables - base,
neutral, acid (B/N/A) and pesticides/PCB, and 80 ml for volatiles (VOA).
The extractables sample is collected in two SO-ounce amber glass bottles,
four 1-liter amber glass bottles, or one 4-liter amber glass bottle. The
volatiles sample is collected in two 40-ml glass vials. For RAS organics
analysis of a water sample estimated as medium level, a four liter volume
is required for extractables and 80 ml for volatiles. The extractables
sample should be collected in four 32-ounce glass jars, and the volatiles
sample in two 40-ml glass vials. For RAS organics analysis of a
soil/sediment sample estimated as low or medium level, a six ounce volume
is required for extractables. The siample should be collected in one 8-ounce
glass jar for extractables and two 120-ml glass vials for volatiles.
For a laboratory to perform matrix spike, matrix spike duplicates, and
contractual reanalyses, triple the. sample volume is required in at least one
sample in twenty for each sample with the same concentration/matrix.
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. Soil
blanks are supplied to Regions by EMSL/LV. Use of aqueous blanks for soil
samples is not appropriate.
For shipping purposes, each sample estimated as medium level (water or
soil) must be enclosed and sealed in a metal paint can for shipment.
Because it is not certain whether a sample is actually low or medium level,
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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.
If sufficient sample volume is not provided, completion of all required
parameters and/or complete QA/QC determinations 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.
2. Compounds Identified and Quantified
The organic RAS program provides identification and quantification of EPA
Target Compound List (TCL) (previously termed the Hazardous Substances
List ~ HSL) organic compounds (VOA, B/N/A, and pesticide/PCB fractions)
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 NBS
Mass Spectral Library searches for compounds not identified on the TCL
(HSL). The 10 peaks of greatest apparent concentration in the volatile
fraction and the 20 peaks in the base/neutral/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-TCL (HSL) organic compounds provides information
on potential organic contaminants outside of the analytical parameters of
the RAS program.
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3. Contract Deliverable Requirements
The organic RAS program specifies contractually required deliverables by
the laboratory for sample extraction, volatile analysis and data reporting.
These requirements include:
o Completion of sample extraction for water samples within 5 days of
sample receipt and for soil samples within 10 days of sample receipt;
o Completion of volatile analysis for water samples within 7 days of
sample receipt and for soil samples within 10 days of sample receipt;
o Completion of extractable analysis and reporting of data within 30 or
40 days (as specified by the contract delivery schedule) following
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.
The organic RAS data package provides a complete set of data for
independent 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 QC processes applied.
o Copies of sample Traffic Reports.
o Quality control summary, containing surrogate, method blank, matrix
spike and matrix spike duplicate analyses recoveries, and instrument
tuning and performance information.
o Sample data, including tabulated results of the organic TCL (HSL)
compounds identified and quantified, and the tentative identification
and estimated concentration of up to 30 non-TCL (HSL) organic
IS
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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, including chromatograms, spectra and data
system printouts amd initial and continuing calibration reports.
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 B.
4. Analytical Protocols
The standardized organic analytical methods are based on Federal Register
(FR) Methods 625 (B/N/A), 608 (pesticide), and 624 (VOA) modified for CLP
use in the analysis of both water and soil samples. Analysis for the organic
HSL compounds includes an optional GC screen (to determine appropriate
dilution fraction or aliquote sizes for GC/MS analysis) and GC/MS analysis.
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: semivolatile (B/N/A);
volatile (VOA); and pesticide/PCB. Extracts are cleaned up when
necessary, using optional column chromatography techniques.
The identification and quantification of the organic TCL (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 fraction.
In addition, the 20 highest non-TCL (HSL) base/neutral/acid compound
peaks and the 10 highest non-TCL (HSL) volatile peaks are tentatively
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identified and their concentrations estimated, using a forward search of
the NBS Mass Spectral Library.
Soil Method
Soil samples for full organic analysis (base/neutral/acid and pesti-
cide/PCB compounds) are prepared by sonification prior to solvent
extraction. Extracts are cleaned up using optional column chromato-
graphy techniques when necessary.
The identification and quantification of the organic TCL (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.
In addition, the 20 highest non-TCL (HSL) base/neutral/acid peaks
and the 10 highest non-TCL (HSL) volatile peaks are tentatively
identified and their concentrations estimated, using a forward search
of the NBS Mass Spectral Library.
Contract Required Quantitation Limits (CRQLs)
Low level analysis contract required quantitation limits for water
samples are based on CRQLs for each organic compound using FR
Methods 624, 625, and 608 and are at the part-per-billion (ppb) level.
Approximate achievable sample quantitation levels for low and
medium level water and soil samples can be calculated based on the
sample size and on concentration/dilution factors.
CRQLs are provided for analytical guidance, as the limits are highly
matrix dependent. Matrix interferences vary considerably depending
on the nature and homogeneity of the sample, on the interferent
contaminants which coextract from the sample, and on the sample
volume taken for analysis.
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5. Contract Quality Control Requirements
The CLP. quality control (QC) program for organic RAS laboratory analysis
is structured to provide consistent results of known and documented
quality. The program, therefore, places stringent quality control require--
ments on all laboratories performing sample analyses. 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 applica-
bility to each sampling effort. 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 organic RAS program consist of both
an initial and ongoing demonstration of laboratory capability to generate
acceptable performance with the contract methods in the 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.
Instrument QC procedure:
o GC/MS instrument tunes for both volatile and semi-volatile compound
analyses.
o Initial multi-level calibration for each TCL (HSL) compound,
o Continuing calibration for each TCL (HSL) compound.
Sample QC procedure:
o Addition of surrogate compounds to each sample and blank for
determining percent recovery information.
o Duplicate matrix spike analyses.
o Method blank analyses.
Certain QC procedures listed above demonstrate that the instrument is
operating within contract specifications. These include:
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o A demonstration that the two tuning compounds (DFTPP for
extractables and BFB for volatiles) meet the defined ion abundance
criteria.
o 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.
o 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:
o 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.
o Analysis of duplicate matrix spiked samples to display the precision of
the method for the particular matrix and also to provide percent
recovery information for defined TCL (HSL) compounds (specified
matrix spikes) as for surrogates.
o 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 must be re-
analyzed by the laboratory if sufficient sample volume is available.
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B. Inorganic Routine Analytical Services (RAS)
1. Sample Matrices, Concentration Levels, Volumes Required and
Preservation 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 an appropriate matrix. Sample matrices other than
water, sediment or soil are processed through the SAS program.
Inorganic RAS contract methods determine concentrations of inorganic
priority pollutant constituents ranging from low 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 priority pollutant (PP) contaminants. Medium level samples
are most often those collected on-site, in areas of moderate dilution by
normal environmental processes. Medium level samples are estimated to
contain concentrations 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 any PP contaminant higher than 15 percent of the sample
must be sent through High Concentration SAS for sample preparation and
analysis.
The sample volume, container types, and preservations required for inor-
ganic 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, 1 liter volume is required for metals analysis and 1
liter volume is required for cyanide analysis. These samples should each be
collected in a 1-liter polyethylene bottle. For RAS inorganic analysis of a
water sample estimated as medium level, 16 ounce volume is required for
metals and 16 ounce volume for cyanide. These samples should each be
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collected in a 16-ounce glass jar. For RAS inorganic analysis of a soil
sample estimated as low or medium level, 6 ounce sample volume is
required for both metals and cyanide analyses. These samples should each
be collected in an S-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.
The standard procedure applied by the analytical laboratory for
homogenization is to shake the sample in its original sample container and
transfer 100 mL aliquots to a 250 mL beaker. For aqueous samples with
high solids content, the user has the option to specify that the sample not
be mixed and the analysis be performed on the supernatant. When
collecting low level water samples, different preservation techniques apply
to the metals and cyanide portions, as follows. For "total" metals analyses,
the sample is acidified to pH < 2 with HN03. (Total meaning inclusion of
particulate and dissolved fractions.) For dissolved metals analyses, the
sample is filtered, then acidified to pH < 2 with HN03. Note of caution:
if the sample contains a significant particulate fraction, acidification
without filtration could result in deceptively high metal values for the
water sample. Varying amounts of particulate matter can also give large
differences in metal values for duplicate acidified water samples.
For the cyanide aliquot, the following guidelines should be followed:
o Test a drop of sample with potassium iodide-starch test paper (KI-
starch paper); a blue color indicates the presence of oxidizing agents
and the need for treatment. Add ascorbic acid, a few crystals at a
time, until a drop of sample produces no color on the indicator paper.
Then add an additional 0.6g of ascorbic acid for each liter of sample
volume.
o Test a drop of sample on lead acetate paper previously moistened
with acetic acid buffer solution. Darkening of the paper indicates
2- 2-
the presence of S . If S is present, add powdered cadmium
carbonate until a drop of the treated solution does not darken the
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lead acetate test paper and the filter the solution before raising the
pH for stabilization.
o Preserve samples with 2 ml of 10 N sodium hydroxide per liter of
sample (pH >_ 12).
o Store the samples such that their temperature is maintained at 4°C
until the time of analysis.
No chemical preservation is required for medium level water samples or
low or medium soil samples.
For soil samples the standard procedure applied by the analytical
laboratory for homogenization is to thoroughly mix the contents of the
sample container. For solid samples with significant amounts of water, the
user has the option to specify that the supernatant be decanted and the
remaining sample be mixed thoroughly and analyzed.
Each sample estimated as medium level (water or 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. Soil blanks are currently not available. It is
recommended that the user not submit soil field blanks for analysis. If the
user submits a rinsate blank with a case of soil samples, it will be treated
as a separate aqueous matrix sample with full QC and accordingly, a
sufficient volume for analysis should be provided to the laboratory. When a
suitable soil blank material becomes available through EMSL, one soil blank
will be supplied for each Case. No additional volume is required for
duplicate analyses of either water or soil samples.
The user may specify that the duplicate and matrix spike be performed on
a particular sample. If sufficient sample volume is not provided, analysis
of all required parameters and/or complete QA/QC determination may not
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be possible. If this occurs, SMO will contact the RSCC to determine
appropriate adjustments 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 Repositories, 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 or 35 days (as specified by the contract delivery
schedule) following sample receipt at the laboratory. Laboratories 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 provides a complete set of data for
independent 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 page, 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; including a brief description of the sample.
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o Individual analytical results are flagged by the laboratory when QC
indicates potential bias due to matrix effects, homogeneity, etc.
o QC results for: preparation blanks, calibration blanks, calibration
verification standards, matrix spikes, duplicates, laboratory control
samples, interference check samples, analytical spikes and serial
dilution analyses.
o Tabulation of instrument detection limits determined in pure water
solutions.
o Digestion/distillation logs, sample traffic reports, and raw data
system printouts identifying calibration standards, calibration 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.
k. 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-846),
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.
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For water samples, a quantitative determination for cyanide is made
by midi-distillation and colorimetric analysis or by titration.
Mercury is quantitated in water samples by the cold vapor technique.
Soil/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. Mercury is
quantitated in soil/sediment samples by the cold vapor technique.
Contract Required Detection Limits (CRDLs)
Exhibit C of the Statement of Work of inorganics IFB contracts
contains minimum contract-required detection levels (CRDLs) that
must be met by all laboratories for each of the metals and cyanide in
pure water. On a quarterly basis, the contract laboratories are
required to verify that their instrument detection limits (IDL) meet
the CR.DL's.
The instrument detection limits reported by the laboratory on the
inorganic data sheets (see Appendix B Form I) are based on analysis
of analytes in pure water. Detection limits for the sample analyses
may 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
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considerably depending on the nature and homogeneity of the sample,
interferent contaminants that coextract from the sample, and by the
analytical method. Lowest detection limits are achieved on low level
water samples in the ppb range, where sample matrix interferences
are minimal.
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" IDL, results
below the CRDL should be used with caution. Results below the
CRDL are bracketed by the laboratory to indicate a value near the
instrument detection limit.
5. Contract Quality Control Requirements
The CLP quality control (QC) program for inorganic RAS laboratory
analysis is structured to provide consistent results of known and docu-
mented 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 applic-
ability 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 performance with the contract methods in the analysis
of water and soil samples. CLP contracts define extensive QA procedures
that must be performed and documented, and criteria that must be met.
These include, but are not limited to, the following:
o Initial calibration and calibration verification (ICV).
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o Continuing calibration verification (CCV).
o ICP interference check sample (ICS) analysis,
o ICP serial dilution analysis,
o Preparation blank (PB) analysis,
o Spiked sample analysis,
o Duplicate sample analysis,
o Furnace A A QC analysis,
o Laboratory control sample (LCS) analysis.
The instrument QC operations include initial and continuing calibration
checks, which are performed daily and/or every 10 samples. These checks
determine that the analytical system is meeting contract-required criteria.
Analytical QC operations include:
o ICP Interference Check Sample Analyses: Performed at least twice per
eight-hour shift, to verify interelement and background correction
factors.
o Preparation Blank Analyses: Performed for each batch of samples or for
each set of 20 samples, to ascertain whether sample concentrations
reflect contamination.
o Spiked Sample Analyses and Duplicate Sample Analyses: Performed for
each concentration and matrix within 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.
o Serial Dilution Analyses: Performed for each group of samples of a
similar matrix type and concentration for each Case of samples, or for
each 20 samples received (whichever is more frequent) to ascertain
whether significant chemical or physical interferences exist due to
sample matrix.
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o Furnace AA QC Analysis: Required for quantitation; incorporates
duplicate injections and analytical spikes in order to evaluate the
precision and accuracy of the individual analytical determinations on
each sample.
o Laboratory Control Samples (LCS): Standards carried through sample
preparation and analysis procedures to document the performance of
the entire analytical process. The results for analysis of LCS are
submitted with the data package. Laboratories on a quarterly basis
verify their instrument detection limits, ICP linear ranges, ICP
interelement correction factors and ICP integration times.
It is the responsibility of the contractor laboratory to document, in each
data package submitted, that both initial and ongoing instrument and
analytical QC requirements have been met. Any samples analyzed when
contract QC requirements have not been met are re-analyzed by the
laboratory.
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Dioxin Routine Analytical Services (RAS)
1. Sample Matrix and Volume Required
The dioxin RAS contract method applies to analysis of soil/sediment and
water samples. Soil/sediment and water amples for analysis should be
single-phase, homogeneous and of a similar matrix. Sample matrices other
than soil/sediment or water 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 and water samples. No
concentration levels are designated in the dioxin program. All samples
suspected to contain dioxin are considered hazardous and handled accord-
ingly.
The sample volume required to perform RAS dioxin analysis is four ounces
of soil/sediment or 2 liters of water. Each soil sample should be collected
in either one 4-ounce glass jar or one 8-ounce glass jar filled one-half full.
Each water sample should be collected in 2, 1-liter amber glass bottles.
The collection of more than the required 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 (24 or
fewer samples). The sampler must designate one field blank for fortified
matrix spike analysis and one field sample for duplicate analysis. A rinsate
sample, consisting of trichloroethylene used in rinsing sampling equipment,
may be included in a batch. (Rinsates are the only liquid samples analyzed
in the dioxin RAS program.) The sample volumes indicated are sufficient
for duplicate analysis; no additional volume should be collected.
Per program procedures, a QA sample should be included and identified 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 and water samples are illustrated in Appendix C. Pre-
cleaned sample bottles are available through the Sample Bottle Reposi-
tories, as detailed in Chapter IV.
2. Isomer Identified and Quantified
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 and water
samples.
3. Contract Deliverable Requirements
The dioxin RAS program specifies: completion of sample extraction,
clean-up analysis, and data reporting within 21 days following sample
receipt at the laboratory, including automatic re-extraction and re-analysis
of samples where certain criteria are not met in the initial analysis.
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 read-
able versions of the illegible pages.
The dioxin RAS data package provides a complete set of data for
independent 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 all rejected
sample runs.
o Results of analyses of multi-level concentration calibration solutions,
including SICPs, calculated response factors, and computer-generated
quantitation reports.
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o SICPs generated during each performance check solution analysis and
each concentration calibration solution analysis.
o Chronological list of all analyses performed.
A summary of RAS dioxin data deliverables and copies of data reporting
forms are contained in Appendix B.
4. 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
and water samples. Analyses are performed on a "batch" basis. A
sample batch consists of a shipment of 20 to 2k field samples, and
normally includes an equipment rinse solvent (trichloroethylene)
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 chromatographic and other cleanup procedures are
applied to eliminate sample components that may interfere with
detection and quantification of the 2,3,7,8-TCDD isomer.
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.
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b. Contract Required Quantitation Limits (CRQLs)
The RAS contract method provides procedures for the detection and
measurement of 2,3,7,8-TCDD in soil/sediment and water samples at
concentrations as low as 1 ug/kg (equivalent to 1 ppb). Column
chromatography and other clean-up 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 CRQLs 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. Sam-
ple 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 performance within the contract methods for the analysis of
soil/sediment samples for 2,3,7,8-TCDD. 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 Initial and continuing calibration and instrument performance checks.
o Reagent blank analysis.
o Field blank analysis.
o Fortified matrix spike analysis (2,3,7,8-TCDD spiked field blank),
o Rinsate (equipment solvent) sample analysis,
o Duplicate sample analysis.
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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 checks. Continued calibration is performed at the
beginning of each 12-hour shift. Performance checks are performed at least
twice during each 12-hour shift to demonstrate continued acceptable GC/MS
resolution, sensitivity, response factor reproducibility, mass range
calibration, and to validate sample data.
Analytical QC operations include: reagent blank, field blank, spiked field
blank, rinsate, and duplicate sample. Reagent blank analyses are per-
formed by the laboratory prior to and during analysis of each batch, to
demonstrate that identified compound concentrations do not reflect
laboratory contamination. Field blank analyses are performed on one
fortified (native matrix spike) and other unfortified samples of uncon-
taminated soil/sediment or water 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.
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 and duplicate
recoveries falling 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.)
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Special Analytical Services (SAS)
In addition to the standardized analyses provided under the Routine Analytical
Services (RAS) program, the CLP's Special Analytical Services (SAS) program
provides clients with limited customized or specialized analyses, different from
or beyond the scope of the RAS IFB 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-TCL (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 timeframe. Individual SAS subcontracts are
solicited, awarded and administered by Viar and Company, as part of the
company's 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's capabilities
from standardized RAS organic, inorganic and dioxin contract analyses, to
include a wide variety of additional, non-routine analytical services.
The client requestor provides SMO with the analytical methods and QA/QC
requirements needed for each SAS. SMO procures SAS by subcontracting with
CLP RAS laboratories or, when RAS laboratories cannot meet the analytical
requirement of the SAS, with other laboratories which have demonstrated the
ability to meet program performance requirements. RAS contract laboratories
are evaluated for current RAS performance before they are considered for SAS
solicitations, and are not solicited for SAS work if deficient in this area. SAS
organic, inorganic, dioxin and high concentration analysis requests are solicited
to CLP laboratories with IFB contracts in the appropriate analytical program,
and that are performing in accordance with 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.
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Once the laboratory universe is determined, SMO initiates solicitation via
telephone, contacting a minimum of three laboratories (contingent upon avail-
ability of a particular analytical service) and describing the requirements.
Laboratories are asked to bid firm, fixed price(s) 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's ability to bid for SAS work and the prices being bid may 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 may
not be able to accommodate all SAS requests received. Currently, SAS services
are provided on a first-come basis; however, Agency requirements can necessi-
tate that certain work be given priority. In this event, SMO notifies the involved
RSCC Primary Authorized Requestors, who determine Regional sampling priori-
ties.
An analysis request can be processed through SAS only if the types of samples to
be analyzed or the analysis requirements are different from 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 contract award. Analytical services
available through the SAS program are described in the following sections.
Pre-cleaned sample bottles are available through the Sample Bottle Repositories,
as detailed in Chapter IV. These bottles are prepared specifically for RAS
analytical work; however, bottles may be utilized in SAS projects as appropriate.
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1. SAS Services
a. RAS Plus SAS
(1) Fast Turnaround
A fast turnaround request is a request for routine (RAS)
analyses with extraction, analysis or data delivery required in a
shorter timeframe 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 organics,
inorganics and dioxin IFBs, reference Part 3 of Sections A - C
of this chapter.
In 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 of 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.
The following illustrates common "RAS Plus SAS" fast turn-
around requests, with the SAS portion underlined:
o TCL (HSL) volatile organic compound analysis with VOA
analysis and data delivery in 5 days.
o IFB inorganic compound analysis with data turnaround in
10 days.
o IFB dioxin compound analysis with data turnaround in 5
days.
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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 Target Compound List - TCL
(equivalent to Hazardous Substances List - HSL) organic
analysis requirements constitutes this type of SAS request. The
following examples illustrate common "RAS Plus SAS" organic
requests, with the SAS portion underlined:
o TCL (HSL) volatile compound analysis at lower detection
limits than required by the IFB.
o TCL (HSL) full organic analysis with additional non-TCL
(HSL) pesticide/herbicide compounds.
o TCL (HSL) pesticide compound analyses with minor
alterations or additional procedures applied.
o TCL (HSL) B/N/A compound extraction with analysis by a
non-TCL (HSL) method.
(3) Inorganic — Special Requirements in Addition to RAS
As with organics, 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 non-IFB parameters —
nitrate, sulfate, ammonia, sulfide, total organic carbon
and chloride.
o Metals and cyanide analyses with rigorous sample homo-
genization.
o Metals analysis at lower detection limits than required by
the IFB.
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o
Metals and cyanide analysis with minor alterations or
additional procedures applied.
(4) 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 RAS plus SAS request. The following examples illustrate
"RAS Plus SAS" dioxin requests, with the SAS portion under-
lined:
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 or
furan isomers.
b. All 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 SAS-
contracting process referred to as "All SAS." Five categories of "All
SAS" requests are described in the following sections.
(1) Organic — Special Requirements Not Provided by RAS
o Seven TCL (HSL) PCB arochlors analysis only (i.e., not the
entire IFB pesticide fraction).
o Non-TCL (HSL) compound analysis.
o Organic extraction of non-aqueous and non-soil/sediment
samples (e.g., oil, tar or biological tissue samples by a
non-IFB extraction procedure).
o Organic analysis by non-RAS methods.
k 1
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(2) Inorganic — Special Requirements Not Provided by RAS
o Specified IFB element analysis only (e.g., cadmium, mer-
cury and selenium).
o Non-IFB parameter analysis (e.g., total organic carbon,
Sulfate, TSS).
o EP Toxicity tests (metals, pesticides or herbicides).
o Any inorganic preparation/analysis of non-aqueous and
non-soil/sediment samples (e.g., oil, tar or biological
tissue) by a non-IFB procedure.
o Metals analysis by non-RAS methods.
(3) Dioxin — Special Requirements Not Provided by RAS
o 2,3.7.S-TCDD in fish tissue (e.g., matrix other than
soil/sediment).
o 2,3,7,8-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.
(4) High Concentration Sample Analysis — Organic and Inorganic
The SAS program provides for extraction and analysis of High
Concentration (HC) samples. HC sample analysis will
eventually be implemented under the RAS program. HC
analysis services are described below.
o Organic extraction and analysis for TCL (HSL) compounds
by GC/MS with tentative identification of 30 non-TCL
(HSL) compounds of greatest concentration.
o Inorganic preparation/analysis for total metals and total
mercury.
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(5)
Special Topics Analysis
The SA5 program can also accommodate unusual analytical
requests on an "All SAS" basis, when sufficient lead time is
allowed and complete methodology and QA/QC specifications
accompany 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/evaluation studies.
o Asbestos analysis.
o Acid deposition parameters.
o Non-Superfund analytical services of any type.
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 may use RAS
contract deliverable requirements as a guide, but must be specified by the
client at the time of request. The requestor should specify all deliverables
required, to ensure that appropriate data packages are received.
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 as specified in RAS program contracts, may be used as a
guide but must be 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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CHAPTER HI
UTILIZATION OF ANALYTICAL SERVICES
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CHAPTER ffl
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 specific
procedures and required documentation for each program and to provide complete,
step-by-step information on how to properly access the CLP'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 schedul-
ing 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 utiliza-
tion, 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 or Waste Management 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 organic allocation system, as described in the following
section. The Primary AR determines analytical priorities for the Region when
conflicts occur.
Individuals interested in obtaining CLP analytical support are instructed to contact
their Regional EPA office's Regional Sample Control Center (see Appendix A).
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A. Analysis Initiation/Request Procedures
1. RAS Initiation Process
a. User Information Required
To initiate a RAS request, the RSCC Authorized Requestor contacts
the appropriate SMO Coordinator by telephone and provides a com-
plete 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 Name(s), association, and telephone number(s) of sampling
personnel.
o Name, city and state of the site to be sampled,
o Super fund site/spill ID (2 digit alpha-numeric code),
o Dioxin tier assignment, where applicable,
o Number and matrix of samples to be collected,
o Type of analyses required.
Organics: full (VOA, B/N/A and pesticides/PCB) or VOA
and/or B/N/A and/or pesticides/PCB.
Inorganic: metals and/or cyanide.
Dioxin: 2,3,7,8-TCDD.
o Scheduled sample collection and shipment dates.
o Nature of sampling event (i.e., investigation, .monitoring,
enforcement, remedial, drilling project, Cercla Cooperative
Agreements).
o Suspected hazards associated with the sample and/or site.
o Other pertinent information which may affect sample
scheduling or shipment (i.e., anticipated delays due to site
access, weather conditions, sampling equipment).
o Name(s) of Regional or contractor contacts for immediate
problem resolution.
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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.
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.
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. In
order to facilitate laboratory scheduling and resolution of questions
concerning sampling and analysis procedures, and to allow the sam-
pler adequate time to prepare the required sample documentation,
the RSCC is required to provide scheduling information by noon on
Wednesday of the week prior to sample shipment. Advance
scheduling is available and should be utilized whenever possible.
Case Number Assignment and Laboratory Scheduling
At the time of request, SMO assigns a sequential dase 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
collected at one site or geographical location during a predetermined
and finite tir
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analyses, number of samples, program contract capacity, sample
balance among the various laboratories, and laboratory loading and
instrument conditions. Organic laboratory selection is also based on
the Regional Distribution of Laboratories System developed by the
NPO, designed to minimize the number of laboratories producing data
for any one Region. When possible, the nearest available laboratory
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
samplings effort, to follow up with SMO in finalizing sampling
requirements, initiating changes, and coordinating sample shipment.
d. User Knowledge of Analytical Protocol
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 Regional DPO 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.
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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. The analytical SOWs contain specific information on sample
types suited to RAS analysis, compounds identified and quantified,
analytical methods, protocols, detection limits, deliverable
requirements, and quality control requirements. Analytical
requirements differing from these RAS parameters are processed
through the SAS program, as described in Chapter II, Section E.
2. SAS Initiation Process
a. User Information Required
To initiate a SAS request, the RSCC Authorized Requestor contacts
the appropriate SMO Coordinator by telephone and provides a com-
plete 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 number(s) of sampling
personnel.
o Name, city and state of the site to be sampled.
o Superfund site/spill ID (2 digit alpha-numeric code).
o Number and matrix of samples to be collected.
o Specific analyses required and appropriate protocols and
QA/QC.
o Required detection limits.
o Matrix spike and duplicate frequency.
o Data turnaround and data format.
o Justification for fast turnaround request, if appropriate.
o Scheduled sample collection and shipment da+es.
o Nature of sampling event (i.e., investigation, monitoring,
enforcement, remedial, drilling project, Cercla Cooperative
Agreements).
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o Suspected hazards associated with the samples and/or site.
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.
In 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 size and extent of the
miscalculation, 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 two weeks is required to process a
completely defined SAS request. More lead-time is strongly recom-
mended whenever possible. SAS solicitation will not be started until
the SAS requirements have been completely defined by the AR.
Modifications to any SAS request will cause the entire process to
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begin again. Fully-defined requests initiated with less than two
weeks, lead-time may not be solicited and awarded in time to meet
the original shipment date.
Certain types of SAS requests require a longer lead-time, as follows.
A minimum lead-time of two to three weeks is required for SAS
requests which involve distribution of protocols (reference item d.,
this section). A minimum lead-time of four or more weeks is
recommended for large-scale, analytically complex and/or non-
Superfund SAS requests. Award of non-Superfund SAS subcontracts
may only be made after the appropriate funding process is complete.
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 pro-
grams. The AR should contact SMO several weeks in advance, if
there is a question regarding the advance time needed to schedule a
particular SAS request.
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 both case and SAS numbers in
referencing the request throughout sampling and analysis. Like the
Case identification, 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.
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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 perform-
ing 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
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 additional time for resolicitation 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 QC procedures to be
utilized for each SAS request. Before SMO can commence a SAS
solicitation, the analytical methodology and QC requirements to be
applied under the 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 to three weeks in
advance of scheduled sample shipment under the SAS. This additional
lead-time is required for protocol distribution and review by solicited
laboratories.
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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 to
three weeks in advance of sample shipment, to allow time for
protocol distribution and review by solicited laboratories.
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.
3. Procedures for Making Changes to Analytical Requests
The RSCC Authorized Requestor is responsible for immediately notifying
the appropriate SMO Coordinator 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 Coordinator of any
changes in sampling before and during the on-site sampling event and after
shipment of samples to laboratories.
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Failure to notify SMO of such changes can result in: delay in sampling to
accommodate scheduling changes, delay in start of analysis due to con-
flicts, unsuitability of a particular sample to an analytical program, and/or
analysis data inappropriate for client purposes.
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B. Regional Organic Allocation System
An allocation system has been established by the NPO to equitably apportion
available organic laboratory capacity to the Regions during periods of heavy
sampling activity when analysis capacity for all requests may not be available.
Currently, capacity is available for the projected sample demand; however, when
the allocation system is in effect, all organics RAS and RAS plus SAS Cases will
be scheduled accordingly.
During the last month of each quarter (fiscal year), the NPO provides the RSCC
with the Region's monthly allocation of organic sample analyses for the following
quarter. The RSCC is responsible for planning the month's sampling activities in
accordance with the NPO allocation.
Under the allocation system, each Wednesday preceding the week that samples
are expected to be shipped, the RSCC requests sample analyses for all planned
Regional sampling activities for that week, assigning a priority to each activity
requested. (Analysis request procedures are delineated in the following sections
of this chapter.)
Upon receiving the Region's sampling requests, SMO makes laboratory assign-
ments for the week, scheduling requests received up to each Region's 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 week is determined. The NPO then prioritizes Regional sampling
requests which exceed allocations, on a national basis. Following NPO prioriti-
zation, 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's
Group Leader for Analytical Services (see Appendix A).
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Sample Documentation
Each sample processed by the CLP must be properly documented to ensure
timely, correct and complete analysis for 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)/Usage, Distribution, Ordering
The sample documentation system for the RAS organic and inorganic
programs is based on the use of the EPA 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 two types of TRs currently in use
are Organic and Inorganic. Copies of the two types of TRs are included in
Appendix B, along with examples of properly completed TR forms. (High
Concentration TRs are used when HC preparation and analysis is performed
through the RAS plus SAS mechanism and will be used for -the RAS HC
Program when it is implemented.)
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 and site/spill ID, analysis laboratory, sampling office,
dates of sample collection and shipment, and sample concentration and
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matrix. Numbers of sample containers and volumes are entered by the
sampler beside the analytical parameter(s) requested for particular sample
portions.
After 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 analytical
laboratory documents sample condition and signs the TR, returning the
signed copy to SMO and keeping a laboratory file copy. Copies of the
laboratory-signed TRs are provided to the RSCC as part of the data
package.
A strip of adhesive sample labels printed with the TR sample number come
attached to the TR for the sampler's 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.
When a RAS sample is to be analyzed for RAS with SAS treatment
(described in Chapter II as "RAS Plus SAS" request), TR forms are used for
the "RAS Plus SAS" samples. A SAS Packing List is not required in
addition to the TR. 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. Caution
is to be taken not to include the Case Number on "All SAS" samples taken
at the same site. 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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2. Dioxin Shipment Record (DSR)/Usage, Distribution, Ordering
Sample documentation for the RAS dioxin program utilizes the CLP Dioxin
Shipment Record, a four-part carbonless form. The DSR provides a record
for one shipment batch of dioxin samples (up to 2k 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 informa-
tion (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's 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,
labels 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.
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Dioxin 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.
3. SAS Packing List (PL)/Usage, Distribution, Ordering
Only for "All SAS" samples (as described in Chapter II), are samplers to
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., 2000E-1, 2000E-2, 2000E-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. Regions/samplers should consult SMO to verify that
the PL is appropriate to use in their situation.
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's 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.
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 the effects of water and solvent(s). The sample
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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.
4. 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 waste site 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.
The information recorded on an EPA sample tag includes:
o CLP Case/SAS No(s). — The unique number(s) assigned by SMO to
identify the sampling event. (Entered under "Remarks" heading.)
o CLP Sample No. — The unique sample identification number (from
the TR, DSR 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-digit number indicating the month, day and year of
collection.
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o Time — A four-digit number indicating the military time of col-
lection.
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 pre-printed 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.
' Each sample tag is completed and securely attached to the sample
container. Samples are then shipped under chain-of-custody procedures as
described ih the following section.
5. 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 (i.e., Traffic Report, Dioxin Shipment
Record and SAS Packing List) for all 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; or it was in your possession and then locked up or sealed to
prevent tampering; or it is in a secured 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
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or dispatched properly. In 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 cooler shipped 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 num-
ber, samplers' signatures and the CLP Case/SAS number (entered on the
upper right of the form). Do not include the commonly known name of the
site, as CLP laboratories may perform work for the responsible party of
that site. For each station number, the sampler indicates: date, time,
whether the sample is a composite or grab, station location, number of
containers, analytical parameters, CLP sample number(s) (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 Chain-of-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
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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 labora-
tory's responsibility to maintain internal log books and records that provide
a custody record throughout sample preparation and analysis.
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Sample Packaging and Shipment
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 must 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.
Inside the cooler, sample containers must be enclosed in clear plastic bags
through which sample tags and labels are visible. Dioxin samples as well as
water and soil samples suspected to be of medium or high concentration or
those suspected to contain dioxin must be enclosed in a metal can with a
clipped or sealable 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.
Water samples for low or medium level organics analysis and low
level inorganics analysis must be shipped cooled to 4°c with ice. No ice
is to be used in shipping: inorganic low level soil samples or
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medium/high level water samples; or organic high level water or soil
samples; or dioxin samples. Ice is not required in shipping soil samples, but
may be utilized at the option of the sampler. All cyanide samples;
however, must be shipped cooled to 4°C.
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, labeled sample bottles (or labeled 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. Ice should be in sealed plastic bags to prevent melting ice from
soaking packing material which, when soaked, makes handling of samples
difficult in the lab.
Unless otherwise instructed through SMO in advance, the laboratory
disposes of unused sample volume, sample bottles and packing materials 60
days following data submission.
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
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inorganic program, three days is the recommended period for collection of
a Case of samples.
All samples should be shipped through a reliable commercial carrier, such
as Federal Express, Emery, Purolator, 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
EPA-approved sample packaging and shipment techniques. In addition,
general questions concerning sample packaging and shipment may be
directed to SMO.
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 of all sample shipments on the day of shipment. At that
time, the sampler should provide the following information:
o Sampler name and phone number,
o Case Number and/or 5AS Number of the project,
o Site name/code,
o Batch numbers (dioxin only)
o Exact number(s), matrix(ces) and concentration(s) of samples
shipped.
o Laboratory(ies) sainples were shipped to.
o Carrier name and airbill number(s) for the shipment,
o Method of shipment (e.g., overnight, two-day),
o Date of shipment.
o Suspected hazards associated with the samples or site.
o Any irregularities or anticipated problems with the samples,
including special handling instructions, or deviations from estab-
lished sampling procedures.
o Status of the sampling project (e.g., final shipment, update of
future shipping schedule).
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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 information has 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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E. Procedures for Problem Resolution
1. 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 for
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 deliverables 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 Project Officer 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's 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
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
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permanent part of the Case/SAS 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
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CHAPTER IV
AUXILIARY SUPPORT SERVICES
In addition to the 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 Containers Available
Under the Sample Bottle Repository operation, ten types of sample
containers are available to CLP clients for use in hazardous waste sampling
activities of the Superfund Program. Containers provided through this
i
program are precleaned and QC-tested according to prescribed procedures
to ensure that no contamination exists that might affect sample data
results. (Sample coolers and sample preserving agents are not supplied
through the Repository program.)
The following chart lists the types of containers provided, the number of
containers per carton, and the type(s) of samples appropriate for collection
in each container type. Each container type is cleaned and QC tested by
procedures directly related to the specific analyses that may be performed
on samples collected in the container. Therefore, to ensure appropriate
quality control, users are instructed to utilize containers only to collect
sample types as listed on the following chart.
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2. Ordering Procedures
The Sample Bottle Repository program may be used by any organization
scheduling Superfund sample analysis 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 container requests
through the program. State personnel should access the program through
their EPA Regional office.
Users should contact SMO initially to become authorized to order from a
Repository and to obtain a supply of Delivery Request forms. Thereafter,
the RAR requests containers directly from the Repository. Since the
Repository can respond only to requests submitted by a SMO-designated
RAR, users must promptly notify SMO of any change in RAR designations.
There are three types of container requests, defined by the amount of time
between the date the order is placed and the requested delivery date:
o Routine Request — Fifteen or more working days lead-time
for delivery.
o Fast-Turnaround Request — More than three days, but less than
fifteen days lead-time for delivery.
o Emergency Request — Less than three days lead-time for de-
livery.
Routine requests are mailed to the appropriate Repository utilizing the
Delivery Request (DR), a three-part carbonless form. The DR must be
signed by an RAR. The top (original) copy of the completed DR is sent to
the Repository at the address indicated on the form, the second copy is
retained for the user's file, and the third copy is sent to SMO.
Fast-turnaround and emergency requests should be called in to the
appropriate Repository, at the telephone number provided on the form, and
the written Delivery Request distributed as outlined above, to confirm the
order. When placing a telephone order, the RAR must give the Repository
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SAMPLE BOTTLE REPOSITORY SERVICES
Container
Type
Description
80-oz amber glass bottle
with teflon-lined black
phenolic cap
No. Per
Carton
Used for RAS
Sample Type'
Extractable Organics
Low Concentration
Water Samples
B 40-ml glass vial 72
with teflon-lined silicon
septum and black
phenolic cap
C 1-liter high-density 42
polyethylene bottle
with white poly cap
D 120-ml wide mouth glass vial 72
with white poly cap
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
Volatile Organics
Low & Medium Concentration
Water Samples
Metals, Cyanide
Low Concentration
Water Samples
Volatile Organics
Low Medium Concentration
Soil Samples
Metals, Cyanide
Medium Concentration
Water Samples
Extractable Organics
Low & Medium Concentration
Soil Samples
- and -
Metals, Cyanide
Low & Medium Concentration
Soil Samples
- and -
Dioxin
Soil Samples.
- 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)
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SAMPLE BOTTLE REPOSITORY SERVICES (continued)
Container
TyPe
H
K
Description
k-oz wide mouth glass jar
with teflon-lined black
phenolic cap
1-liter amber glass bottle
with teflon-lined black
phenolic cap
32-oz wide mouth glass jar
with teflon-lined black
phenolic cap
4-liter amber glass bottle
with teflon-lined black
phenolic cap
No. Per
Carton
120
2k
36
Used for
Sample Type"
Extractable Organics
Low & Medium Concentration
Soil Samples
- and -
Metals, Cyanide
Low & Medium Concentration
Soil Samples
- and -
Dioxin
Soil Samples
- and -
Organic <5c Inorganic
High Concentration
Liquid & Solid Samples
Extractable Organics
Low Concentration
Water Samples
Extractable Organics
Medium Concentration
Water Samples
Extractable Organics
Low Concentration
Water Samples
'This column specifies the only type(s) of samples that should be collected in each
container.
7k
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the DR number for the request and provide the corresponding written DR
in follow-up.
Users should submit requests a minimum of two weeks in advance of the
required delivery date, whenever possible, to ensure timely and complete
delivery of containers. Emergency and fast-turnaround requests are filled
on an "as available" basis from the Repository's emergency inventory stock.
It may not be possible to respond to all emergency and fast-turnaround
requests, as response depends on Repository inventory and in-process
requests.
In the event that a request is cancelled, the user must immediately contact
the Repository to verbally cancel the request, 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 DR number.
3. Shipment Information
Upon receipt of the Delivery Request, Repository personnel schedule ship-
ment and begin preparing the request. Repository personnel immediately
notify the RAR if for any reason the request 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 requests 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 Center(s) in determining the priority of container requests
based on the Region's sampling needs.
Each carton in a Repository shipment is marked "Box of and a
Repository Packing List (PL) is included in Box 1 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
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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.
4. Procedures for Problem Resolution
a. Resolving Problems Concerning Container Shipment
If there are problems relating to shipment (i.e., 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 Container 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: descrip-
tion of the problem, rationale for suspecting container
contamination, supporting documentation (if available), and lot
number(s) for all containers concerned. Container lot numbers must
be provided before any corrective action can be taken. Prior to
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 tp
initiate appropriate follow-up action. Upon notification by SMO, the
Repository will first check the QC analysis record for the concerned
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iot(s) of containers and verify that contract procedures were cor-
rectly 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
container(s) 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
containers could be pulled before use in the field.
5. Summary of Container 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 container type are
determined, so that a container lot is not split between cases.) Containers
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 container lot is assigned a unique identifying number. This lot
number is permanently affixed to each container in the lot, recorded in the
Repository logbook, and entered on the shipment Packing List when
containers 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.
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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. If
a container fails to pass the QC check, the associated lot of containers is
pulled and reprocessed through the system.
A QC release number is assigned to each lot of containers that passes QC
analysis, and is marked on both the analysis and storage QC containers for
each lot. 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.
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 mpnitored for volatile
compounds. The QC storage containers are retained as a backup to
recheck for cleanliness, should possible contamination of a lot of bottles
come into questions at a later date.
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B. Information Services
1. Regional Sample List Report
Upon request, SMO distributes a Regional Sample List Report to the
Regional Deputy Project Officer (DPO). This computerized report provides
a summary of the Region's use of CLP resources during a specified period
of time. 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 deliverables
(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. An example of the Regional Sample List is contained
in Appendix D.
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 DPOs, Regional Sample Control Centers, and laboratories regard-
ing sample status, and responds to inquiries from concerned parties as
appropriate. A backlog report is sent twice monthly to DPOs and
laboratories listing each laboratory's samples and the number of days the
samples have been in-house.
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3. General Program Information
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 informa-
tion as appropriate.
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Enforcement Support
1. Generation of Enforcement Quality Data
One major objective of Superfund 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 uses
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 controlled and available for
litigation. The CLP, in cooperation with the EPA National Enforcement
Investigations 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 analytical 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 docu-
mentation 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 docu-
ment inventory.
Before a laboratory is awarded a CLP contract and continuing
periodically throughout the life of the contract, each laboratory
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facility is audited by NEIC to ensure compliance with these require-
ments. In 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 aire 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 within 80 days 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 to determine adherence to
procedure. A list of Case file purge materials is included in Appendix
D.
NEIC evidence audits may 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 is intended to identify all
evidence and sequence of events necessary to reconstruct the sample
history. The goal is to present to the case attorney a depiction of the
sample integrity. Examples of NEIC sample profiles for organic and
inorganic Cases are included 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. In 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/SAS number(s) of specific site sampling(s)
o Sample number(s)
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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.
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Cost Recovery Substantiation
The CLP prqvides documentation concerning program analytical costs to the
EPA's Office of Waste Programs Enforcement (OWPE) in support of Superfund
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 docu-
mentation 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 docu-
mentation 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.
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.)
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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
OWPE's 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. Information on how sample
management costs are computed is included.
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
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contract status; and lists total contract costs on SAS and laboratory
bases.
o Copies of all SAS-Related Cancelled Checks and Laboratory Invoices —
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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E. Contract Compliance Screening
SMO performs Contract Compliance Screening (CCS) on all RAS data produced
by the CLP. Modified CCS can also be performed on a case-by-case basis on
mixed RAS-plus-SAS or All-SAS data.
CCS is a structured review which determines completeness of data deliverables
and compliance of QA/QC parameters with contract specifications. Primary
objectives of CCS are:
o To resolve identified discrepancies in a timely manner,
o To form the basis for the recommendation for payment made by the PO.
Structurally similar CCS procedures are applied to organics, inorganics and
dioxin data. CCS results are produced on a fast-turnaround (15 day) basis and
identify compliance discrepancies by code, criterion, fraction and sample.
Results are distributed to the relevant laboratory and Region and to EMSL/LV.
A reconciliation process deals with responses to CCS results. Data which meet
all CCS criteria at initial receipt are recommended for 100% payment of the
amount due. Data with CCS defects have some payment recommendation
withheld, either temporarily or permanently, depending on the nature and extent
of the defect identified.
CCS results are accumulated in the CCS Database in order to produce routine
and on-demand summaries of laboratory performance and of compliance trends.
Examples of CCS result forms are included in Appendix D.
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F. Data Review Services
A full range of review services are used to assess CLP data. Objectives of the
review services are:
o To determine the usability and limitations of data given particular field or
policy assessment criteria.
o To maximize the amount of usable data by identifying critical properties of
data and by resolving or proposing solutions to analytical or quality control
problems.
o To provide systematic and standardized data quality assessment and status
summary to determine method, laboratory, and program performance.
These review services are performed by a number of operations:
o Review for data usability is performed by Regional personnel and contractors
as a service for the clients for whom sampling and analyses have been
performed. Recommended review procedures have been standardized and
organized into functional guidelines for evaluating CLP data. EPA Data
Validation Work Groups have produced specific documents for review of
organic, inorganic and dioxin analyses.
o Comprehensive QA review is performed by EMSL/LV on specific data
packages. Review and assessment of some program-wide QA results is also
performed by EMSL/LV to evaluate method and laboratory performance, and
the quality of analytical data.
o Review of completeness and contract compliance of key criteria in CLP data
is performed by SMO on all RAS data. Completeness of all SAS data is also
determined. Results are used for payment recommendation purposes and also
to provide summary information on program status and performance.
o Under direction of the CLP management, EMSL/LV and/or SMO may perform
additional data review, to assess a problem Case or provide a second opinion
on usability.
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Regional client requests for Data Review Services should be directed to the Regional
Deputy Project Officer (DPO). For SMO review, a copy of the request should be
submitted to SMO (Attention: Data Review Team) and a copy should be provided to
the Regional Sample Control Center. In follow-up, the DPO must notify SMO that the
request is authorized. Alternatively, 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.
All requests should be placed using the SMO Data Review Request memorandum. An
example of this memorandum is provided in Appendix D. Copies are available from
SMO.
1. 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
0
Site name
o
Analytical laboratory name(s)
o
Number of samples
o
Sample list
0
Type(s) of review requested
0
Requested date for review completion
o
User name and contact
o
Intended use of data
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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.
2. Documentation Provided by CLP
An evaluation report, including a sample/result matrix, and 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 qualifi-
cations noted, or unacceptable. Reasons for the designation are 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 D.
The contents and format of reports for Problem Case, Applications and
Consulting Reviews are determined by the nature of the data problem(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 support-
ing 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 of 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 usable for Agency enforcement actions keyed to identification of pollu-
tant 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 three primary aspects of QA:
(1) field QA, which includes field sampling operations and QA project planning;
(2) laboratory QA, which is comprised of analytical method QC and external or
program QA; and (3) post-laboratory QA to review laboratory and method per-
formance and their impact on data quality.
Field operations include sampling activities performed by the EPA Regions and
National Remedial Action/Field Investigation Team {REM/FIT) 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 Assurance Program Plans and site-specific Quality
Assurance Project Plans. These plans include the consistent use of Agency-
specified analytical procedures, 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 techniques, and
specifies types of sample containers and required sample volumes for appropriate
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target analyses. Through its Sample Bottle Repository system, the CLP provides
Superfund samplers with the precleaned 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 docu-
mentation 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 labora-
tory facility evaluations, required submission of laboratory Standard Operating
Procedures (SOPs) for analytical operations and documentation, continuous
monitoring of lab performance by Headquarters POs and Regional DPOs, and a
multi-level data review process to evaluate the validity of the data product,
individual laboratory performance and methods performance.
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 laboratory 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 requir-
ements are discussed. Analysis or method QC is addressed for each analytical
program in Chapter II, which contains a description of contract analytical
methods arid QC requirements for each program. The following sections of this
chapter describe the program's external laboratory QA activities.
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B. Laboratory Selection Process
1. Prebid Conference
The CLP prebid conferences are requested and chaired by the National
Programs Office and are arranged by SMO to facilitate the invitation for
bid (IFB) process for all interested laboratories. During each conference,
the appropriate program officer will explain a particular aspect of the IFB.
Areas of review include: contracting aspects; pre-award information;
statement of work; and the role in the CLP of the Environmental
Monitoring Systems Laboratory, SMO and the National Enforcement
Investigations Center.
Whenever possible, a prebid conference is scheduled for each routine
analytical service IFB series. Prebid conferences are announced and
logistical information provided in the IFB. In addition, if time allows, the
conference is advertised in advance in Chemical and Engineering News.
Prebid conferences are generally, held three to four weeks prior to the bid
opening. The conferences are held at various U.S. cities.
2. Preaward PE Sample Analysis
The first criterion for laboratory selection is pre-award performance
evaluation (PE) sample analysis. For some solicitations prior to bid
opening, interested laboratories may request preaward PE samples through
the contracting officer and submit a deposit that is returned upon
completion of sample analyses and submission of the PE sample data
package. For other solicitations, PE samples will be available only after
bid opening and only to bidders determined by EPA to be in the competitive
range.
PE samples are prepared by EMSL/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
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sample data according to IFB requirements, within a specified time period,
usually 21 days. Bidders' PE sample data are evaluated, by NPO and
EMSL/LV personnel, in terms of compliance with contract requirements
and accuracy of determination of compounds at the levels 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.
Bid Price
The second criterion for laboratory selection is bid price. Following bid
opening, bid abstracts are reviewed and evaluated by EPA NPO and EPA
Procurement and Contracts Management Division (PCMD) 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.
Preaward Bid Confirmations
Preaward bid confirmations may include: 1) bidder analysis of PE samples
(discussed in 2, above), 2) bidder submission of Standard Operating
Procedures (SOPs), and 3) site evaluation of the bidder's facility performed
by EPA program management and PCMD personnel.
a. 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 labora-
tory 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.
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b. On-Site Laboratory Evaluation
EPA NPO, EMSL/LV, and NEIC personnel participate in on-site
evaluations of laboratory facilities of bidders which scored
acceptably on the PE sample analyses and are within the EPA
determined competitive range. EPA personnel perform a walk-
through of the facility and perform a thorough on-site evaluation.
The results of the on-site evaluation are considered in the final
determination of bidder responsiveness/responsibility for contract
award.
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Laboratory Start-Up Process
Laboratories entering the program undergo a learning curve process during which
they become fully familiarized and obtain expertise in application of program
methodologies and quality control procedures. To reduce the learning 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 Reference materials (SRMs) to the contractor, through the
Agency's contractor-operated QA Materials Bank. These SRMs are utilized
by the laboratory as the official standards to which laboratory supplied
standards must be traceable 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 labora-
tory 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 or DPO may visit the laboratory facility and
work on-site with laboratory personnel in rectifying problems. This process
also occurs on an ongoing basis during the life of the contract. On-site
laboratory evaluations are performed yearly by EPA staff, EMSL/LV,
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NEIC, and the PO and/or Deputy Project Officer (DPO), as well as on an
as-needed basis to resolve performance problems.
'f. PO/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 gen-
eral, the laboratory notifies SMO immediately upon identification of any
problem regarding the samples 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 or DPO,
who contacts the laboratory and resolves the problem. The resolution and
any specific actions taken are reported to the appropriate SMO personnel,
who records this information as part of the permanent Case record. The
laboratory also records the problem and resolution in the narrative portion
of the sample data report, so that the Region considers this information in
association with evaluating and using the data. Regional DPOs assist in the
monitoring of contractor performance and play a major role in ongoing
laboratory problem resolution in coordination with the PO.
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D. Laboratory Performance Evaluation
1. 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.
Aqueous organic and inorganic PE samples are typically shipped as "double
blind" samples (i.e., the PE samples are not discernable from routine field
samples) to ensure that the laboratory processes the samples in a routine
manner. Evaluation 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 pro-
gram's QA Data Base, and are utilized, along with other laboratory data, in
trend analyses, and evaluation and revision of contract QC criteria.
2. On-Site Laboratory Evaluation
At least once a year, EPA NPO, NEIC, Regional and EMSL/LV personnel
visit each contract laboratory facility and evaluate laboratory procedures.
The evaluation reports which result from these on-site visits are utilized by
the NPO in identifying and remedying laboratory performance problems.
Repeat on-site visits 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 sam-
ples for analysis until the problem has been corrected.
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.
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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 perfbrm 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 over-
all 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 contractor's responsiveness/responsibility for award under
future CLP solicitations.
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E. Sample Data Evaluation
1. Intercomparison Check Sample Studies
Intercomparison 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 (i.e., the laboratory is aware
samples are check samples but does not know sample composition). Analy-
tical 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 applica-
tions. 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 of the complete data package to the CLP SMO, EMSL/LV and the
Regional client. Each of 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 a
statistically significant subset of CLP sample data packages using a Mil.
Standard 105D approach. EMSL/LV also provides data audits, data
evaluation and participates in special requests such as enforcement
support, preparation/evaluation of data review SOPs and special projects
(e.g., Dioxin Incineration Study, Love Canal Habitability Study.) Based on
these reviews, EMSL/LV prepares a detailed report on the data packages,
which is provided to the NPO, DPOs, Regional Data Reviewers, 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 maintains the program's QA/QC Data Base. This
data base includes:
o Spike recoveries
o Blanks
o Duplicates
o Tuning
o Calibration
o Method of standard additions
o ICP check
o Analytical results for dioxin
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These data are then statistically evaluated and utilized to determine and
update contract QC acceptance windows for CLP-generated data and to
characterize laboratory and method performance.
2. Regional Data Review
The Regional client reviews all data packages resulting from Regional sam-
pling 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 the CLP data review Standard Operating
Procedures and references the requirements of the contract Statement of
Work under which the analyses were performed.
3. Contract Compliance Screening (CCS)
Every RAS CLP-generated data package is screened by SMO upon receipt
on a fast-turnaround basis (See Chapter IV, Section E). CCS determines if
all contractually required forms are included, that forms are completed
according to contract specifications, and that QA/QC results meet
contract specifications. CCS results are distributed to the laboratory,
Region and EMSL/LV and are used to determine recommendation for
payment. All CLP data packages are checked for completeness by SMO. If
any missing information, incomplete forms or other problems with the data
package are identified, the laboratory is contacted and instructed to
submit the missing or incorrect portions of the data package. Other
compliance discrepancies are addressed by the CCS reconciliation process.
4. SMO Data Review Services
Under direction of the NPO, SMO may perform additional data review,
checking the data for compliance to contract QC procedures and
parameters and for applicability *o its intended uses. This review is pro-
vided on a limited basis in response to specific Regional requests. Consult
Chapter IV, Section F, for a complete description of the data review
services provided and appropriate request procedures.
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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 defined 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 coordi-
nated 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 appli-
cation 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 Regions, SMO, laboratories and other program support contractor per-
sonnel. 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, existing
laboratory contracts are modified by the Contracting Officer to include
recommended revisions, through contract change order actions. Whenever
possible, all laboratory contracts within an analytical program are changed
concurrently to maintain consistency across the program. NPO-approved
protocol revisions are included in any new IFB solicitations.
2. Method Development
Development of new analytical methods may be initiated by a newly identi-
fied or redefined Agency analysis requirement, such as dioxin analysis.
Analytical methods utilized in the CLP are based on EPA developed and
approved methodologies. The NPO, EMSL/LV, EMSL/Cincinnati, EPA
Regions and the contractor community 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.
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APPENDICES TO
CLP USER'S GUIDE
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APPENDIX A
CLP DIRECTORY
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CLP
NATIONAL PROGRAM OFFICES
January 1987
USEPA Analytical Operations Branch (WH 548-A)
401 M Street, S.W.
Washington, DC 20460
(Room S-201)
202/382-7906
FT5/382-7906
James S. Vickery, Branch Chief
Gary Ward, Deputy Branch Chief, 382-4619
National Inorganics Program Manager
Joan Fisk, National Organics 382-3115
Program Manager
Bill Langley, Chemist/Inorganics 382-7906
Emile Boulos, Technical Officer/Organic 382-7942
Angelo Carasea, Technical Officer/Organic 382-7911
Duane Geuder, QA Officer 382-7943
Mike Carter, Program Coordinator, SMO PO 382-7909
Mary Mahsetky, Secretary
Rona Haley, Clerk Typist
USEPA Office of Administration
Procurement <5c Contracts Management Division (PM-214)
401 M Street, S.W.
Washington, DC 20460
Delivery Address:
499 S. Capitol Street
Fairchild Building, 3rd Floor
Superfund Section:
John Comstock, Section Chief 382-3168
Marian Bernd, CLP Solicitations 382-3195
Administrative Section:
Kathy Seikel, Team Leader
David Watson, Administrative Contracting Officer
Lee Levine, Contract Specialist
382-3192
382-3199
475-8233
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USEPA Environmental Monitoring Systems Laboratory (EMSL/LV)
944 East Harmon Avenue
Las Vegas, NV 89109
-or-
P.O. Box 15027
Las Vegas, NV 89114
Data to: EMSL/LV Executive Center
944 East Harmon Avenue, Room 226
Las Vegas, NV 89109
Attn: Data Audit Staff
Ronald K. Mitchum, Director, QA Division
702/798-2103 FTS 545-2103
Llewellyn Williams, Deputy Director, Toxics & Hazardous Waste Operations Branch
702/798-2383 FTS 545-2383
John.Moore, Acting Chief, Quality Assurance Research Branch
702/798-2132 FTS 545-2132
George Brilis, Chemist
702/798-2112 FTS 545-2112
Edward Kantor, Analytical Standards
702/798-2690 FTS 545-2690
G. Wayne Sovocol, Analytical Standards
702/798-2212 FTS 545-2212
Larry Butler, Program Manager, PE Studies
702/798-2114 FTS 545-2114
Steve Billets, Chief, Methods Evaluation Branch
702/798-2232 FTS 545-2232
Dave Bottreil, Chemist
702/798-2142 FTS'545-2142
Bob Schonbrod, Acid Deposition - Aqueous
702/798-2229 FTS 545-2229
Lou Blume, Acid Deposition - Soil
702/798-2213 FTS 545-2213
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EMSL/LV Contractors:
LEMSCO Lockheed
944 East Harmon Avenue
Las Vegas, NV 89109
-or-
1050 E. Flamingo, Suite 120
Las Vegas, NV 89109
Steve Simon, Environmental Chemistry, Department Manager
702/734-3285
Joseph Donnelly, Chemistry Research Dept. Manager
702/798-2299
Mike Homsher, QA Department Manager
702/734-3312
K.S. Kumar, Scientific Supervisor, Data Evaluation
702/734-3312
Richard Flotard, Protocol Development
'702/734-3315
Chuck Hoover, Laboratory Performance
702/798-3143
Dean Mericas, Scientific Supervisor, Acid Deposition QA
702/734-3229
Sevda Drouse, Supervisor, Acid Deposition Aquatic it Soil QA
702/734-3295
Joan Bartz, Acid Deposition Soil QA Group
702/734-3222
Briant Hess, Acid Deposition Aquatic QA Group
702/734-3288
M.J. Pearson, Scientific Supervisor, Computer Services
702/734-3206
Ken Asbury, Environmental Monitoring Dept. Manager
702/734-3267
Henry Kerfoot, Methods Development
702/734-3217
University of Nevada/Las Vegas
QA Support Laboratory
4505 Maryland Parkway
Las Vegas, NV 89154
702/739-3142
Joe Compana, Laboratory Director
Armand Lange, Organic Specialist
Donald Schoengold, Reference Materials Specialist
Yves Tondeur, Dioxin Specialist
Vern Hodge, Inorganic Specialist
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USEPA National Enforcement Investigations Center (NEIC)
Denver Federal Center
Building 53, Entrance E-2
P.O. Box 25227
Denver, CO 80225
Carroll G. Wills, Deputy Director
303/236-5120 FTS 776-5120
Ted Meiggs, Assistant Director/Laboratory Services
303/236-5132 FTS 776-5132
Dean Hill, Laboratory Services
303/236-7970 FTS 776-7970
Joe Lowry, Inorganic Laboratory
303/236-9963 FTS 776-9963
Robert Laidlaw, Chief, Evidence Audit Team
303/236-5122 FTS 776-5122
Gerri Hilden, Evidence Audit (Chain-of-Custody Expert)
303/236-5122 FTS 776-5122
Donald Roche, Evidence Audit Representative (Primary Contact)
303/236-5122 FTS 776-5122
NEIC Contractors for Document Control;
TechLaw, Inc.
Contractor Evidence Audit Team (CEAT)
12600 West Colfax, Suite C310
Lakewood, CO 80215
303/233-1248
Norm Shutler, Program Director
George Duba, Team Leader
Keith Wegner, Deputy Team Leader
Rich Greenberg, Environmental Counsel
Bill Rhyne, Evidence Auditor
Brenda Barkas, Evidence Auditor
Jeff Worthington, Evidence Auditor
Bill von Shulz, Evidence Auditor
Ellen Holder, Project Leader/Evidence Auditor (Files Purge)
Mary Franquemont, Evidence Auditor
Leo Oserow, Evidence Auditor
Fred C. Hart Associates, Inc. (Historical Information)
1110 Vermont Avenue N.W.
Suite 410
Washington, DC 20005
202/223-5621
Eileen Simons
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USEPA Environmental Monitoring & Suppport Laboratory (EMSL/CINN)
26 West St. Clair Street
Cincinnati, OH 45268
Bob Booth, Laboratory Director
FTS 684-7301 513/569-7301
Bill Budde, Advanced Instrumentation/CLP Specialist
FTS 684-7309 513/569-7309
Tom Bellar, Research Chemist
FTS 684-7512 513/569-7512
Ed Berg, Performance Evaluation
FTS 684-7325 513/569-7325
Ted Martin, Inorganic Chemist/Methods Development
FTS 684-7312 513/569-7312
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Field Contractors - Main Office:
NUS Corporation (FIT II - East)
1300 North 17th Street
Suite 1320
Arlington, VA 22209
Paul Clay
Tom Centi
.703/522-8802
Ecology & Environment (FIT II - West)
1700 North Moore Street, Suite 1105
Arlington, VA 22209
Lou Welzel, Cooler UPS Accounts
Robyn Seay
703/522-6065
Camp, Dresser & McKee/NPMO (REM II)
7611 Little River Turnpike, Suite 104
Annandale, VA 22003
Gary Dunbar
703/642-5500
Steve Paquette
Andy Szilazyi
703/642-0544
Ebasco Services, Inc. (REM III)
Zone Program Management Office
2000 Fifteenth Stree-t North
Arlington, VA 22201
Arthur Chu
Gail Solomon
703/558-7555
CH2M Hill (REM IV)
628 Herndon Parkway
Herndon, VA 22070
Bill Dehn
703/471-1441
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USEPA REGIONS
Environmental Services Division (ESD) Directors
Waste Management Division (WMD) Directors
Laboratory Directors
Technical Deputy Project Officers (DPO)
ESAT DPOs
RSCC Authorized Requestors*
Sampling Contractors
Data Submission
REGION I
USEPA Region I
3.F. Kennedy Federal Bldg.
Boston, MA 02203
617/565-3698
Merrill Hohman, SF Coordinator 617/565-3698 FTS 835-3698
Waste Management Division Director
~Nancy Barmakian - Primary AR
617/565-3666 FTS 835-3666
~Rosalie Baldassari
617/565-3660 FTS 835-3666
USEPA Region I
Environmental Services Division
60 Westview Street
Lexington, MA 02173
617/861-6700 FTS 828-6700 (Main Office)
*Dr. Thomas Spittler 617/861-6700 FTS 828-6700
Chief, Technical Support Branch
~Wayne Wirtanen, ESAT and Technical DPO 617/861-6700 FTS 828-6700
Edward Conly .17/861-6700 FTS 828-6700
Director, ESD
Data Submission
USEPA Region I
JFK Federal Building, Room 1903
Boston, MA 02203
Attn: Nancy Barmakian
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REGION n
USEPA Region II
Environmental Services Division
Building 209
Woodbridge Avenue
Edison, New Jersey 08837
Barbara Metzger 201/321-6754 FTS 340-6754
Director, ESD
Dan Sullivan, FTS 340-6706
Assistant Deputy Director, ESD
Dan Lillian
Chief, Technical Support Branch
ESAT DPO, Laboratory Director FTS 340-6707
Bill C oakley, Technical DPO FTS 340-6702
SF QA Coordinator
Dr. Richard Spear 201/321-6685 FTS 340-6685
Chief, Surveillance & Monitoring Branch
*Regina Mulcahy - Primary AR 201/321-6705 FTS 340-6705
Director, Emergency &. Remedial Response Div.
NUS Corporation (FIT II - East)
Raritan Plaza III
Fieldcrest Avenue
Edison, NJ 08837
Mike Young 201/225-6160
Data Submission
USEPA Region II
Environmental Services Division
Woodbridge Avenue
Building 209
Edison, New Jersey 08837
Attn: Dr. Richard Spear
*Sharon Steltz
*Darvene Adams
*Doug Stout
* Diana Messina
201/906-6087 FTS 340-6807
201/321-6700 FTS 340-6700
201/321-6717 FTS 340-6717
201/321-6776 FTS 340-6776
USEPA Region II
26 Federal Plaza
New York, New York 10278
Stephen Luftig, SF Coordinator
FTS 264-1574
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REGION m
USEPA Region III
Superfund Branch
841 Chestnut Street
Philadelphia, PA 19107
Greene Jones
Director, ESD
Thomas Voltaggio
SF Coordinator
Stephen Wassersug
Director, Haz. Waste Mgmt. Div.
Harold "Butch" Byer
FIT DPO
Catherine Hodgkiss
CERCLA Enforcement Section Chief
Neil Swanson
CERCLA Remedial Enforcement Acting Chief
USEPA Region III
Central Regional Laboratory
839 Bestgate Road
•Annapolis, MD 21401
301/224-2740 FTS 922-3752 (Main Office)
Orteria Villa, Jr.
Director, Central Regional Laboratory
* Patricia Krantz
Technical DPO; ESAT DPO
*John Austin (through January 1, 1987)
Jim Borson (February through May)
Chief, Laboratory Section
* Colleen Walling - Primary AR
John Austin - Organic Chemist
215/597-4532 FTS 597-4532
215/597-8132 FTS 597-8132
215/597-8131 FTS 597-8131
215/597-3437 FTS 597-3437
NUS Corporation
992 Old Eagle School Road (FIT II
Suite 916
Wayne, PA 19087
Russ Sloboda
Garth Glenn
East)
215/687-9510
215/687-9510
Data Submission
USEPA Region III
Central Regional Laboratory
839 Bestgate Road
Annapolis, MD 21401
Attn: Patricia Krantz
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REGION V
USEPA Region V
230 S. Dearborn St.
13th Floor (HR-13)
Chicago, 1L 60604
312/353-8370 FTS 353-8370
William Miner 312/886-4658 FTS 886-4658
SF Enforcement
Richard Bartelt 312/886-7570 FTS 886-7570
SF Coordinator (Remedial Response)
Greg Vanderloon FTS 886-6217
Chief, Site Management Section
Basil Constantelos FTS 886-7579
Director, Waste Management Division
USEPA Region V
Environmental Services Division
536 South Clark St., 10th Floor, CRL
Chicago, IL 60605
William Sanders, III 312/353-3808 FTS 353-3808
Director, ESD
Thomas Yeates FTS 353-3808
Deputy Director, ESD
*Curtis Ross FTS 353-8370, 9064
Director, Central Regional Lab
* Chuck Elly FTS 353-9087, 8370
Technical DPO; ESAT DPO, Primary AR
~Dennis Wesolowski FTS 886-1971
Frank Thomas - Organic Coordinator, Dioxin FTS 353-5482
Jay Thakkar - Acting Inorganic Coordinator FTS 886-1972
* Jan Pels FTS 353-2720
Ecology & Environment
111 West Jackson Blvd.
Chicago, IL 60604
* * Renee Hicks 312/663-9415
**Kathy Getty 312/663-9415
Cindy Bacunas 312/663-9415
CH2M Hill (Rem II)
West Wisconsin Ave.
Suite 700
P.O. Box 2090
Milwaukee, WI 53201
**Jeff Kaiser
**Shirley Stringer
414/272-2426
414/272-2426
**AR, RAS Only
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REGION V (Continued)
Weston
666 Dundee Road
Suite 1501
Norbrook, IL 60062
**Sue Lorenz
**Sally Matz
312/498-9094
312/498-9094
Camp, Dresser & McKee (RE M II)
11 East Adams
Suite 1100
Chicago, IL 60603
Michigan Department of Public Resources
P.O. Box 30028
Lansing, MI 48909
Data Submission
USEPA Region V
Environmental Services Division
536 South Clark Street, 10th Floor, CRL
Chicago, IL 60605
Attn: Curtis Ross
**AR, RAS Only
~Wendy Dewar
**3ill Line
**Tim Henning
312/786-1313
312/786-1313
312/786-1313
*Barb Grabowski
517/373-4825
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REGION VI
USEPA Region VI
Environmental Services Division
Renaissance Tower
1201 Elm Street
Dallas, Texas 75270
212/767-2724 FTS 729-2724
Russell Rhoades
Director, ESD
Martha McKee
SF Coordinator
Allyn Davis
Director, Hazardous Waste Management Division
~Keith Bradley - Primary AR
*Hank Thompson
*Myra Perez - Alternate
Dick McGlothlin (Forms)
Charles Gazda
Emergency Response Branch
Ecology & Environment (FIT II - West)
1509 Main Street
Suite 814
Dallas, TX 75201
K. Maione, Regional Program Manager
Gene McDonald, FIT Training Coordinator
**David Anderson
**Hunt Chapman
**Lloyd Collins
**John Totin, Assistant Regional Program Manager
**Jairo Guevera
USEPA Region VI Laboratory
Monterey Park Plaza - Bldg. C
6608 Hornwood Drive
Houston, TX 77074
713/954-1771 FTS 526-1771
Diana Ayres - Acting Branch Chief
Melvin Ritter - Data Review
Michael Daggett - ESAT DPO
214/767-2697 FTS 729-2697
214/767-2645 FTS 729-2645
214/767-2730 FTS 729-2730
214/767-9988 FTS 729-9988
214/767-9989 FTS 729-9989
214/767-9789 FTS 729-9789
FTS 729-9788
FTS 729-9798
214/742-4521, 6601
713/954-6771 FTS 526-6771
713/954-6766 FTS 526-1766
**AR, RAS Only
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REGION VI (Continued)
Data Submission
USEPA Region VI Laboratory
Monterey Park Plaza - Bldg. C
6608 Hornwood Drive
Houston, TX 7707k
Attn: Melvin Ritter
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REGION YD
USEPA Region VII
726 Minnesota Ave.
Kansas City, KS 66101
David Wagoner, SF Coordinator & Director 816/374-6529 FTS 758-6529
Air & Waste Management Division
USEPA Region VII
Environmental Services Division
25 Funston Road
Kansas City, KS 66115
913/236-3881 FTS 757-3881
John Wicklund
Director, ESD
Bob Kleopfer
Lab Branch Chief; ESAT DPO
~Bill Bunn
CLP QA Chief
*Debra Morey
Technical DPO
* Joyce Woods, Primary AR 913/236-3881 FTS 757-3881
Paul Dougherty 913/236-3888 FTS 757-3888
RPO - FIT
Ron McCutcheon 913/236-3881 FTS 757-3881
RPO - TAT
Data Submission
USEPA Region VII
Environmental Services Division
25 Funston Road
Kansas City, KS 66115
Attn: Joyce Woods
913/236-3720 FTS 757-3720
913/236-3881 FTS 757-3881
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REGION Yin
USEPA Region VIII
Environmental Services Division
999 - 18th Street, Room 1300
Denver, CO 80202-2402
Robert Duprey, Director, Hazardous Waste
Management Division 303/293-1720 FTS 564-1720
*Keith Schwab 303/293-1686 FTS 564-1686
Associate Director, ESD, Primary AR
J. William Geise, Jr, FTS 564-1518
SF Branch Chief
Judy Wong - SF Enforcement Section FTS 564-1519
Mailing Address:
USEPA Region VIII Lab
Box 25366
Denver Federal Center
Denver, CO 80225
Laboratory (For Cooler Return:
USEPA Region VIII Laboratory
Denver Federal Center
Bldg. 53, Room 2707
Denver, CO 80225
James Lehr
Director, ESD
~John Tilstra
Technical DPO; ESAT DPO
Rolland Grabbe
Assistant DPO, Data Review
Joan Barnes
Chief, Lab Services Section.
Ralph Allen, Inorganic Contact 303/236-5065
CH2M Hill (REM II)
P.O. Box 22508
Denver, CO 80222
Jim Schwing 303/757-4984
Cary Jackson, (Support Systems, Inc) 303/226-3561
Assistant Organic Contact
Camp Dresser & McKee (REM IV)
2300 - 15th St.
Suite 400 Riverpoint
Denver, CO 80202
Dick Cheatham 303/458-1311
Assistant Inorganics Contact
303/236-5061 FTS 776-5061
303/236-5056
FTS 776-5056, 5073
303/236-5065
FTS 776-5073
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REGION Vni (Continued)
Ecology & Environment (FIT II)
^ 105 E. Florida Ave.
Suite 350
Denver, CO 80222
Stuart Richardson
Lynn Roberts
Randy Greaves - Organics Technical Contact
Montana EPA Office
301 S. Park,
P.O. Drawer 10096
Helena, MT 59626
Lee Shanklin
Data Submission
US EPA Region VIII
Denver Federal Center
Bldg. 53, Room 2707
Denver, CO 80225
Attn: John Tilstra
303/757-4984
303/757-4984
303/757-4984
406/444-5414 FTS 585-5414
FTS 584-5414
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REGION IX
USEPA Region IX
Office of Policy & Management (OPM)
Environmental Services Branch (ESB)
Quality Assurance Management Section
215 Fremont Street
San Francisco, CA 94105
David Mowday FTS 454-8189
Deputy Director, OPM (equiv. to ESD Director)
Harry Seraydarian, SF Coordinator FTS 454-7460
Director, Toxics & Waste Management Division
Terry Stumph, ESAT DPO 415/974-7483 FTS 454-7483
Chief, ESB
Kent Kitchingman, Technical DPO 415/974-0924 FTS 454-0924
~Stewart Simpson FTS 454-0925
*Thomas Huetteman FTS 454-0923
Patti Connaughton, Analytical Specialist FTS 454-8004
David Binghman, Team Leader FTS 454-8149
Ecology & Environment 415/777-2811
120 Howard St.
Suite 640
San Francisco, CA 94105
Ron Karpowitz - FIT Leader
Dr. P.K. - Data Review Coordinator
John Mue - Sampling Advisor
Camp Dreser & Mckee (REM II)
100 Spear St.
Suite 700
San Francisco, CA 94105
Craig Von Bargen - Principal Engineer 415/495-5009
CH2M Hill (REM IV)
2510 Redhill Ave.
Suite A
Santa Ana, CA 92705
Michael Bitner 714/250-5500
Data Submission
USEPA Region IX
Environmental Services Branch (ESB)
215 Fremont Street, P-3-2
San Francisco, CA 94105
Attn: Kent Kitchingman
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REGION X
USEPA Region X
Environmental Services Division
1200 Sixth Avenue
M/S 329
Seattle, WA 98101
Robert Courson FTS 399-0404
ESD Director
Chuck Findley FTS 399-1906
Hazardous Waste Division Director
William Schmidt
Chief, Field Operation & Technical
Support Branch
* Joyce Crosson
~John Osborn - RPO/FIT
USEPA Region X Laboratory
P.O. Box 549
Manchester, WA 98353
For Federal Express Only;
7411 Beach Drive East
Port Orchard, WA 98366
. Mike Johnston 2061442-0370 FTS 399-0370
Chief, Lab Section
Joseph Blazevich
Assistant DPO
Gerald Muth - Technical and ESAT DPO
206/442-1526
FTS 399-1526, 1296
FTS 399-8562
FTS 399-0837
Ecology & Environment (FIT II)
108 S. Washington
Suite 302
Seattle, WA 98104
Andy Hafferty - FIT/QA, Senior Chemist 206/624-9537
CH2M Hill 206/453-5000
1500 - 114th Ave., S.E.
Bellevue, WA 98004-2050
Neil Geitner
Data Submission
USEPA Region X
1200 Sixth Avenue
MS/329
Seattle, WA 98101
Attn: Joyce Crosson
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MISCELLANEOUS INFORMATION
ERT/Edison
USEPA
Environmental Response Branch
GSA Raritan Depot
Woodbridge Avenue
Edison, New Jersey 08837
George Prince
Mike Urban
Royal Nadeau
Cooler Return - UPS Account:
Ecology <3c Environment
1700 N. Moore St.
Rosslyn Center
Arlington, VA 22209
Lou Welzel
Bottle Repository:
I-Chem Research Corp.
23787-F Eichler Street
Hayward, CA 94545
Anita Rudd
I-Chem Research Corporation
104 Quigley Blvd.
New Castle, DE 19720
FTS 340-6649, 6689 & 6743
703/522-6065
415/782-3905
302/322-7657
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SAMPLE MANAGEMENT OFFICE
CLP Sample Management Office
P.O. Box 818
Alexandria, Virginia 22313
703/557-2490 FTS 557-2490
Street Address:
300 North Lee Street
Alexandria, Virginia 22314
David H. Stewart
Vice President
Management Services Division
Don Trees, Program Manager
Data Processing and Applications Support
Peter Isaacson, Senior QA Chemist
Contract Compliance Screening (CCS)
Harry McCarty, Chemist
CCS - Organics
Doris Ling, Chemist
CCS - Organics
Bill Eckel, Analyst
CCS - Inorganics
Sa'ad Masri, Quality Assurance Chemist
CCS - Inorganics
Richard Thacker, Program Manager
SMO Operations/Management Planning
Steven Manzo, Environmental Program Analyst
Management Planning/Programmatic Support
Linda Boynton, Project Leader
Analytical Services Group
Coordination & Implementation of CLP Systems
(DPO, RSCC, Allocation, etc.) Acid Rain, ESAT Programs
Roch Mongeon, Environmental Program Analyst
O.S.W. Ground Water Monitoring Task Force, Group Leader 5
Paula Ausserer, Environmental Program Coordinator
EPA Regions VIII, X
Carol Shaeffer, Environmental Program Coordinator
EPA Regions III, IV
Mike Whittington, Environmental Program Coordinator
EPA Region II
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Analytical Services Group (continued)
Maka Grogard, Environmental Program Analyst
EPA Region IX, Group Leader;
Leslie Braun, Environmental Program Coordinator
EPA Region V
Sean Kolb, Environmental Program Coordinator
EPA Regions I, VII
Tony Nesky, Environmental Program Coordinator
EPA Region VI
Sheila Frey, Management Information Coordinator (RAS)
Backlog Inventory, Fonms Management
Lulu Eager, Senior Bookkeeper (SAS)
SAS Invoice Processing
John Schlesinger, Management Information Coordinator
(RAS)
Hoang Ho, Management Information Coordinator
(SAS)
Deborah Miller, Project Leader
Program/Contracts Support Group
Mike Tindle, Environmental Program Coordinator
IFB Support, Meeting Coordinator
Talia Peters, Environmental Program Coordinator
Bottle Repository Support, CLP Materials Distribution,
Program Directory Compilation
Tina DeYoung, Project Leader
Management Information Group
DPO Reports, Ad Hoc Requests, Blue Book Reports
Pam Werntz Simons, Management Information Systems Manager
Site/Cost Accounting, Invoicing and Reconciliation Production
Rhonda Harmon, Initial Invoicing Coordination
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REGIONAL DEPUTY PROJECT OFFICERS
FOR
CLP TECHNICAL ADMINISTRATION
USEPA Region I
Wayne Wirtanen
USEPA Region I
Environmental Services Division
60 Westview Street
Lexington, MA 02173
617/861-6700
USEPA Region II
William Coakley
Superfund QA Coordinator
USEPA Region II
Environmental Services Division
Building 209
Woodbridge Avenue
Edison, New Jersey 08837
201/321-6702
USEPA Region III
Patricia Krantz
QA Officer
USEPA Region III
Annapolis Field Office
Central Regional Office
839 Bestgate Rd.
Annapolis, MD 21401
301/224-2740
USEPA Region IV
Tom B. Bennett, Jr.
Chief, Chemistry Section
USEPA Region IV
Environmental Services Division
College Station Road
Athens, Georgia 30613
404/546-3112
USEPA Region V
Chuck Elly
Technical DPO
USEPA Region V
536 S. Clark St.
Tenth Floor, CRL
Chicago, Illinois 60605
312/353-9087
USEPA Region VI
David Stockton
USEPA Region VI
Monterey Park Plaza, Bldg. C
6608 Hornwood Drive
Houston, Texas 77074
713/954-6766
USEPA Region VII
Debra Morey
USEPA Region VII
Environmental Services Division
25 Funston Rd.
Kansas City, Kansas 66115
913/236-3881
USEPA Region VIII
John Tilstra
USEPA Region VIII - Laboratory
Denver Federal Center
Bldg. 53, Entrance W-l
2nd Floor, Room D-2707
Denver, CO 80225
303/236-5056
USEPA Region IX
Kent Kitchingman
Technical DPO
USEPA Region IX
215 Fremont Street
San Francisco, California 94105
415/974-7483
USEPA Region X
Gerald Muth
Chief, Laboratory Branch
USEPA Region X
P.O. Box 549
Manchester, WA 98353
206/442-0370
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CLIENT
Region I
REGIONAL SAMPLE CONTROL CENTERS
12/86
AUTHORIZED REQUESTORS
Region II
Region III
Region IV
Nancy Barmakian*
8-835-3666; 617/565-3666
Rosalie Baldassari
8-835-3660; 617/565-3660
Dr. Thomas M. Spittler
8-828-6700; 617/861-6700
Regina Mulcahy*
8-340-6705; 201/321-6705
Sharon Steltz
8-340-6807; 201/321-6807
Darvene Adams
8-340-6700; 201/321-6700
Doug Stout
8-340-6717; 201/321-6717
Diana Messina
8-340-6776; 201/224-6776
Colleen Walling*
8-922-3752; 301/224-2740
Pat Krantz
8-922-3752; 301/224-2740
Doug Lair
8-250-5413; 404/546-5413
Tom Bennett, Jr.*
8-250-3112; 404/546-3112
Myron Stephenson
8-250-3385; 404/546-3385
Debbie Colquitt
8-250-3388; 404/546-3388
Doug Mundrick
8-250-3321; 404/546-3321
~Primary Authorized Requestor
A-24
-------
CLIENT
AUTHORIZED REQUESTORS
Region V
Chuck Elly*
8-353-8370; 312/353-8370
Dennis Wesolowski
8-886-1971; 312/886-1971
Jan Pels
8-353-2720; 312/353-2720
Curtis Ross
8-353-8370; 312/353-8370
RAS Only
E&E:
CH2M Hill:
Weston:
Camp,
Dresser
& McKee:
Michigan
DNR:
Kathy Getty
Renee Hicks
312/663-9415
Jeff Kaiser
Shirley Stringer
414/272-2426
Sally Matz
Sue Lorenz
312/498-9094
Wendy DeWar
Jill Line
Tim Henning
312/786-1313
Barb Grabowski
517/373-4825
Region VI
Hank Thompson
8-729-9989; 214/767-9989
Myra Perez
8-729-9789; 214/767-9789
Keith Bradley*
8-729-9988; 214/767-9988
RAS Only .
E&E:
John Totin
David Anderson
Jairo Guevara
Hunt Chapman
Lloyd Collins
214/742-4521
~Primary Authorized Requestor
A-25
-------
CLIENT
AUTHORIZED REQUESTORS
Region VII
Region VIII
Region IX
Region X
Joyce Woods*
8-757-3881; 913/236-3881
Bill Bunn
8-757-3881; 913/236-3881
Debra Morey
8-757-3881; 913/236-3881
Keith Schwab*
8-564-1686; 303/293-1686
John Tilstra
8-776-5056; 303/236-5056
Lynn Roberts
FIT - E&E
303/757-4984
Stewart Simpson*
8-454-0925; 415/974-0925
Thomas Huetteman
8-454-0923; 415/974-0923
Joyce Crosson
8-399-8562; 206/442-8562
John Osborn
8-399-0837; 206/442-0837
~Primary Authorized Requestor
A-26
-------
12/86
CONTRACT LABORATORY PROGRAM
REGIONAL/LABORATORY COMMUNICATION SYSTEM
AUTHORIZED REGIONAL TECHNICAL CONTACTS
REGION I
Organics
Inorganics
Dioxin
Primary:
Primary:
Primary:
Wayne Wirtanen
Wayne Wirtanen
Wayne Wirtanen
617/861-6700
617/861-6700
617/861-6700
REGION D
Organics
Inorganics
Dioxin
Primary:
Alternate:
Primary:
Alternate:
Primary:
Alternate:
Bill Coakley
Regina Mulcahy
Stelios Gerazounis
Elaine Vikara
Fred Elsen
John Birri
Regina Mulcahy
Robert Davis
Lenny Voo
John Birri
Regina Mulcahy
201/321-6702
201/321-6705
201/321-6778
201/321-6778
201/321-6778
201/321-6709
201/321-6705
201/321-6778
201/321-6778
201/321-6709
201/321-6705
REGION III
Organics
Inorganics
Dioxin
Primary:
Alternate:
Primary:
Alternate:
Chuck Sands
Diana Pickens
Primary: Pat Krantz
Chuck Sands
Diana Pickens
301/224-2740
301/224-2740
301/224-2740
301/224-2740
301/224-2740
REGION IV
Organics
Inorganics
Dioxin
Primary:
Primary:
Primary:
Charles Hooper
Michael Waska
Charles Hooper
404/250-3387
404/546-3165
404/250-3387
A-27
-------
12/86
REGION V
REGION VI
REGION VII
REGION Vm
Organics
Primary:
Frank Thomas
312/886-1973
Alternate:
Dennis Wesolowski
Jan Pels
312/886-1971
312/886-1971
Inorganics
Primary:
Jay Thakkar
312/886-9087
Alternate:
Ida Levin
312/886-9087
Dioxin
Primary:
Frank Thomas
312/886-1973
Alternate:
Dennis Wesolowski
312/886-1971
Organics
Primary:
Mel Ritter
713/954-6771
Alternate:
Keith Bradley
214/767-9770
Inorganics
Primary:
Mahmond EI Feky
713/954-6771
Alternate:
Keith Bradley
214/767-9770
Dioxin
Primary:
Mel Ritter
713/954-6771
Alternate:
Keith Bradley
214/767-9770
Organics
Primary:
Debra Morey
913/236-3881
Alternate:
Bill Bunn
913/236-3881
Inorganics
Primary:
Debra Morey
913/236-3881
Alternate:
Bill Bunn
913/236-3881
Dioxin
Primary:
Debra Morey
913/236-3881
Alternate:
Bill Bunn
913/236-3881
Organics
Primary:
Randy Greaves(E<3cE)
303/757-4984
Alternate:
Cary Jackson
303/226-3561
Inorganics
Primary:
Ralph Allen
303/757-5063
Alternate:
Richard Cheatham
(CDM)
303/458-1311
Dioxin
Primary:
Alternate:
Randy Greaves (E3cE)
Cary Jackson
303/757-4984
303/226-3561
A-28
-------
REGION IX
Organics
Inorganics
Dioxin
Primary:
Primary:
Alternate:
Primary:
Kent Kitchingman
Kent Kitchingman
P.K. Chattopadhyay
Kent Kitchingman
415/974-0924
415/974-0924
415/777-2811
415/974-0924
REGION X
Organics
Inorganics
Dioxin
Primary:
Alternate:
Primary:
Alternate:
Primary:
Alternate:
Joe Blazevich
Gerald Muth
Andrew Hafferty
Steven Pope
Andrew Hafferty
Bob Rieck
Gerald Muth
Joe Blazevich
206/442-0370
206/442-0370
206/624-9537
206/442-0370
206/624-9537
206/442-0370
206/442-0370
206/442-0370
A-29
-------
APPENDIX B
RAS DELIVERABLES AND DATA REPORTING FORMS
B-l
-------
RAS ORGANICS
DELIVERABLES INDEX
I. Case Narrative
The Case narrative must contain: Case number, Contract number, summary of any
QC, sample, shipment and analytical problems, and documentation of all internal decision
tree processes used. Outline problems encountered and final solutions. Be as specific and
detailed as necessary.
Summary
Surrogate Percent Recovery Summary (Form II)
Matrix Spike/Matrix Spike Duplicate Summary (Form III)
Method Blank Summary (Form IV)
(If more than a single form is necessary, it must be arranged in chronological
order.)
GC/MS Tuning and Calibration Standard (Form V)
1. DFTPP in chronological order; by instrument.
2. BFB in chronological order; by instrument.
III. Sample Data
A. Samples should be arranged in packets with the Traffic Report, the Organic
Analysis Data Sheet (Form I), followed by the raw data for volatile, semi-
volatile and pesticide sample fractions. These sample packets should then be
placed in increasing SMO sample number order.
1. Copy of Sample Traffic Report
2. HSL Results — Organic Analysis Data Sheet (Form I)
3. Tentatively Identified Compounds (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."
Raw data — in order: VOA, BNA, Pesticide
a. Reconstructed ion chromatogram(s) (GC/MS), chromatogram(s)
(GC)
b. Data System Printout
o Quantitation report or legible facsimile (GC/MS)
B-2
II. QC
A.
B.
C.
D.
-------
o Integration report or data system printout (GC)
o Calibration plots (area vs. concentration) for 4,4'-DDT, 4,4'-
DDD, *t,V-DDE or toxaphene (where appropriate)
c. Raw HSL mass spectra and the background subtracted HSL mass
spectra with lab generated HSL standard spectra (dual display)
o Data systems incapable of dual display shall provide spectra in
order:
Raw HSL compound spectra
- Enhanced or background subtracted spectra
Laboratory generated HSL standard spectra
d. GC/MS library search spectra for Tentatively Identified Com-
pound^) (TIC)
e. Quantitation/Calculation of TIC concentration(s)
f. Manual work sheets
g. GPC chromatograms (if appropriate)
IV. Standards Data
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.
I. 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 instrufnent used.
1. When more than one Continuing Calibration is performed, forms must be
in chronological order.
D. Pesticide forms in the following order:
1. Form VIII — Pesticide Evaluation Standards Summary (all GC columns)
2. Form IX — Pesticide/PCB Standards Summary (all GC columns)
B-3
-------
3. Form X — Pesticide/PCB Identification (only required for positive
results)
E. VOA standard(s) reconstructed ion chromatograms and quantitation reports (or
legible facsimile) for both the initial (five point) and all continuing (12 hour)
calibrations. Spectra are not required.
F. BNA standard(s) reconstructed ion chromatograms and quantitation reports (or
legible facsimile) for both the initial (five point) and all continuing (12 hour)
calibrations. Spectra are not required.
G. All pesticide Evaluation Standard(s) (A, B and C) chromatograms and data
system printouts in chronological order by GC column type.
H. All pesticide Individual Standard Mix (A or B) chromatograms and data system
printouts in chronological order by GC column type.
I. Pesticide Quantitation Standard(s) chromatograms and data system printouts.
V. Raw QC Data
A. DFTPP (for each 12-hour period, for each GC/MS system utilized)
1. Bar graph spectrum
2. Mass listing
B. BFB (for each 12-hour period, for each GC/MS system utilized)
1. Bar graph spectrum
2. Mass listing
C. Blank Data
1. Tabulated results (Form I)
2. Tentatively Identified Compound(s) (TlC) (Form I, Part B), even if none
found
3. Raw Data — in order: VOj^, BNA, Pesticide
a. Reconstructed ion chromatogram(s) and quantitation report(s) or
legible facsimile (GC/MS)
b. Chromatogram(s) and data system printout(s) (GC)
c. HSL spectra with lab generated standard (dual display)
o Data systems incapable of dual display shall provide spectra in
order:
B-4
-------
Raw HSL compound spectra
Enhanced or background subtracted spectra
Laboratory generated HSL standard spectra
d. GC/MS library search spectra for Tentatively Identified Com-
pound(s) (TIC)
e. Quantitation/calculation of TIC concentration(s)
Matrix Spike Data
1. Tabulated results (Form I) of non-spiked HSL compounds
a. Form I, Part B not required
2. Raw Data — in order: VOA, BNA, Pesticide
a. Reconstructed ion chromatogram(s) and quantitation report(s) or
legible facsimile (GC/MS)
o Spectra not required
b. Chromatogram(s) and data system printout(s) (GC)
o Both primary and confirmation column data is required
Matrix Spike Duplicate Data
1. Tabulated results (Form I) of non-spiked HSL compounds
a. Form I, Part B not required
2. Raw Data — in order: VOA, BNA, Pesticide
a. Reconstructed ion chromatogram(s) and quantitation report(s) or
legible facsimile (GC/MS)
o Spectra not required
b. Chromatogram(s) and data system printout(s) (GC)
o Both primary and confirmation column data is required
B-5
-------
RAS ORGANIC DATA REPORTING FORMS
B-6
-------
Sample Number
Organics Analysis Data Sheet
(Page 1)
Laboratory Name: Case No:
Lab Sample ID No: QC Report No:
Sample Matrix. Contract No:
Data Release Authorized By: Date Sample Received:
Volatile Compounds
Concentration: Low Medium (Circle One)
Date Extracted/Prepared:
Date Analyzed:
Conc/Dil Factor: pH
Percent Moisture: (Not Decanted)
CAS
Number
ug/l or ug/Kg
(Circle One)
CAS
Number
ug/lor ug/Kg
(Circle One)
74-87-3
Chloromethane
78-87-5
1. 2-Dichloropropane
74-83-9
Bromomethane
10061-02-6
Trans-1, 3-Dichloropropene
75-01 -4
Vinyl Chloride
79-01-6
Trichloroethene
75-00-3
Chloroethane
124-48-1
Dibromochloromethane
75-09-2
Methylene Chloride
79-00-5
1. 1. 2-Trichloroethane
67-64-1
Acetone
71-43-2
Benzene
75-15-0
Carbon Disulfide
10061-01-5
cis-1, 3-Dichloropropene
75-35-4
1,1 -Dichloroethene
110-75-8
2 -Chloroethylvinylether
75-34-3
1,1 -Dichtoroethane
75-25-2
Bromoform
156-60-5
Trans-1, 2-Dichloroethene
108-10-1
4-Methyl-2-Pentanone
67-66-3
Chloroform
591-78-6
2-Hexanone
107-06-2
1.2-Dichloroethane
127-18-4
Tetrachloroethene
78-93-3
2-Butanone
79-34-5
1.1,2. 2-Tetrachloroethane
71-55-6
1,1, 1-Trichloroethane
108-88-3
Toluene
56-23-5
Carbon Tetrachloride
108-90-7
Chlorobenzene
108-05-4
Vinyl Acetate
100-41-4
Ethylbenzene
75-27-4
Bromodichloromethane
100-42-5
Styrene
Total Xylenes
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 each flag must 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 bul not detected Report the
minimum detection limit for the sample with the Ufe.g.. 10U) based
on necessary concentration/dilution action. (This is not necessarily
the instrument detection limit ) The footnote should read: U-
Compound was analyzed lor 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 is assumed or when the mass spectral data
indicated 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) If limit of detection is 10 pg/l and a
concentration of 3 *jg/l is calculated, report as 3J.
C This flag applies to pesticide parameters where the identification has
been confirmed by GC/MS. Single component pesticides^lO
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
B-7
Form I
11/85
-------
Laboratory Name
Case No
Concentration: Low
Date Extracted Prepared
Date Analyzed
Conc/Dil Factor
Organics Analysis Data Sheet
(Page 2)
Semivolatile Compounds
Medium (Circle One)
Sample Number
GPC Cleanup DYes DNo
Separatory Funnel Extraction DYes
Continuous Liquid - Liquid Extraction DYes
Percent Moisture (Decanted).
CAS
Number
uglorug/Kg
(Circle One)
108-95-2
Phenoi
111 -44-4
bis(-2-Chloroethvl)Ether
95-57-8
2-Chlorophenol
541-73-1
1 3-Dichlorobenzene
106-46-7
1. 4-Dichlorobenzene
100-51-6
Benzv' Alcohol
95-50-1
1. 2-Dichlorobenzene
95-48-7
2-Methylphenol
39638-32-9
bis(2-chloroisopropyl (Ether
106-44-5
4-Methylpheno'
621-64-7
N-Nitroso-Di-n-Propylamine
67-72-1
Hexachloroethane
98-95 3
Nitrobenzene
78-59-1
Isophorone
88-75-5
2-Nitrophenol
105-67-9
2. 4-Dimethylphenol
65-85-0
Benzoic Acid
111-91-1
bis(-2-Chloroethoxy)Methane
120-83-2
2. 4-Dichlorophenol
120-82-1
1. 2, 4-Trichlorobenzene
91-20-3
Naphthalene
106-47-8
4-Chlofoaniline
87-68 3
Hexachlorobutadiene
59-50-7
4-Chloro-3-Methylphenol
91-57-6
2-Methylnaphthalene
77-47-4
Hexachlorocyclopentadiene
88-06-2
2. 4, 6-Trichlorophenol
95-95-4
2. 4. 5-Trichlorophenol
91 58-7
2-Chloronaphthalene
88-74-4
2-Nitroaniline
131-11-3
Dimethyl Phthalate
208-96-8
Acenaphthylene
99-09-2
3-Nitroaniline
CAS
Number
ug 'l or ug/Kg
(Circle One)
83 32-9
Acenaphihene
51-28-5
2. 4-Dinitrophenol
100-02-7
4-Nitrophenol
132-64 9
Dibenzofuran
121-14-2
2 4-Dmitrotoluene
606-20-2
2. 6-Dinitrotoluene
84-66-2
Diethylphthalate
7005-72-3
4-Chlorophenyl-phenylether
86-73-7
Fluorene
100-01-6
4-Nitroaniline
534-52-1
4. 6-Dinitro-2-Methylphenol
86-30-6
N-Nitrosodiphenylamine (1)
101-55-3
4-Brornophenyl-phenylether
118-74-1
Hexachlorobenzene
87-86 5
Pentachlorophenol
85-01-8
Phenanthrene
120-12-7
Anthracene
84-74-2
Di-n-Butylphrhalate
206-44-0
Fluoranthene
129-00-0
Pyrene
85-68 7
Butylbenzylphthalate
91-94-1
3, 3'-Dichlorobenzidine
56-55-3
Benzo(a)Anthracene
117-81-7
bis(2-Ethylhexyl)Phthalate
218-01-9
Chrysene
117-84-0
Di-n-Ociyl Phthalate
205-99-2
Benzo(b)Fluoranthene
207-08-9
Benzo(k )F luoranthene
50-32-8
Benzo(a)Pyrene
193-39-5
lndeno<1. 2, 3-c
-------
Laboratory Name:
Case No
Sample Number
Organics Analysis Data Sheet
(Page 3)
Pesticide/ PC Bs
Concentration Low Medium (Circle One) GPC Cleanup OYes DNo
Date Extracted 'Prepared: Separatory Funnel Extraction DYes
Date Analyzed Continuous Liquid • Liquid Extraction DYes
Conc/Dil Factor
Percent Moisture (decanted)
CAS ug/lorug/Kg
Number (Circle One)
319-84-6
Alpha-BHC
319 85-7
Beta-BHC
319-86-8
Delta-BHC
58 89-9
Gamma-BHC (Lindane)
76-44-8
Heptachlor
309-00-2
Aldrin
1024-57-3
Heptachlor Epoxide
959-98-8
Endosulfan I
60-57-1
Dieldrin
72 55-9
4,4-DDE
72-20-8
Endrin
33213-65-9
Endosulfan II
72-54-8
4. 4 -ODD
1031-07-8
Endosulfan Sulfate
50-29-3
4, 4 -DDT
72-43-5
Methoxychlor
53494-70 5
Endrin Ketone
57-74-9
Chlordane
8001-35 2
Toxaphene
12674-11-2
Aroclor-1016
11104-28-2
Aroclor-1221
11141-16-5
Aroclor-1232
53469-21-9
Aroclor-1242
12672-29-6
Aroclor-1248
11097-69-1
Aroclor-1254
11096-82-5
Aroclor-1260
V, = Volume of extract injected (ul)
Vs = Volume of water extracted (ml)
Ws = Weight of sample extracted (g)
V, = Volume of total extract (ul)
Vs orWs r—— V, V,
B-.9
Form I
7/85
-------
Laboratory Name:
Case No
Organics Analysis Data Sheet
(Page 4)
Tentatively Identified Compounds
CAS
Number
Compound Name
Fraction
RT or Scan
Number
Estimated
Concentration
(ug/l or ug/kg)
1
9
a
A
S
R
7
ft
9
in
11
19
13
14
IS
16
17
1ft
1fl
9t\
71
99
9a
9A
9R
91
?ft
99
an
Sample Number
B-10
Form I
7/85
-------
WATER SURROGATE PERCENT RECOVERY SUMMARY
Case No Contract Laboratory : Contract No.
• VOLATILE
SEMI-VOLATILE '
¦-PESTICIOE-
SMO
TRAFFIC
NO.
TOLUENE-D8
(88-110)
BFB
(86-115)
1.2 OICHLOftO-
ETNANE-04
<76*114)
NITRO-
BENZENE-OS
(35-114)
2-FLUORO-
BIPHENYL
(43-116)
TEflPHENYL-
014
(33-141)
PHEN0L-05
(10-94)
2-FLUORO-
PHENOL
(21-100)
2.4,6 TRI0ROMO"
phenol
(10-123)
~ ~
OlBUfYL-
CHLOftENOATE
(24-154)
t
* VALUES ARE OUTSIDE OF CONTRACT REQUIRED QC LIMITS Volatiles: out of ; outside of QC limits
""^ADVISORY LIMITS ONLY S6irti"Vol3tilcs! out of 5 outside of QC limits
Pesticides: out of ; outside of QC limits
Comments:
FORM II
7/85
-------
SOIL SURROGATE PERCENT RECOVERY SUMMARY
Case No . Contract Laboratory Contract No.
Low Medium
VOLATILE
--PESTICIDE--
SMO
TRAFFIC
NO.
TOLUENE-D9
(61-117)
BFB
(74-121)
1,2 OtCHLORO-
ETHANE-04
(70-121)
NITRO-
BENZENE-OS
<23-120)
2-FLUOflO-
0IPHENYL
(30-115)
TERPHENYL-
014
(18-137)
PMEN0L-05
(24-113)
2-FLUOftO-
PHENOL
(25-121)
2.4.6 TRIBROMO-
PHENOL
(19-122)
*#
OlBUTYL-
CHLORENOATE
(20-i 50)
• VALUES ARE OUTSIDE OF CONTRACT REQUIRED QC LIMITS Volatiles: out of ; outside of QC limits 7/85
^ ^ADVISORY LIMITS ONLY ScfTM Voldtilss! out of 1 outside of QC limits
Pesticides: out of ; outside of QC limits
Comments:
FORM II
-------
WATER MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Case Mo. Contractor Contract No.
FRACTION
COMPOUND
CONC. SPIKE
ADDED (ug/L)
SAMPLE
RESULT
CONC.
MS
%
REC
CONC.
MSD
%
REC
RPD
nr. i imits*
bpd
RECOVERY
VOA
SMO
SAMPLE NO.
1.1-Dichloroethene
14
61-145
Trichloroethene
14
71-120
Chlorobenzene
13
75-130
Toluene
13
78.125
Benzene
11
78-1 27
8/N
SMO
SAMPLE NO.
1,2.4-Tnchlorobeniene
28
39 98
Acenaphthene
31
46-118
2,4 Dinitroioluene
38
24 96
Pyrene
31
26-127
N-Nitroso-Di-n-^opylemine
38
41-116
1,4-Oichlorobenzene
28
36-97
ACID
SMO
SAMPLE NO.
Pentachlorophenol
50
9-103
Phenol
42
12 89
2-Chlorophenol
40
27-123
4-Chloro-3-Methylphenol
42
23-97
4-Nitrophrnol
50
10 80
PEST
SMO
SAMPLE NO.
Lindane
15
56-123
Heptachlor
20
40-131
Aldrin
22
40-J20
Dieldrin
18
52-126
Endrin
21
56-121
4,4'DDT
27
38-127
'asterisked values are outside qc limits.
RPD: VOAs out of ; outside QC limits RECOVERY: VOAi out of : outside QC limits
B/N out of ; outside QC limit! B/N out of : outside QC limiu
ACID out of : outside QC limits ACID out of ; outside QC limits
PEST out of ; outside QC limits PEST out of ; outside QC limits
Comments:
FORM III
7/85
-------
SOIL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Caaa No Contractor Contract No
Low Laval Medium Laval :
FRACTION
COMPOUND
CONC. SPIKE
ADDED (ug/Kg)
SAMPLE
RESULT
CONC.
MS
%
REC
CONC.
MSD
%
REC
RPO
_L_L_Pf
* LlMOri*
RecovERV
VOA
SMO
SAMPLE NO.
1,1 •Oicholorethene
22
59-172
Trichloroethene
24
62-137
Chlorobenzene
21
60-133
Toluene
21
59-139
Benzene
21
66-142
B/N
SMO
SAMPLE NO.
1,2,4-Tf ichlorobenzene
23
38-107
Acenaphthene
19
31-137
2.4 Dinitrotoluene
47
2889
Pyrene
36
35 142
N-Nitrosodi-n-ft-opvlamine
38
41-126
1,4-Dichlorobenzene
27
28-104
ACID
SMO
SAMPLE NO.
Pentachlorophenol
47
17-109
Phenol
35
26-90
2-Chlorophenol
50
25 102
4-Chloro-3-Methylphenol
33
26-103
4-Nitrophenol
50
11-114
PEST
SMO
SAMPLE NO.
Lindane
50
46-127
Heptachlor
31
35-130
Aldrin
43
34-132
Dieldrin
38
31-134
Endrin
45
42 139
4,4'-DDT
50
23134
"ASTERISKED VALUES ARE OUTSIDE QC LIMITS.
RPO: VOAi.
B/N_
ACID.
PEST.
Comments: _
. out of.
, out of.
. out of.
. out of.
outside QC limits
outside QC limits
outside QC limits
outside QC limits
RECOVERY:
VOAs.
B/N
ACID.
PEST.
.out of.
.out of.
.out of.
.out of.
outside QC limits
outside QC limits
outside QC limits
outside QC limits
FORM III
7/85
-------
METHOD BLANK SUMMARY
Case No. Region Contractor Contract No.
Fit 10
oatc or
analysis
FRACTION
MATRIX
CONC.
ICVCL
msr. 10
CAS NUMBER
COMPOUNO (HSL.TIC 0* UNKNOWN)
CONC.
UNITS
CROL
Comments:
FORM IV
7/85
-------
GC/MS TUNING AND MASS CALIBRATION
Bromofluorobenzene (BFB)
Case No.,
Instrument ID
Contractor
Date
Contract No.
Time
m ft
ION ABUNDANCE CRITERIA
%RELATIVE ABUNDANCE
50
15.0 • 40.0% of the base peak
75
30.0 - 60.0% of the base peak
95
Base peak, 100% relative abundance
96
5.0 - 9.0% of the base peak
173
Less than 1.0% of the base peak
174
Greater than 50.0% of the base peak
175
5.0 - 9.0% of mass 174
( )1
176
Greater than 95.0%, but less than 101.0% of mass 174
C )1
177
5.0 - 9.0% of mass 176
( )2
THIS PERFORMANCE TUNE APPLIES TO THE FOLLOWING
SAMPLES. BLANKS AND STANDARDS.
Value in parenthesis is % mass 174.
^Value in parenthesis is % mass 176.
SAMPLE ID
LAB ID
DATE OF ANALYSIS
TIME OF ANALYSIS
B-16
7/85
Form V
-------
GC/MS TUNING AND MASS CALIBRATION
Decafluorotriphenylphosphin« (DFTPP)
Case No Contractor Contract No.
Instrument ID Date Time
Lab ID Data Release Authorized By:
m/e ION ABUNDANCE CRITERIA %RELATIVE ABUNDANCE
51
30.0 - 60.0% of mass 198
68
less than 2.0% of mass 69
C D1
69
mass 69 relative abundance
70
less than 2.0% of mass 69
c y
127
40.0 - 60.0% of mass 198
197
less than 1.0% of mass 198
198
base peak, 100% relative abundance
199
5.0 • 9.0% of mass 198
275
10.0 - 30.0% of mass 198
365
greater than 1.00% of mass 198
441
present, but less than mass 443
442
greater than 40.0% of mass 198
443
17.0 - 23.0% of mass 442
C f
THIS PERFORMANCE TUNE APPLIES TO THE FOLLOWING
SAMPLES, BLANKS AND STANDARDS.
Value in parenthesis is % mass 69.
'Value in parenthesis is % mass 442.
SAMPLE ID
LAB ID
DATE OF ANALYSIS
TIME OF ANALYSIS
•
B-17
7/86
Form V
-------
Initial Calibration Data
Volatile HSL Compounds
Case No: Region; Instrument I D: .
Contractor: Calibration Date:
Contract No:
Minimum EF for SPCC is 0.300 Maximum % RSD for CCC is 30%
(0 25 for Bromoform)
Laboratory ID
Compound
RF2q
^50
RF100
rf150
rf200
R?
% RSD
CCC*
SPCC"
Chloromethane
* a
Bromomethane
Vinyl Chloride
•
Chloroethane
Methylene Chloride
Acetone
Carbon Disulfide
1. 1 -Dichloroethene
*
1, 1-Dichloroethane
* m
Trans-1. 2-Dichloroethene
Chloroform
*
1, 2-Dichloroethane
2-Butanone
1,1. 1-Trichloroethane
Carbon Tetrachloride
Vinyl Acetate
Bromodichloromethane
1. 2-Dichloropropane
m
Trans-1, 3-Dichloropropene
Tnchloroethene
Dibromochloromethane
1,1, 2-Trichloroethane
-
Benzene
cis-1, 3-Dichloropropene
2-Chloroethylvinylether
Bromoform
* *
4-Methyl-2-Pentanone
2-Hexanone
Tetrachloroethene
1, 1,2, 2-Tetrachloroethan«
* »
Toluene
*
Chlorobenzene
* »
Ethylbenzene
*
Styrene
Total Xylenes
RF -Response Factor (subscript is the amount of ug/L) CCC -Calibration Check Compounds (•)
-Average Response Factor SPCC -System Performance Check Compounds (••)
%RSD -Percent Relative Standard Deviation
B-18
Form VI
7 85
-------
Initial Calibration Data
Semivolatile HSL Compounds
(Page 1)
Case No: Region: Instrument ID: _
Contractor: ! Calibration Date:
Contract No:
Minimum RF for SPCC is 0.050 Maximum % RSD for CCC is 30%
Laboratory ID
Compound
rf20
rf50
rf80
rf120
rf160
RF
% RSD
CCC*
SPCC"
Phenol
*
bis(-2-Chloroethyl)Ether
2-Chlorophenol
1, 3-Dichlorobenzene
1, 4-Dichlorobenzene
~
Benzyl Alcohol
1, 2-Dichlort>benzene
12-Methylphenol
bis(2-chloroisopropyl)Ether
4-Methylphenol
IM-Nitroso-Di-n-Propylamine
* ~
! Hexachloroethane
Nitrobenzene
Isophorone
2-Nitrophenol
*
2, 4-Dimethylphenol
Benzoic Acid
t
bis( - 2 - Ch loroethoxy)Methane
2, 4-Dichlorophenol
1, 2, 4-Trichlorobenzene
Naphthalene
4-Chloroaniline
Hexachlorobutadiene
~
4-Chloro-3-Methylphenol
*
2-iYIethylnaphthalene
Heynchlorocyclopentadiene
* *
2, 4, 6-Trichlorophenol
*
2, 4, 5-Trichlorophenol
t
2-C.hloronaphthalene
2-Nitroaniline
t
Dimethyl Phthalate
Acenaphthylene
3-Nitroaniline
t
Acenaphthene
*
2, 4-Dinitrophenol
t
* *
4-Nitrophenol
t
* *
Dibenzofuran
Response Factor (subscript is the amount of nanograms) SPCC -System Performance Check Compounds (••)
RF -Average Response Factor t -Not detectable at 20 ng
%RSD -Percent Relative Standard Deviation
CCC -Calibration Check Compounds (.)
B-19
Form VI
10/85
-------
Initial Calibration Data
Semivolatile HSL Compounds
(Page 2)
Case No: Region: Instrument ID:
Contractor: Calibration Date:
Contract No: ;
Minimum RF for SPCC is 0.050 Maximum % RSD for CCC is 30%
Laboratory ID
Compound
rf20
o
If)
U.
ff
RF80
RF120
rf160
% RSD
CCC»
SPCC"
2, 4-Dinitrotoluene
2. 6-Dinitrotoluene
Diethylphthalate
4-Chlorophenyl-phenylether
Fluorene
4-Nitroamline
t
4, 6-Dinitro-2-Methylphenol
r
N-Nitrosodiphenylamine (1)
*
4-Bromophenyl-phenylether
Hexachlorobenzene
Pentachlorophenol
t
*
Phenanthrene
Anthracene
Oi-N-Butylphthalate
,
Fluoranthene
~
Pyrene
Butylbenzylphthalate
3. 3 -Dichlorobenzidine
Benzo(a)Anthracene
bis(2-Ethylhexyl)Phthalate
Chrysene
Di-n-Octyl Phthalate
*
Benzo(b)Fluoranthene
Benzo(k)Fluoranthene
BenzcHalPyrene
•
*
lndeno(1. 2, 3-cd)Pyrene
Dibenz(a, h)Anthracene
Benzo(g, h, i)Perylene
Response Factor (subscript is the amount of nanograms)
IP -Average Response Factor
%RSD -Percent Relative Standard Deviation
CCC -Calibration Check Compounds (•)
SPCC -System Performance Check Compounds (••)
t - Not detectable at 20 ng
(1) -Cannot be separated from diphenylamine
B-20
Form VI
7'85
-------
Continuing Calibration Check
Semivolatile HSL Compounds
(Page 1)
Region: Calibration Date:
Time:
Laboratory ID:
Initial Calibration Date:
Minimum RF for SPCC is 0.050 Maximum %D for CCC is 25%
Compound
**so
% D
CCC
SPCC
Phenol
*
bis(-2-Chloroethyl)Ether
2-Chlorophenol
1, 3-DicMorobenzene
1 4-Dichlorobenzene
~
Benzyl Alcohol
1. 2-Dichloroberzene
2-Methylphenol
bis(2-chloroisopropyl)Ether
4-Methylphenol
N-Nitroso-Di-n-Propylamine
* *
Hexachloroethane
Nitrobenzene
Isophorone
2-Nitrophenol
*
2. 4-Dimethylphenol
Benzoic Acid f
bis(-2-Chloroethoxy)Methane
2, 4-Dichlorophenol
~
1. 2. 4-Tnchlorobenzene
Naphthalene
4-Chloroanilme
Hexachlorobutadiene
*
4-Chloro-3-Methylphenol
~
2-Methylnaphthalene
Hexachlorocyclopentadiene
* #
2. 4. 6-Tnchlorophenol
*
2. 4. 5-Trichlorophenol f
2-Chloronaphthalene
2-Nitroamline t
Dimethyl Phthalate
Acenaphthylene
,3-Nitroaniline f
Acenaphthene
«
2,4-Dinitrophenol f"
» *
4-Nitrophenol f
* »
Dibenzofuran
RF^o Response Factor from daily standard file at concentration 00D -Percent Difference
indicated (50 total nanograms) CCC Calibration Check Compounds (•)
EF Average Response Factor from initial calibration Form VI SPCC System Performance Check Compounds (..)
¦J--Due to low response, analyze
at 80 total nanograms
Form VII
Case No:
Contractor:
Contract No: _
Instrument ID:
Br-21
7/85
-------
Continuing Calibration Check
Semivolatile HSL Compounds
(Page 2)
Case No:
Contractor: _
Contract No: .
Instrument ID
Minimum RF for SPCC is 0.050 Maximum %D for CCC is 25%
Regioni Calibration Date:
Time:
Laboratory ID:
Initial Calibration Date:
Compound
RF
RF50
%D
CCC
SPCC
2. 4-Oinitrotoluene
2. 6-Dinitrotoluene
Diethylphthalate
4-Chlorophenyl-phenylether
Fluorene
4-Nitroamline f
4, 6-Dinitro-2-Methylphenol |
N-Nitrosodiphenylamine (1)
~
4-Bromophenyl-phenylether
Hexachlorobenzene
Pentachlorophenol "f
*
Phenanthrene
Anthracene
Di-N-Butylphthalate
Fluoranthene
»
Pyrene
Butylbenzylphthalate
3, 3'-Dichlorot>enzidine
Benzo(a)Anthracene
bis(2-Ethylhexyl)Phthalate
1
Chrysene
Di-n-Octyl Phthalate
*
Benzo(b)Fluoranthene
Benro(k)Fluoranthene
Ber»zo(a)PYrene
*
lndeno(1,2, 3-cd)Pyrene
Dibenz(a. h)Anthracene
Benro(g. h, i)Perylene
RFjq -Response Factor from daily standard file at concentration
indicated (50 total nanograms)
RF -Average Response Factor from initial calibration Form VI
%D Percent Difference
f - Due to low response, analyze
at BO total nanograms
CCC Calibration Check Compounds (•)
SPCC System Performance Check Compounds
(1) Cannot be separated from diphenylamme
B-22
Form VII
7/85
-------
Continuing Calibration Check
Volatile HSL Compounds
Case No: Region: Calibration Date:
Contractor: Time:
Contract No Laboratory ID:
Instrument ID: Initial Calibration Date:
Minimum RF for SPCC is 0.300 Maximum %D for CCC is 25%
(0 25 for Bromoform)
Compound
RF
RF50
% D
CCC
SPCC
Chloromethane
* *
Bromomethane
Vinyl Chloride
*
Chloroethane
Methylene Chloride
Acetone
Carbon Disulfide
1. 1 -Dichloroethene
*
1, 1 -Dichloroethane
9 *
Trans-1. 2-Dichloroethene
Chloroform
*
1. 2-Dichloroethane
2-Butanone
1.1, 1-Trichloroethane
Carbon Tetrachloride
Vinyl Acetate
Bromodichloromethane
1. 2-Dichloropropane
*
Trans-1. 3-Dichloropropene
Trichloroethene
Dibromochloromethane
1.1. 2-Trichloroethane
Benzene
cts-1, 3-Dichloropropene
2-Chloroethylvinylether
Bromoform
* *
4-Methyl-2-Pentanone
2-Hexanone
Tetrachloroethene
1. 1.2. 2-Tetrachloroethane
* •
Toluene
*
Chlorobenzene
* *
Ethylbenzene
*
Styrene
Total Xylenes
RF50 -Response Factor from daily standard file at 50 ug 'I
RF -Average Response Factor from initial calibration Form VI
%D -Percent Difference
CCC -Calibration Check Compounds (•)
SPCC -System Performance Check Compounds (••)
B-23
Form VII
7/85
-------
Pesticide Evaluation Standards Summary
(Page 1)
Case No: Region: Laboratory :
Contract M«v GC Column:
Date of Analyse Instrument ID.'.
Evaluation Check for Linearity
Laboratory
ID
Pesticide
Calibration
Factor
Eval. Mix A
Calibration
Factor
Eval Mix B
Calibration
Factor
Eval Mix C
% RSD
( <10%)
Aldrin
Endrin
4.4'- DDT*1'
Dibutyl
Chlorendate
Evaluation Check for 4,4'- DDT/Endrin Breakdown
(percent breakdown.expressed as total degradation)
Laboratory
ID
Time of'
Analysis
Endrin
4.4'- DDT
Combined'2'
Eval Mix B
72 Hour
Eval Mix B
Eval Mix B
Eval Mix B
Eval Mix B
- Eval Mix B
Eval Mix B
Eval Mix B
Eval Mix B
Eval Mix B
Eval Mix B
Eval Mix B
(1) See Exhibit E, Section 7.5 4
(2) See Exhibit E, Section 7.3.1.2.2.1
B-24
Form VIII
7/85
-------
Pesticide Evaluation Standards Summary
(Page 2)
Evaluation of Retention Time Shift for Dibutyl Chlorendate
Report all standards, blanks and samples
SMO
Sample No
Lab
ID
Time of
Analysis
Percent
Diff
SMO
Sample No.
Lab
ID
Time of
Analysis
Percent
Diff
B-25
Form VIII
7/85
-------
PESTICIDE/PCB STANDARDS SUMMARY
Case No Laboratory
Contract No. QC Column QC Instrument 10
OATF OF ANAI YSIfi
r>ATF DF ANAI YSI<5
TIUF (V ANAI YSIJ5
TIUF ^ ANAI YRIR
1 ARDRATORY in
i AnnRATnoY in
COMPOUND
RT
RETENTION
TIME
WINDOW
CALIBRATION
FACTOR
CONF.
OR
QUANT.
RT
CALIBRATION
FACTOR
CONF.
OR
QUANT.
PERCENT
DIFF. »•
alpha -BHC
beta-BHC
delta - BHC
gamma-BHC
Heptachlor
Aldrin
Heptachlor Epoxide
Endosulfan I
Oieldrin
4.4'-DDE
Endrin
Endosulfan I
4.4'-DDD
Endosulfan Sulfate
4,4'-DDT
Me thoxychlor
Endrin Ketone
Tech. Chlordane
alpha-Chlordane*
gamma-Chlordane*
Toxaphene
Aroclor - 1016
Aroclor — 1 22 1
Aroclor - 1 232
Aroclor - 1 242
Aroclor - 1248
Aroclor - 1 254
Aroclot - 1 260
^ SEE EXHIBIT E PART 7 CONF. —CONFIRMATION («20% DIFFERENCE)
QUANT. =QUANTITATION C «l 5% DIFFERENCE)
FORM IX
-------
Case No.
Contract No.
P«stlcld«/PCB Identification
Laboratory
SAMPLE
ID
PRIMARY
COLUMN
PESTICIDE/
PCB
RT OF
TENTATIVE
ID
RT WINDOW
OF APPROPRIATE
STANDARD
CONFIRMATION
COLUMN
RT ON
CONFIRMATORY
COLUMN
RT WINDOW OF
APPROPRIATE
STANDARD
GC/MS
CONFIRMED
(Y or N)
4/84
FORM X
-------
RAS INORGANIC
DELIVERABLES INDEX
A. Weekly Progress Reports — Tabulation of samples received, date of receipt, and a
tabulation of problems encountered.
B. Sample Traffic Report (Original Lab Copy for Return to SMO) —Copy of SMO
Sample Traffic Report with lab receipt information and original Contractor signa-
ture.
C. Sample Data Package —Data report package for analyses of each sample (including
all required QA/QC-Exhibit E) must be complete before submission and shall
include:
1) Copies of completed SMO Sample Traffic Reports with receipt of information
completed for all samples reported in data package.
2) The cover page for the inorganic data package (Exhibit B), including general
comments, Statement of Work (SOW) Number, QC Report //, sample EPA cross
reference numbers, footnotes used in the data package, and the statement on
use of ICP background and interelement corrections for the samples. The SOW
number defines the Statement of Work used to obtain the reported values.
3) Tabulated results in ug/L for aqueous samples or mg/kg for solid samples
(identification and quantity) of specified chemical constituents (Exhibit C) by
the specified analyses (Exhibit D), validated and signed in original signature by
the Laboratory Manager, and reported on Form I.* The results for solid
samples will be reported on a dry weight basis. Percent solids are not required
on aqueous samples. If the value or the result is greater than or equal to the
Instrument Detection Limit (IDL), corrected for dilutions, as determined in
Exhibit E, report the value and indicate the analytical method used for the
metals. Use P for ICP, A for Flame AA and F for Furnace AA. All dilutions
not required by the contract and affecting the IDL, must be noted on an
element by element basis on Form I. If the value is less than the Contract
Required Detection Limits (CRDL) in Exhibit C, put the value in brackets e.g.,
DQj If the element was analyzed for but not detected, report the instrument
detection limit value with a "U" (e.g., 10U). Use an "E" as the footnote to
indicate an estimated value or value not reported due to the presence of
interference, and an explanatory note must be included on the cover page. If
the duplicate sample analysis is not within the control limits, ilag it with an
asterisk (*). Use "S" as a footnote to indicate a value determined by Method
of Standard Additions (MSA). If the correlation coefficient (r) for method of
standard additions is less than 0.995, flag the value with a plus sign (+). If
duplicate injection precision criteria specified for Furnace AA analysis in
Exhibit E cannot be met, flag the data with an "M". If . the spike sample
recovery is not within control limits, flag the data with the letter N_. Report
results to two significant figures for values from 0 to 100 and three significant
figures for results greater than 100, with the exception of
*In the event the Laboratory Manager cannot validate all data reported for each sample,
he/she will provide a detailed description of the problems associated with the sample.
B-28
-------
Mercury (see Mercury Methods — Exhibit D). For rounding rules, follow the
EPA Handbook of Analytical Quality Control in Water and Wastewater
Laboratories (EPA-600/4-79-019).
Under the comments section on Form I, provide a brief physical description of
the sample using the following guidelines:
A. Water samples — Coloration and clarity
B. Solid samples — Coloration, texture and artifacts
Recommended Descriptive Terms
Coloration: Red, blue, yellow, green, orange, violet, white, colprless,
brown, grey, black
Clarity: Clear, cloudy, opaque
Texture: Fine (powdery), Medium (sand), Coarse (large crystals or
rocks)
Also note any significant changes that occur during sample preparation (i.e.,
coloration shifts, emulsion formation).
4) Analytical results for samples and spikes, duplicates, standards, ICP Interfer-
ence Check Samples, reagent blanks, laboratory control samples, instrument
detection limits and holding times on QA Forms II, III, IV, V, VI, VII, VIII, IX
and X. Multiple forms require identification (i.e., Form IIA, Form IIB etc.).
Summarize each full method of standard addition performed on Form VIII.
5) Legible photocopy of raw data (sequential measurement readout record)
clearly labeled with sufficient information to unequivocally identify:
a) Calibration standards (including prep date).
b) Calibration blanks and preparation blanks.
c) Initial and continuing calibration verification standards and interference
check samples.
d) Diluted and undiluted samples (by EPA number) and all weights, dilutions
and volumes used to obtain the reported values. If the volumes, weights
and dilutions are consistent for all samples in a given Case, a general
statement outlining these parameters is sufficient.
e) Duplicates
f) Spikes (indicating standard solutions used, final spike concentrations, and
volumes involved).
g) Any instrument adjustments, data corrections or other apparent anoma-
lies on the measurement record, including all data voided or data not
used to obtain reported values.
B-29
-------
h) All information for furnace analysis contained in Form VIII (Exhibit E),
clearly identified on the raw data, including sample //, initial single spike
data, % recovery, full MSA data, MSA correlation coefficient, slope and
intercept of linear fit, and final sample concentration (standard addition
concentration).
6) Copies of digestion logs for the ICP, flameless AA and Hg preparations and of
the distillation log for cyanide. These logs must include: 1) date, 2) sample
weights and volumes, 3) sufficient information to unequivocally identify which
QC samples (i.e., LC5, preparation blank).correspond to each batch digested,
4) comments describing any significant sample changes or reactions which
occur during preparation, and 5) indication of pH< 2 or >12, as applicable.
7) The order of raw data in the data package shall be: 1) ICP, 2) Flame AA,
3) Furnace AA, 4) Hg, 5) CN, 6) Digestion and Distillation logs, and 7) Percent
Solids. AH raw data must include intensities (ICP) and absorbances (AA) unless
instrument direct readout is in concentration units.
8) For each reported value, the data package must contain all raw data from the
instrument used to obtain that value and the QA/QC values reported. All A A
and ICP instruments must provide a hard copy of the instrument readout (i.e.,
stripcharts, printer tapes, etc.). A photocopy of the direct instrument readout
must be included in the raw data package.
Information shall include a key to abbreviations, with response units stated and a
cross reference to EPA sample numbers.
D. Results of Intercomparison/Performance Evaluations (PE) Sample Analyses — Tabu-
lation of analytical results for intercomparison/PE sample analyses include all
requirements specified in C above.
E. Complete Case File Purge (formerly termed the "Document Control and Chain-of-
Custody Package") — The Complete Case File Purge package must include all
laboratory records received or generated for a specific case that have not been
previously submitted to EPA as deliverables. These items include, but are not
limited to: sample tags, custody records, sample tracking records, analysts logbook
pages, bench sheets, instrument readout records, computer printouts, raw data
summaries, instrument logbook pages (including instrument conditions),
correspondence and the document inventory.
Shipment of each Complete Case File Purge package by first class mail, overnight
carrier, priority mail or equivalent is acceptable. Custody seals, which are provided
by EPA, must be placed on shipping containers and a document inventory and
transmittal letter included. The laboratory is not required to maintain any
documents for a case after shipment; however, it is recommended that you maintain
a copy of the document inventory and transmittal letter.
B-30
-------
F. Quarterly Verification of Instrument Parameters — The Contractor must perform
and report quarterly verification of instrument detection limits by methods speci-
fied in Exhibit E and report type and model it for each instrument used on this
contract. For the 1CP instrumentation and methods, the Contractor must also
report quarterly: linearity range verification, interelement correction factors,
wavelengths used and integration times. This information is reported using Forms
XI, XII and XIII. Submissions of Quarterly Verification of Instrument Parameters
must include the raw data used to determine those values reported.
G. Results of Solid Laboratory Control Samples (LCS) — Tabulation of analytical results
and QC for solid LCS analysis, as specified in Exhibit E.
B-31
-------
RAS INORGANIC DATA REPORTING FORMS
B-32
-------
U.S. EPA Contract Laboratory Program
Sample Management Office
P.O. Box 818 - Alexandria, VA 22313
703/557-2490 FTS: 8-557-2490 Date
COVER PAGE
INORGANIC ANALYSES DATA PACKAGE
Lab Name Case No.
SOW No. Q.C. Report No.
Sample Numbers
EPA No. Lab ID No. EPA No.
Lab ID No.
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 time
Form I:
Value If the result is a value greater than or equal to the instrument
detecion 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), A (for Flame AA) or F (for Furnace AA).
U - Indicates element was analyzed for but not detected. Report with the
instrument detection limit value (e.g., 10U).
E - Indicates a value estimated or not reported due to the presence of
interference. Explanatory note included on cover page.
s - Indicates value determined by Method of Standard Addition.
N - Indicates spike sample recovery is not within control limits.
* - Indicates duplicate analysis is not within control limits.
+ - Indicates the correlation coefficient for method of standaird addition is
less than 0.995
M - Indicates duplicate injection results exceeded control limits.
Indicate method used: P for ICP; A for Flame AA and F for Furnace.
B-33
IFB Amend. One
-------
Form I
U.S. EPA Contract Laboratory Program
Sample Management Office
P.O. Box 81b - Alexandria, VA 22313
703/557-2490 FTS: 8-557-2490
Date
INORGANIC ANALYSIS DATA SHEET
LAB NAME CASE NO.
EPA Sample No.
SOW NO. Lab Receipt Date
LAB SAMPLE ID. NO. QC REPORT NO.
Elements Identified and Measured
Concentration: Low Medium
Matrix: Water Soil Sludge Other
ug/L or mg/kg dry weight (Circle One)
1.
Aluminum
13.
Magnesium
2.
Antimony
14.
Mangane se
3.
Arsenic
15.
Mercury
4.
Barium
16.
Nickel
5.
Beryllium
17.
Potassium
6.
Cadmium
18.
Selenium
7.
Calcium
19.
Silver
8.
Chromium
20.
Sodium
9.
Cobalt
21.
Thallium
10.
Copper
22.
Vanadium
11.
Iron
23.
Zinc
12.
Lead
Precent Solids (%)
Cyanide
Footnotes: For reporting results to EPA, standard result qualifiers are used
as defined on Cover Page. Additional flags or footnotes explaining
results are encouraged. Definition of such flags must be explicit
and contained on Cover Page, however.
Comments:
Lab Manager
IFB Amend. One
B-34
-------
Form II
Q. C. Report No.
INITIAL AND CONTINUING CALIBRATION VERIFICATION3
LAB NAME CASE NO.
SOW NO.
DATE UNITS: ug/L
Compound Initial Calib.l Continuing Calibration^
Metals:
1. Aluminum
True Value
Found
%R
True Value
Found
%R
Found
%R
Method^|
2. Antimony
3. Arsenic
4. Barium
5. Beryllium
b. Cadmium
7. Calcium
8. Chromium
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. Vanadium
j
23. Zinc
i
|
|
Other:
1
i
Cyanide
I
1
1 Initial Calibration Source 2 Continuing Calibration Source
3 Control Limits: Mercury and Tin 80-120; Other Metals 90-110; Cyanide 85-115
^ Indicate Analytical Method Used: P - IC'P; A - Flame AA; F - Furnace AA
B-35
IFB Amend. One
-------
Form III
Q. C. Report No.
BLANKS
_ CASE NO.
UNITS
Compound
Initial
Continuing Calibration
Preparation Blank
Calibration
Blank Value
Blank Value
12 3 4
Matrix:
Matrix:
1
2
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
15. Mercury
16. Nickel
17. Potassium
lb. Selenium
19. Silver
2U. Sodium
21. Thallium
22. Vanadium
23. Zinc
Other:
-¦
Cyanide
1 Reporting Units: aqueous, ug/L; solid mg/kg
LAB NAME
DATE
B-36
IFB Amend. One
-------
Form IV
Q. C. Report No.
ICP INTERFERENCE CHECK SAMPLE
LAB NAME CASE NO.
Check Sample I.D.
DATE Check Sample Source
Units: ug/L
Compound
Control Limits*
True^-
Initial
%R
Final
%R
Mean
Std. Dev.
ubse rved
Observed
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
15. Mercury
16. Nickel
17. Potassium
18. Selenium
19. Silver
20. Sodium
21. Thallium
22. Vanadium
23. Zinc
Other:
1 Mean value based on n =
2 True value of EPA ICP Interference Check Sample or contractor standard.
B-37
IFB Amend One.
-------
Form V
Q. C. Report No.
SPIKE SAMPLE RECOVERY
LAB NAME CASE NO.
EPA Sample No.
DATE Lab Sample ID No.
Units
Matrix
Compound
Metals:
1. Aluminum
Control Limit
Spiked Sample
Sample
Spiked
%ra
%R
Result (SSR)
Result (SR)
Added (SA)
75-125
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
15. Mercury
16. Nickel
17. Potassium
18. Selenium
19. Silver
20. Sodium
21. Thallium
,
22. Vanadium
23. Zinc
Other:
Cyanide
ft
1 %R = [(SSR - SR)/SA] x 100
"N"~ out of control
"NR." - Not required
Comments:
B-38
-------
Form VI
Q. C. Report No.
DUPLICATES
LAB NAME CASE NO.
EPA Sample No.
DATE Lab Sample ID No.
Units
Matrix
Compound
Control Limit *
Sample(S)
Duplicate(D)
RPD2
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
15. Mercury
16. Nickel
17. Potassium
18. Selenium
19. Silver
20. Sodium
21. Thallium
22. Vanadium
23. Zinc
Other:
Cyanide
* 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-39
-------
Form VII
Q.C. Report No.
INSTRUMENT DETECTION LIMITS AND
LABORATORY CONTROL SAMPLE
LAB NAME CASE NO. . DATE
LCS NO.
Compound
Required Detection
Instrument Detection
Lab Control Sample
ug/L mg/kg
Limits (CRDL)-ug/l
Limits (IDL)-ug/l
ICP/AA Furnace
ID# ID#
(circle one)
True Found %R
tletals:
1. Aluminum
200
2. Antimony
60
3. Arsenic
10
4. Barium
200
5. Beryllium
5
fa. Cadmium
5
7. Calcium
5000
8. Chromium
10
9. Cobalt
50
10. Copper
25
11. Iron
.100
12. Lead
5
13. Magnesium
5000
14. Manganese
15
15. Mercury
0.2
16. Nickel
40
17. Potassium
5000
18. Selenium
5
19. Silver
10
20. Sodium
5000
21. Thallium
10
22. Vanadium
50
23. Zinc
20
Other:
Cyanide
10
NR
NR
NR - Not required
B-40
-------
Form VIII
Q.C. Report No.
STANDARD ADDITION RESULTS
LAB NAME CASE NO.
DATE UNITS ug/L
EPA
Sample it
Element
Matrix
0 ADD
ABS.
1 ADD
2 ADD
3 ADD
FINAL
CON.3
r*
CON.
ABSZ
CON.
ABS.Z
CON.
ABS.Z
* Matrix abbreviations: Low Solid, LS; Medium Solid, MS; Low Aqueous, LA; Medium
Aqueous, MA.
2 CON is the concentration added, ABS. is the instrument readout in absorbance or
concentration.
3 Concentration as^ determined by MSA
*"r" is the correlation coefficient.
+ - correlation coefficient is outside of control window of 0.995.
IFB Amend. One
B-41
-------
Form IX
Q. C. Report No.
ICP SERIAL DILUTIONS
LAB NAME . CASE NO.
EPA Sample No.
DATE Lab Sample ID No.
Units ' ug/L
Matrix
Compound
Initial Sample
Concentration(I)
Serial Dilution
Result(S)
2
% Difference
Metals:
1. Aluminum
2. Antimony
3. Arsenic
4. Barium
5. Beryllium
6. Cadmium
7. Calcium
b. Chromium
y. Cobalt
10. Copper
11. Iron
12. Lead
13. Magnesium
14. Manganese
15. Nickel
lb. Potassium
17. Selenium
18. Silver
iy. Sodium
-
20. Thallium
21. Vanadium
22. Zinc
Other:
1 Diluted sample concentration corrected for 1:4 dilution (see Exhibit D)
2 Percent Difference = 1 * ~ SI x 100
I
NR - Not Required, initial sample concentration less than 10 times IDL
NA - Not Applicable, analyte not determined by ICP
B-42
IFB Amend. One
-------
Form X
QC Report No.
HOLDING TIMES
LAB NAME
DATE CASE NO.
EPA
Sample No.
Matrix
Date
Received
Mercury
Prep Date
Mercury
Holding Time *•
(Days)
CN Prep
Date
CN
Holding Time*
(Days)
^Holding time is defined as number of days between the date received and the
sample preparation date.
IFB Amend One.
B-43
-------
Form XI (Quarterly) •
INSTRUMENT DETECTION LIMITS
LAB NAME DATE
ICP/Flame AA (Circle One) Model Number Furnace AA Number
Element
Wavelength
(nm)
CRDL
(ug/L)
IDL
(ug/L)
Element
Wavelength
(nm)
CRDL
(ug/L)
IDL
(ug/L)
1. Aluminum
200
13. Magnesium
5000
2. Antimony
60
14. Manganese
15
3. Arsenic
10
15. Mercury
0.2
4. Barium
200
16. Nickel
40
5. Beryllium
5
17. Potassium
5000
6. Cadmium
5
18. Selenium
5
7. Calcium
5000
19. Silver
10
8. Chromium
10
20. Sodium
5000
9. Cobalt
50
21. Thallium
10
10. Copper
25
22. Vanadium
50
11. Iron
100
23. Zinc
20
12. Lead
5
Footnotes: • Indicate the instrument for which the IDL applies with a "P" (for ICP),
an "A" (for Flame AA), or an "F" (for Furnace AA) behind the IDL value.
• .Indicate elements commonly run with background correction (AA) with
a "B" behind the analytical wavelength.
• If more than one ICP/Flame or Furnace AA is used, submit separate
Forms XI-XIII for each instrument.
COMMENTS:
Lab Manager
B-44
-------
Form XII (Quarterly)
ICP Interelement Correction Factors
LABORATORY ICP Model Number
DATE
Interelement Correction Factors
for
Analyte
Analyte
Wavelength
(nm)
A1
Ca
Fe
Mg
1. Antimony
2. Arsenic
3. Barium
4. Beryllium
5. Cadmium
6. Chromium
7. Cobalt
8. Copper
9. Lead
10. Manganese
11. Mercury
12. Nickel
13. Potassium
14. Selenium
15. Silver
16. Sodium
17. Thallium
18. Vanadium
19. Zinc
COMMENTS:
Lab Manager
B-45
-------
Form XII (Quarterly) (cont'd)
ICP Interelement Correction Factors
LABORATORY_
DATE
ICP Model Number
Interelement Correction Factors
for
Analyte
Analyte
Wavelength
(nm)
1. Antimony
2. Arsenic
3. Barium
4. Beryllium
5. Cadmium
6. Chromium
7. Cobalt
8. Copper
9. Lead
10. Manganese
11. Mercury
12. Nickel
13. Potassium
14. Selenium
15. Silver
16. Sodium
17. Thallium
18. Vanadium
19. Zinc
COMMENTS:
Lab Manager
B-46
-------
Form XIII (Quarterly)
ICP Linear Ranges
LAB NAME ICP Model Number
DATE
Analyte
Integration
Time
(Seconds)
Concen-
tration
(ug/L)
Analyte
Integration
Time
(Seconds)
Concen-
tration
(ug/L)
1. Aluminum
13. Magnesium
2. Antimony
14. Manganese
3. Arsenic
15. Mercury
4. Barium
16. Nickel
5. Beryllium
17. Potassium
6. Cadmium
18. Selenium
7. Calcium
19. Silver
8. Chromium
20. Sodium
9. Cobalt
21. Thallium
10. Copper
22. Vanadium
11. Iron
23. Zinc
12. Lead
Footnotes: • Indicate elements not analyzed by ICP with the notation "NA".
COMMENTS:
Lab Manager
B-47
-------
RAS DIOXIN
DELIVERABLES INDEX
I. Case Narrative
The case narrative oust contain: Case number; contract number; summary
of any QC, sample, shipment, and analytical problems; and documentation
of all Internal decision tree processes used. Outline problems encoun-
tered and final solutions. Be as specific and detailed as necessary.
II. Tabulated Data (Form B-l to Form B-4)
III. Standard Data By Instrument
A) All quantitation reports, and SIM mass chromatgrams for concentration
calibration solutions
1. Organized in order: Triplicate runs of CC1
Triplicate runs of CC2
Triplicate runs of CC3 etc.
B) All quantitation reports, and SIM mass chromatograms for routine
calibration
1. Performance check solutions organized in chronological order
2. Concentration calibration solution #1 organized in chronological
order
IV. Sample Data
A) All quantitation reports, and SIM mass chromatograms for method
blank(s) organized in chronological order
B) All quantitation reports, and SIM mass chromatograms for samples
(organized by increasing EPA number)
V. Chain of Custody and In House Laboratory Control Documents
A) EPA Chain of Custody Records
B) SMO Dioxln Shipment Records
C) Sample Log-in Sheets
D) In-House Dioxln Bench Sheet
E) GC/MS Standard and Sample Run Logs
B-4 8
-------
RAS DIOXIN DATA REPORTING FORMS
B-49
-------
FORM B-1S. TCDD SOIL DATA REPORT FORM
Page 1 of 2
Lab: Report Date:
Case/BaCch No:__ Column:
Instrument ID:
EPA
Sample No.
Extr.
Date
Wet wt
ug/kg
Meas.
TCDD
MPC
GC/MS Analysis
Surr.
S/N Ratio
*
Z REC(IS)
Date
Time
MB =
Method Blank
FB
-
Field Blank
N -
Native TCDD Spike
IS
-
Internal Standard
D -
Duplicate/Fortified Field Blank
RR
-
Rerun
PE -
EMSL-LV Performance Evaluation Sample'
RS
-
Recovery Standard
MPC -
Maximum Possible Concentration
ND
m
Not Detected
*Note:
Relative to Cjj-l>2,3,4-TCDD
9/86
B-50
-------
Lab:
Case/Batch No:
Instrument ID:
FORM B-1S. TCDD SOIL DATA REPORT FORM
Report Date:_
Column:
Page 2 of 2
Rel.
EPA Response Ratios Response (Area)
Sample
Number
320/
322
332/
334IS
332/
334RS
259
320
322
328
332IS
334IS
332RS
334RS
•
•
i
i
MB -
Method Blank
FB -
Field Blank
N -
Native TCDD Spike
IS -
Internal Standard
D -
Duplicate/Fortified Field Blank
RR -
Rerun
PE =¦
EMSL-LV Performance Evaluation Sample
ND -
Not Detected
MPC -
Maximum Possible Concentration
RS -
Recovery Standard
9/86
B-51
-------
FORM B-1W. TCDD WATER DATA REPORT FORM Page 1 of 2
Lab: Report Date:
Case/Batch Ho: Column:
Instrument ID:
EPA
Sample No*
Extr.
Date
volume
ng/L
Meas.
TCDD
MPC
GC/MS
Date
Analysis
Time
Surr.
S/N Ratio
*
Z REC(IS)
•
MB -
Method Blank
FB -
Field Blank
N -
Native TCDD Spike
IS -
Internal Standard
D -
Duplicate/Fortified Field Blank
RR -
Rerun
PE -
EMSL-LV Performance Evaluation Sample
RS -
Recovery Standard
MPC -
Maximum Possible Concentration
ND -
Not Detected
~Note:
Relative to ^C^-l »2,3,4-TCDD
9/86
B-52
-------
FORM B-1W.
TCDD WATER DATA REPORT FORM
Page 2 of 2
Lab:
Case/Batch No:
Instrument ID:
Report Date:
Column:
Rel.
EPA Response Ratios Response (Area)
Sample
Number
320/
322
332/
33AIS
332/
334RS
259
320
322
328
332IS
334IS
332RS
334RS
•
MB -
Method Blank
FB
m
Field Blank
N -
Native TCDD Spike
IS
m
Internal Standard
D -
Duplicate/Fortified Field Blank
RR
-
Rerun
PE -
EMSL-LV Performance Evaluation Sample
ND
-
Not Detected
MPC -
Maximum Possible Concentration
RS
-
Recovery Standard
9/86
B-53
-------
A. TODD REPORT FORM (Form B-l)
This form is used for tabulating and reporting case results.
Complete the header information at the top of the page including instru-
ment ID, laboratory name, case/batch number, report date, and column used.
EPA sample number is tabulated along with date sample was extracted, and
weight (wet) extracted to the nearest tenth (0.1) of a gram or volume extracted
(water) to the nearest 10 milliliters.
Calculate the concentration of 2,3,7,8-TCDD using the formula:
Ax • QlS
Ais . RRFgj . U
Cx = 2,3,7,8-TCDD concentration in ug/kg or ug/L
Ax = the sum of integrated ion abundance detected for m/z 320
and 322
Ais = the sum °f integrated ion abundances detected for m/z 332
and 334 (characteristic ions of Cj^-2,3 ,7,8-TCDD the
internal standard).
Q^s ™ quantity (in ng) of ^C^-2,3,7,8-TCDD added to the sample
before extraction
RRFn '=" calculated mean response factor for unlabeled 2,3,7,8-TCDD
relative to C12"2,3,7,8-TCDD
W = The weight (in g) of soil/sediment extracted or volume of
water extracted (in mL)
Positive samples are quantitated with values >10.0 ug/kg or 100 ng/L
recorded to three (3) significant figures and those values <10.0 ug/kg or
100 ng/L reported to two (2) significant figures.
For samples in which unlabeled 2,3,7,8-TCDD was not detected calculate
the estimated maximum possible concentration, which is the concentration
required to produce a signal with a peak height of 2.5 times the background
signal height.
Use the formula:
2.5 . Hx . Qis
Hls . RRFn . W
where: MPC = maximum possible concentration of unlabeled 2,3,7,8-TCDD
required to produce Hx.
B-54
-------
Hx - peak height for m/z 320 or 322 In Che same group
of >5 scans used to measure
Hls " peak height for the appropriate ion characteristic of the
internal standard, m/z 332 when 320 is used to determine Ax,
and m/z 334 when 322 is used to determine Ax.
Qls - quantity (in ng) of i2~2,3,7,8-TCDD added to the
sample before extraction.
RRFn ¦ calculated mean response factor for unlabeled 2,3,7,8-TCDD
relative to "X^2-2,3,7,8-TCDD.
W ¦ weight (in g) of wet soil/sediment sample or volume of water
extracted (in mL).
Report GC/MS Instrument ID, the date and time the analysis was performed,
and the signal to noise ratio for the surrogate compound.
B-55
-------
FORM B-2
Page 1 of 2
INITIAL CALIBRATION SUMMARY
Laboratory: ______________________________ CC Solution Alternative:
Case/Batch No.: Instrument ID:
AREA
Date
Time
Sol.
ID
320
322
328
332IS
33AIS
332RS
33ARS
CC1
CC1
CC1
CC2
CC2
CC2
CC3
CC3
CC3
*
CCA
CCA
CCA
t /
t /
/
/ t
/ t
Solution ID Codes:
CC1Concentration calibration solution #1 * Not present In CC Solution
CC2 - Concentration calibration solution #2 Alternative One.
CC3 - Concentration calibration solution #3
CCA - Concentration calibration solution #A
B-56
9/86
-------
FORM B-2 Page 2 of 2
INITIAL CALIBRATION SUMMARY
Laboratory: CC Solution Alternative:
Case/Batch No.: Instrument ID:
Date
Time
Sol.
ID
Measured
RRFn
Mean
RRFn
Measured
RRFi
Mean
RRF.i
CC1
CC1
CC1
CC2
CC2
CC2
CC3
CC3
CC3
CCA
CC4
CC4
Solution ID Codes:
CC1 - Concentration calibration solution 01
CC2 - Concentration calibration solution #2
CC3 - Concentration calibration solution #3
CC4 - Concentration calibration solution #4
ZRSD: RRFn RRF^
CC1=»
CC2-
CC3-
CC4-
9/86
Native Mean IS Mean
of Means: of Means:
B-57
-------
B. Initial Calibration Summary (Form B-2)
Record all routine calibrations (PCS and CC1) performed during initial
calibration on form B-3.
Complete all header information including laboratory, case/batch number,
and instrument ID and EPA CC Solution Alternative.
Date and time along with response for each ion is recorded for each cali-
bration solution. The response factors are calculated with the following
equations:
RRFn (native Response Factor) RRF^ (internal Standard Response Factor)
• Qis ^is * Qrs
RRFn = RRFj =
Ais • Qn Ars . Q^s
Where:
Ax = the sum of integrated ion abundance of m/z 320 and 322 for unlabeled
2,3,7,8-TCDD
Ais = t£e sum integrated ion abundancces of m/z 332 and m/z 334 for
C12"2'3'7'8"TCDD
Ars = the sum of integrated ion abundance of m/z 332 and m/z 334 for
1 C12"1»2»3»4~TCDD
Qn = quantity of unlabeled 2,3,7,8-TCDD injected
Q^s = quantity of *3Cj2-2,3,7,8-TCDD injected
Qrs » quantity of 13C12-1,2,3,4-TCDD
Calculate the mean RRF and the percent relative standard deviation for the
triplicate runs of each calibration solution.
SD
%RSD = -- x 100
X
B-58
-------
Where:
SD
JJilL~-—-
*1-1 N - 1
X = mean of each of the three Response Factors respectively
From the A mean native response factors and A mean internal standard
response factors: calculate the mean of means for each respective RRF's.
B-59
-------
FORM B-3
ROUTINE CALIBRATION SUMMARY
Laboratory: ^Solution Alternative:
Case/Batch No.: _______________________________ Instrument ID:
(CC1)
(PCS)
PERFORMANCE CRI
:ck SOL.
CON. CALIB. SOL. 01
Date
Time
Response
259
320
322
328
332IS
334IS
332RS
334RS
Ratios
320/322
332/334IS
332/334RS
RRPn
-
-
RRF-r
Z Valley
9/86
B-60
-------
C. Routine Calibration Summary (Form B-3)
Complete the header information including the laboratory, instrument ID
Case/Batch number and EPA CC Solution Alternative.
For each performance check solution analyzed complete the date and time
of analysis, the response for m/z 259, 320, and 322 for unlabeled 2,3,7,8-
TCDD, 328 for 37Cl4-2,3,7,8-TCDD, and 332 and 334 for C12-2,3,7,8-TCDD
and 13C12-1,2,3,4-TCDD.
Ion ratios for m/z 320/322, m/z 332/334 for ^3C22-2,3,7,8-TCDD and m/z
332/334 for *3C^2-1,2,3,4-TCDD are to be calculated and recorded.
Response factors are to be calculated as in the Initial Calibration Summary
(Section B). '
For calculation of valley percent see Section D, Section 9.2.6.1.
For each Concentration Calibration Solution #1 used in Routine Calibration,
complete all the above information.
B-61
-------
FORM B-A
QUALITY CONTROL SUMMARY
Laboratory Name
Case/Batch No.
Instrument ID
Accuracy, Fortified/
Spike Field Blank:
Relative Difference (%),
Duplicate Analysis:
SOIL
WATER
EPA Sample Number:
EPA Sample Number:
Accuracy, Fortified/
Spike Field Blank:
Relative Difference (%),
Duplicate Analysis:
EPA Sample Number:
EPA Sample Number:
B-62
9/86
-------
0. QC Summary
Complete all the header information.
Report the sample number for the fortified field blank and the % accuracy
of the fortified/spike field blank by using the following equation:
amount measured
Z accuracy = x 100
1.0
Record the sample used for duplicate and the Relative Percent Difference
which is calculated as follows:
|Sl - s2|
RPD = x 100
Si - S2
2
Where:
Sj^ and S2 represent sample and duplicate sample results.
B-63
-------
APPENDIX C
SAMPLE INFORMATION AND DOCUMENTATION
C-l
-------
ORGANIC SAMPLE COLLECTION
REQUIREMENTS
WATER SAMPLES
EXTRACTABLE ANALYSIS
(LOW LEVEL)
EXTRACTABLE ANALYSIS
(MEDIUM LEVEL*)
VOLATILE ANALYSIS
(LOW OR MEDIUM LEVEL*)
REQUIRED
VOLUME
1 GALLON
1 GALLON
80 ML
A
A.
A
CONTAINER TYPE
1 x 4-LITER AMBER
GLASS BOTTLES
OR
2 x 80-OZ. AMBER
GLASS BOTTLES
OR
4 x 1 -LITER AMBER
GLASS BOTTLES
00
4 x 32-OZ. WIDE-MOUTH
GLASS JARS
2 x 40-ML GLASS VIALS
SOIL/SEDIMENT SAMPLES
EXTRACTABLE ANALYSIS
(LOW OR MEDIUM LEVEL*)
REQUIRED
VOLUME
6 OZ.
on
CONTAINER TYPE
1 x 8-OZ. WIDE-MOUTH
GLASS JAR
OR
2 x 4-OZ. WIDE-MOUTH
GLASS JARS
VOLATILE ANALYSIS
(LOW OR MEDIUM LEVEL*)
240 ML
00
2 x 120-ML WIDE-MOUTH
GLASS VIALS
*ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT ^
$ )
x
C-2
-------
INORGANIC SAMPLE COLLECTION
REQUIREMENTS
WATER SAMPLES
METALS ANALYSIS
(LOW LEVEL)
METALS ANALYSIS
(MEDIUM LEVEL*)
REQUIRED
VOLUME
1 LITER
16 OZ.
A
CONTAINER TYPE
1 x 1-LITER
POLYETHYLENE BOTTLE
1 x 16-OZ. WIDE-MOUTH
GLASS JAR
CYANIDE (CN~) ANALYSIS
(LOW LEVEL)
CYANIDE (CN ) ANALYSIS
(MEDIUM LEVEL*)
1 LITER
16 OZ.
n
1 x 1-LITER
POLYETHYLENE BOTTLE
1 x 16-OZ. WIDE-MOUTH
GLASS JAR
SOIL/SEDIMENT SAMPLES
METALS AND CYANIDE (CN")
ANALYSIS
(LOW OR MEDIUM LEVEL*)
REQUIRED
VOLUME
6 OZ.
CONTAINER TYPE
1 x 8-OZ. WIDE-MOUTH
GLASS JAR
OR
2 x 4-OZ. WIDE-MOUTH
GLASS JARS
~ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT
i
9
w
X
C-3
-------
DIOXIN SAMPLE COLLECTION
REQUIREMENTS
WATER SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
2,3.7.8-TCDD
ANALYSIS
(MULTI-CONCENTRATION)
2 LITERS
A
2 x 1-LITER AMBER
GLASS BOTTLES
SOIL/SEDIMENT SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
a
2.3,7,8-TCDD 4 OZ.
1 x 4-OZ. WIDE-MOUTH
ANALYSIS
—
GLASS JAR
(MULTI - CONCENTRATION)
OR
1 x 8-OZ. WIDE-MOUTH
GLASS JAR
HIGH HAZARD SAMPLE COLLECTION
REQUIREMENTS
LIQUID OR SOLID SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
ORGANIC AND INORGANIC 6 OZ.
1 x 8-OZ. WIDE-MOUTH
ANALYSIS
GLASS JAR
•ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT
C-4
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
CLP Sample Management Office
P.O. Box 818 - Alexandria, Virginia 22313
Phone: 703/557-2490 - FTS/557-2490
SAS Number
SPECIAL ANALYTICAL SERVICES
Client Request
1 1 Regional Transmittal
A. EPA Region/Client:
B. RSCC Representative:
C. Telephone Number: ( )
D. Date of Request:
E. Site Name:
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:
~
Telephone Request
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 Superfund (enforcement or remedial action),
RCRA, NPDES, etc.):
-------
4. Estimated date(s) of collection:
5. Estimated date(s) and method of shipment:
6. Number of days analysis and data required after laboratory receipt of samples:
— — t
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:
Phone: ( )
C-6
-------
12. Data Requirements
Precision Desired
Parameter Detection Limit (-% or Concentration)
13. QC Requirements
Limits
Audits Required Frequency of Audits (Percent or Concentration)
14. Action Required if Limits are Exceeded
Please return this request to the Sample Management Office as soon as possible to
.expedite processing of your request- fpr special analytical services. Should you have any
questions or need any assistance, please contact your Regional representative at the
Sample Management Office.
C-7
-------
CONTRACT LABORATORY PROGRAM
RAS RE-ANALYSIS REQUEST/APPROVAL RECORD
t
SECTION A
01. Case No. SAS No. //2. DPO or RSCC
V3. Details of Re-Analysis Request:
o Laboratory Name:
o Sample No(s). + Fraction(s):
o Reason for Re-Analysis:
o Procedure for Re-Analysis:
0 Name of PO Contacted: . Date / /
REQUEST: Approved Not Approved
RE-ANALYSIS: Billable Not Billable
05. Name of SMO Contact: Date / /
SECTION B (TO BE COMPLETED BY SMO)
01. Date of Laboratory Notification (Verbal) / / •
02. Re-Analysis Start Date / / 03. Data Due Date / /
SECTION C (PROJECT OFFICER CONCURRENCE)
Concurrence By Date / /
Project Officer Signature
Return intact form to:
Sample Management Office
P.O. Box 818
Alexandria, Virginia 22313
Distribution: (l) POCopy (2) DPO/RSCC Copy (3) SMO FUe Copy (4) Lab Copy
7/22/86
C-8
-------
CONTRACT LABORATORY PROGRAM
SAS RE-ANALYSIS REQUEST/APPROVAL RECORD
SECTION A
V1. SAS No. 112. DPO or RSCC
//3. Details of Re-Analysis Request:
o Laboratory Name;
o Sample No(s). + Parameter(s):
o Reason for Re-Analysis:
o Procedure for Re-Analysis:
#**. Name of SMO Contact: Date / /
REQUEST: Approved Not Approved
RE-ANALYSIS: Billable Not Billable
SECTION B (TO BE COMPLETED BY SMO)
//I. Date of Laboratory Notification (Verbal) / /
H2. Re-Analysis Start Date / / #3. Data Due Date / /
SECTION C (COORDINATOR CONCURRENCE)
Concurrence By Date / /
SMO Coordinator Signature
Return intact form to:
Sample Management Office
P.O. Box 818
Alexandria, Virginia 22313
Distribution: (1) DPO/RSCC Copy (2) SMO File Copy (3) Lab Copy
7/22/86
C-9
-------
SAMPLE DOCUMENTATION
C-10
-------
* Form to be revised
)
U.S. ENVIROI^MENTAL PROTECTION AGENCY HW Sample Management Office.:;
';:'PO.B3x818:A]ey:Xid':a.:VL-r!inic:22313 - 7CS: b57-M93*rrSv55V-2-190 ¦'
ORGANICS TRAFFIC REPORT
Sample Number
0 Cass Number
Sample Site Name/Code:
(D SAMPLE CONCENTRATION
(Check One)
Low Concentration
Medium Concentration
(D SAMPLE MATRIX
(Check One)
Water
Soil/Sediment
© Ship To:
Attn:
Transfer
Ship To:
(D Regional Office:
(D For each sample collected specify number
of containers used and marie volume level
on each bottle.
(Name)
Number of
Containers
(Phone)
Sampling Date:
Water
(Extractable)
(Begin)
(End)
Water
(VOA)
© Shipping Information
Name of Carrier
Date Shipped:
Airbill Number
Soil/Sediment
Water
(Ext/VOA)
Other
Approximate
Total Volume
® Sample Description
Surface Water
Ground Water
Leachate
(D Sample Location
Mixed Media
Solids
Other (specify).
© Special Handling Instructions:
(e.g.. safety precautions, hazardous nature)
SMOOOPY
C-ll
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY HW1 Sample Management Office
:^P.O. Box818.Alexcmdrio.-Viiginia22313 - 703: SS7:2490- ITS 557 2^
)S2i ORGANICS TRAFFIC KEPORT Bfil'W
(7) Case Number:
5*8^
Sample Site Name/Code:
"fcfcMfA SmrC
SMALL TOuiJj M£
1
(D SAMPLE CONCENTRATION
(Check One)
^ Low Concentration
Medium Concentration
(D SAMPLE MATRIX
(Check One)
X Water
Soil/Sediment
0 Ship To:
/JNAL.
/OO AJ/9rAJ ST
Attn:£C MSSP£C_
TVansfer
Ship To:
(D Regional Office: S3Z.
Sampling Personnel:
Tfc£ SdMPt££
i (Name)
&/7/««r£-swa/SL
(Phone)
Sampling Date:
<1/9. -«/
-------
*Form to be revised
t®
? U.S. ENVIRONMENTAL PROTECTION AGENCY : HW1 Sample Management Office
: P.O. Box 818 Alexandria.VA22313-703/&57-2490 -FTS 557-2490
INORGANICS TRAFFIC REPORT
Sample Number
(?) Cm* Number:
S«mpl» Site Name/Code:
0 Sampling Office:.
Sampling Personnel:
(Name) _____
(Phone)
Sampling Date:
(Beoin)
(End)
©Sample Description:
(Check One)
— Surface Water
—— Groundwater
— Leachate
Mixed Media
____ Solids
_____ Other
(specify)
MATCHES ORGANIC SAMPLE NO.-
0 SAMPLE CONCENTRATION
(Check One)
Low Concentration
Medium Concentration
® SAMPLE MATRIX
(Check One)
Water
—— Soil/Sediment
(7) Shipping Information:
Name Of Carrier:
Date Shipped:.
Airbill Number:
0 Mark Volume Level
On Sample Bottle
Check Analysis required
.Total Metals
(?) Ship To:
Attn:
Tranafar
Ship To:
C-13
-------
<£s>
US. ENVIRONMENTAL PROTECTION AGENCY HWI Sample Management Office
P.O. Box 81 b. Alexandna, VA 22313-703 /557-2490 • FTS /557-2490
INORGANICS TRAFFIC REPORT
Sample Number
MAA ooi
Sample Site Name/Code:
TlftMM STTF
<>MALi.7CXjJtJ
*o/
0 SAMPLE CONCENTRATION
V (Check One)
** Low Concentration
Medium Concentration
® SAMPLE MATRIX
^ (Check One)
A Water
Soil/Sediment
0 Ship To:
METALS
lo=> MAT^ STREET
A^yTCKoOjC^ WH|
Ihnitar
Ship To:
Sampling Perronnel:
(PhM*)
Rumplmj Date:
(Beam) tljl (End) Uft/jfto
0 Shipping Information:
Name Of Carrier:
PfefteeAt. fcxPKES*
Date Shipped: If j^ j S(o
AirhmNumharr 1 ^ Vb fc 7
0 ANALYSIS LAS:
Reed by:
n>toHorrl'
@
Sample Condition
On Receipt:
(eg. broken, leakage, chain of custody, etc.)
/j\ Sample Description:
^ (Check One)
Surface Water
/> Groundwater
. Leachate
___ Mixed Media
® Mark Volume Level
On Sample Bottle
Check Analysis required
X Total Metals
2-Qjnnlde
(specily) . .
MATCHES ORGANIC SAMPLE NO**W|
C-14
-------
* Form to be revised
USEPA Contract Laboratory Program
Sample Management Office
P.O. Box 618 Alexandria. Virginia 22313
FTS 8-557-2490 703/557-2490 C|J> D|OX|N SHIPMENT RECORO
Site Name:
City & State:
EPA Site Spill I.D.:
Tier: 12 3 4 5 6 7
(rirrlp nnp)
Instructions: 1) Ship all samples as Medium level, in paint cans
2) Send rlnsate samples In TCE or hexane organic solvents.
3) Sample Requirements: Soll/Scd: G ox./sample In glass Jar
Aqueous: 2 Liters/sample In amber glass. Send one 4 Liter
sample/batch for lat» QC.
MATRIX
DESCRIPTION
SAS ONLY
SAMPLE
NUMBERS
SOIL/ f
SEDIMENT 1
S
o
W
sr
EQUIP RINS
(ORG SOLV)
OTHER ¦§
(SAS ONLY) h
0>
o c
H O
W
W UM
4-S MO
o. cuo>
r cnc
< V
tA
SAMPLE TO
DUPLICATE
(check- one)
SAMPLE
LOCATION
(or other
field desc)
SPECIFY
ADDITIONAL
SAS
ANALYSES
paramaters)
•
WHITE—SMO Copy YELLOW—Region Copy PINK—Lab Copy tor Return to SMO COLO—Lab Copy
C-15
-------
USEPA Contract Laboratory Program
Sample Management Office
P.O. Box 818 Alexandria. Virginia 22313
FTS 8-557-2490 703/557-2490
Site Name:
RUSTW bPUM S\Tb
City & State:
RuftUv'iilf..) Pfl-
EPASrtfe Spill I.D.:
3-4
Tier
2 3 4 5 6 7
n"°)
Instructions: 1) Ship all saspies as Medlus level, in paint cans
2) Send rlnsate samples in TCE or hexane organic solvents.
3) Sample Bequlreafents: Soil/Sed: 4 ox./sample In glass jar
Aqueous: 2 Liters/sample In amber glass. Send one * Liter
sample/batch for lab QC.
"matrix
Region Number
Sampling Contact
"3oe SttmplffV a&oc!
^ n ¦ //
(name)
Sampling Date:
SAMPLE
NUMBERS
SOIL/ I
SEDIMENT I
s
o
10
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<
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(ORG SOLV)
A
1*2 O
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(check, one)
SAMPLE
LOCATION
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field desc)
I
SPECIFY
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SAS
ANALYSES
parameters)
t)DOl\X O I
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t>T>oit ^ oX
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WHITE—SMO Copy YELLOW—Region Copy PINK—Lab Copy lor Return to SMO GOLD—Lab Copy
C-16
-------
* Form to be revised
A \
$81]
vPO. Bo* 818—AlexArdna Virginia 22313 Phone 703^'Sd/-249C-FTS'557-2490
FIELD SAMPLE RECORD
(D Case Number
Sample Site Name/Code:
© Fiekl Sample Description:
Drum
Aqueous Liquid
_Oi
_ Other.
(3) Ship To:
Attn:
(?) Sampling Office:
(D Known or Suspected Hazards:
Sampling Personnel:
(name)
(phone)
Sampling Date:
(becpn;
(end)
(Z) Preparations Requested:
(check below)
Sample Volume:
® Shipping Information:
(name of carrier)
(date shipped)
. Volatile Organics
. Bases/NeutoaL Aod.
TCDD
. Pestades, PCB
. Inoiganks
. Total Metals
. Total Mercury
. Strong Acid Anions
(airbl number)
(D Sample I /nation:
(D Special Handling hstruotians:
SMOCopy
C-17
-------
US. ENVIRONMENTAL PROTECTION AGENCY CLP Sample Management Office
PO.Bcot 6!8-Atecand-a, VrgmB 22313 fticre 703^557-2490-FTS/557-2490 .
FIELD SAMPLE RECORD
(D Cass Number
/«
Sample Site Name/Code:
DuMP /nan
XDrum
—Aqueous Liquid
_Sbdge
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© ShqjTb:
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-tf:
© Known cr Suspected Hazards:
© Sample Location
6 7
rKtocx^nJB
2L foagamcB
jC Total Metals
jL Total Mercury
_a£Strcng Aad Aiions
i ^A/ ^^i(VWfi'cn
< SulP•«!* f "a f.Vmu f.crt
® Special Handling Institutions:
C-18
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
CLP Sample Management Office
P.O. Box 818 - Alexandria, Virginia 22313
Phone: 703/557-2W0 - FTS/557-2490
SPECIAL ANALYTICAL SERVICE
PACKING LIST
Sampling Office:
Sampling Date(s):
Ship To:
For Lab Use Only
Sampling Contact:
Date Shipped:
Date Samples Rec'd:
(name)
Site Code:
Attn:
Received By:
(phone)
Sample
Numbers
1.
Sample Description
i.e., Analysis, Matrix, Concentration
Sample Condition on
Receipt at Lab
2
3
\
5
6
7
8
9
10
11
12
13
14
18 .
19. '
20.
For Lab Use Only
White - SMO Copy, Yellow - Region Copy, Pink - Lab Copy for return to SMO, Gold - Lab Copy
SAS Number
C-19
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
CLP Sample Management Office
P.O. Box 818 - Alexandria, Virginia 22313
Phone: 703/557-2090 - FTS/557-2W0
SPECIAL ANALYTICAL SERVICE
PACKING LIST
Sampling Office:
X*
Sampling Date(s):
~//a -
Ship To:
SAS LAS
IOC* StZEET
A'J Y TOixwJ, CO
s*765*
Attn: TP secveics
For Lab Use Only
Sampling Contact:
vTXM SAMPl££
Date Shipped:
Date Samples Rec'd:
(name)
Co 11 /5?S-/W>
Site Code:
^ nl
Received By:
' (phone)
Sample
Numbers
1. foooA -o |
Sample Description
i.e., Analysis, Matrix, Concentration
loco uiATtre
Sample Condition on
Receipt at Lab
2. lOOOrt *oa
w
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3. /©o
-------
Custody Seal
^ ateq | ZZKS f
a»eq 8
U~<&T -S
1V3S Aaoisno
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CUSTODY SEAL
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Protect Cod*
wbS 3/o.col
Station Na
Month/O«y/VMT
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Grab
Simpler* {Signature*)
8
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(A
W
w
-------
ENVIRONMENTAL PROTECTION AGENCY
Office of Enforcement
CHAIN OF CUSTODY RECORD
3
PROJ. NO.
project name (use site code only)
NO.
OF
CON-
TAINERS
nEMABKS
SAMPLERS: ISignatunl
STA.NO.
DATE
TIME
i
I
STATION LOCATION
Relinquished by: ISlgmturtl
Date /Tim*
Received by: (Sign*tun)
Relinquished by: tSiintnm)
Date / Time
Received by: ISitrvn/rr)
Relinquished by: tSitnttvnl
Date /Time
Received by: (Sitntturti
Relinquished by: fSignttunl
Date/Time
Received by: ttigmtunl
Relinquished by: ISigntur*!
Date /Time
Received for Laboratory by:
(Slftturt)
Oate /Time
Distribution: Origin* Accompanies Shipment; Copy to Coordinator Field Filet
Remarks
0602
-------
ENVI RONMEfclTAL PROTECTION AGENCY
Office of Enforcement
CHAIN OF CUSTODY RECORD
PROJ. NO.
2097
'ROJECT name (use site code only)
^COlZL
NO.
OF
CON-
TAINERS
/ /V//// km# a S2.&7
/*/y//// zo77
/ / y / / / / REMARKS
/^fW / / // T*J*- 1,-Z- f d/t/
/JUv/fW //// **
///////iTA or A T/tC.dL
SAMPLERS: (Sigmtunf
STA. NO.
DATE
(J
TIME
COMP.
CD
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K
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STATION LOCATION
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Relinqyfftied by:t%i*<(?u/«J
Date
Time
Received by: ISignttun)
Relinquished by: tSignininl
Date / Time
Received by: ttip—tunl
Relinquished by: (Signttunl
Date / Time
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5**$4- ^ J/5// ^^3/57 2.
Oiitribution: Original Accompaniet Shipment; Copy to Coordinator Field Filet
0602
-------
SAMPLE PACKAGING AND SHIPMENT
C-24
-------
SAMPLE PACKAGING SUMMARY
SAMPLE
\.
1—~7\
'
|VERMICUUTe|
/A
/
1 ^ v /
r ice
1 1
L A J
• ENCLOSE ALL SAMPLE CONTAINERS IN CLEAR
PLASTIC BAGS.
• PACK ALL MEDIUM AND HIGH LEVEL WATER AND
SOIL SAMPLES IN METAL PAINT CANS.
• LABEL PAINT CANS WITH SAMPLE NUMBER OF
SAMPLE CONTAINED INSIDE.
• SURROUND CONTENTS OF CAN WITH NON-
COMBUSTIBLE, ABSORBENT PACKING MATERIAL.
• USING FREEZER PACKAGES OR ICE SEALED IN PLASTIC
BAGS, COOL ORGANIC LOW OR MEDIUM SAMPLES
AND INORGANIC SAMPLES TO BE ANALYZED FOR
CYANIDE TO 4°C.
• ICE IS NOT REQUIRED IN SHIPPING LOW LEVEL SOIL
SAMPLES, BUT MAY BE UTILIZED AT THE
DISCRETION OF THE SAMPLER.
• DO NOT COOL DIOXIN, INORGANIC LOW LEVEL
WATER, INORGANIC MEDIUM/HIGH LEVEL WATER OR
SOIL, OR ORGANIC HIGH LEVEL WATER OR SOIL
SAMPLES.
• PACK SEALED PAINT CANS OR PLASTIC-ENCLOSED
SAMPLE BOTTLES IN SHIPMENT CONTAINER.
• USE A METAL ICE CHEST FOR SHIPMENT (DO NOT
USE CARDBOARD OR STYROFOAM CONTAINERS TO
SHIP SAMPLES).
• SURROUND CONTENTS WITH NON-COMBUSTIBLE.
ABSORBENT PACKING MATERIAL (DO NOT USE
EARTH OR ICE PACKING MATERIALS).
• TAPE PAPERWORK IN PLASTIC BAGS UNDER COOLER
LID.
• CLOSE COOLER AND SEAL WITH CUSTODY SEALS.
C-25
-------
SAMPLE SHIPMENT
COORDINATION CHECKLIST
IMMEDIATELY UPON SHIPMENT OF SAMPLES, SAMPLERS
CALL SMO AT (703/557-2490), WITH THE FOLLOWING
INFORMATION:
• CASE AND/OR SAS NUMBER
• NAME OF LABORATORY
• DATE OF SHIPMENT
• CARRIER, AIRBILL (SHIPMENT)
NUMBERS AND TYPE OF SERVICE
• NUMBER AND MATRICES
(WATERS, SOILS, ETC.) OF
SAMPLES SHIPPED
• INFORMATION ON COMPLETIONS,
CHANGES, DELAYS,
CONTINUATIONS, ETC.,
PERTINENT TO THE CASE
• SAMPLER'S NAME, REGION, AND.
PHONE NUMBER
• SMO MUST BE NOTIFIED BY
3:00 PM ON FRIDAY FOR
SAMPLES INTENDED FOR
SATURDAY DELIVERY/PICKUP
C-26
-------
POTENTIAL PROBLEMS
WITH SAMPLE SHIPMENT AND ANALYSIS
INCORRECT OR INCOMPLETE PAPERWORK
LABORATORY RECEIPT OF INCORRECT SAMPLES
INSUFFICIENT VOLUME FOR ANALYSIS REQUESTED
BROKEN OR LEAKING SAMPLES
MATRICES OTHER THAN WATER OR SOIL
(I.E., ROCKS, LEAVES, STICKS, OIL, ETC.)
NON-HOMOGENEOUS/MULTI-PHASE
WATER OR SOIL SAMPLES
ANALYTICAL PROBLEMS WITH SAMPLES
LABORATORY ACCIDENTS INVOLVING SAMPLES
IF ANY OF THESE PROBLEMS ARE ENCOUNTERED,
CONTACT SMO IMMEDIATELY
C-27
-------
In Reference to Case No(s):
Contract Laboratory Program
REGIONAL/LABORATORY COMMUNICATION SYSTEM
Telephone Record Log
Date of Call:
Laboratory Name:
Lab Contact:
Region:
Regional Contact:
Call Initiated By: Laboratory Region
In reference to data for the following sample number(s):
Summary of Questions/Issues Discussed:
Summary of Resolution:
Signature Date
Distribution: (1) Lab Copy, (2) Region Copy, (3) SMO Copy
C-28
-------
CONTRACT LABORATORY PROGRAM
Deputy Project Officer Communication Summary
Date DPO Notified of Issue: DPO Notified By;
Subject Laboratory: Case/Sas No:
Contact for Resolution:
(Laboratory or PO)
Date of Contact: Call or Visit (Circle One)
Summary of Issues & Resolutions;
Document the issue(s), resolution(s), and action deadlines, if any.
Signature Date
Region
I. Lab DPO Copy 2. SMO Copy 3. Lab Copy 0. Regional DPO Copy 5. Project Officer Copy
8/11/86
C-29
-------
SAMPLE MANAGEMENT OFFICE
Follow-Up Notice of
Request for Corrective Action
SAS No.
Laboratory, Name:
Date of Verbal Notice: / / Corrective Action Start Date: / /
Sample No(s)/Parameters:
Direction Given:
Direct Inquiries to: 703/557-2^90
White: Lab Yellow: SAS File Pink: Region Gold: SMO Invoice Log
7/22/86
C-30
-------
APPENDIX D
AUXILIARY SUPPORT SERVICES DOCUMENTATION
D-l
-------
Date of Request:
FROM (Name):
Affiliation:
Telephone:
AR Signature:
CLP SAMPLE BOTTLE REPOSITORY
SUPERFUND DELIVERY REQUEST
Type of Request:
Routine
Fast Turnaround
Emergency
REQUEST NO.
(date/time request called in)
(date/time request called in)
Ship the following items for arrival by:
(If applicable) Ship to arrive no earlier than:
(date)
(date)
No. of Items
No. of Cases
Item
Description
Per Case
Requested
A
80-ounce amber glass bottle
6
B
-------
SAMPLE BOTTLE REPOSITORY
SUPERFUND PACKING LIST
REPOSITORY DELIVERY REQUEST NO.
Request Date:
Type of Request: R FTA
Required Delivery Date:
DESTINATION (from Delivery Request)
Name:
Address:
Telephone No:
The materials listed below have been
shipped as requested.
Date Shipped:
Mode of Shipment:
Shipment ID No:
Signature:
Type of Shipment: Complete Partial Partial/Completes Request
Item No of. Cases Lot QC Clearance
No. Description Shipped Number(s) Number(s)
A 80-oz glass
B 40-mL glass
C 1-Lpoly
D 120-mL glass :
E 16-oz glass . .
F 8-02 glass
G U-oz glass
H 1-L glass
J 32-oz glass
K U-L glass
AUTHORIZED REQUESTOR USE ONLY
Sign below and forward the yellow copy to SMO within 7 days of shipment receipt. Keep
the pink copy for your file.
The above request was received by the designee, inspected, and accepted.
Date of Receipt: Requestor Signature:
Send yellow PL copy to: USEPA Sample Management Office (SMO)
P.O. Box 818
Alexandria, Virginia 22313
Distribution: Yellow - Requestor Copy for Return to SMO
White - Shipment/Designee Copy Pink - Requestor File Copy
Green - SMO Copy Gold - Repository Copy
D-3
-------
DATE: 02/24/86
U.S ENVIRONMENTAL PROTECTION AGENCY
HAZARDOUS WASTE INVESTIGATION
SAMPLE MANAGEMENT OFFICE
PAGES
**** REGIONAL SAMPLE LIST *»**
SAMPLES RECEIVED FROM REGION I
FROM 08/01/65 TO 08/31/85
LABORATORY: CONTRACT :
PROGRAM : GC SCREEN* GC/M3 ANALYSIS
DAY LATE/EARLY CODES: N/A : NOT APPLICABLE
N/R: NO CHRONICLE RECEIVED N/O: NOT DUE
CASE NO/
TYPE! INV
REGION/
TYPE2 INV
LAB
SAMPLE NO RECEIVED
SAMPLE
HEIGHT
COMP
CODE
SAMPLE
TYPE
DATA
DUE
DATA
RECEIVEO
DAYS
DATA
LATE/EARLY
EXT VOA
IHHHMHHHMHtMHHilMHHMHMMI
4762 X
WWWWn WWWWWWWWWwWwh wwWi*
00002186
AB969
08/01/85
0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002186
AB970
08/01/85
0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002186
AB971
08/01/85
0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002186
AB972
08/01/85
0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002186
AB973
08/01/85
. 0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002186
AB974
08/01/85
0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002186
ABi975
08/01/85
0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002261
AB975-X
08/01/85
0.40
EB
B
OLH
09/14/85
09/14/85
0
0
N/A
00002186
AB976
08/01/85
0.80
IftJ
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002166
AB976-M
08/01/85
0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002186
AB976-D
08/01/85
0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002186
AB977
08/01/85
0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
00002186
AB978
08/01/85
0.80
EB
EP
B
P
OLH
08/31/85
08/31/85
0
-2
N/A
4770 I
00002326
AC584
08/14/85
1.00
FULL
OLS
09/13/85
09/25/85
12
-2
-I
00002326
AC584-M
08/14/85
1.00
FULL
OLS
09/13/85
09/25/85
12
-2
-1
00002326
AC584-D
08/14/85
1.00
FULL
OLS
09/13/85
09/25/85
12
-2
-I
-------
CASE FILE PURGE MATERIALS
INCLUDE, BUT ARE NOT LIMITED TO:
SAMPLE TAGS
CHAIN-OF-CUSTODY RECORDS
COPIES OF SAMPLE TRACKING RECORDS
ANALYSTS' LOGBOOK PAGES
INSTRUMENT LOGBOOK PAGES
(INCLUDING INSTRUMENT CONDITIONS)
BENCH SHEETS
INSTRUMENT READOUT RECORDS
COMPUTER PRINTOUTS
CHROMATOGRAPHIC CHARTS
RAW DATA SUMMARIES
CORRESPONDENCE MEMOS
DOCUMENT INVENTORY
D-5
-------
QA/QC COMPLIANCE REPORT
D-6
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
Contract Laboratory Program
SAMPLE MANAGEMENT OFFICE
MEMORANDUM
DATE:
TO:
, 1986
USEPA Region
FROM:
SMO Data Review Team
SUBJECT: QA/QC Compliance Review Summary for a Contract Laboratory Program
Organic Sample Data Package: Case No.
As requested, quality control and performance measures for the data packages
noted have been examined and compared to EPA standards for compliance. Measures for
the following general areas were evaluated:
Data Completeness
Spectra Matching Quality
Surrogate Spikes
Matrix Spikes/Duplicates
Calibration
Blanks
DFTPP and BFB Tuning
Chromatography
Holding Times
Compound ID (HSL, TIC)
Any statistical measures used to support the following conclusions are attached so
that the review may be reviewed by others.
Summary of Results
Acceptable as Submitted
Acceptable with Comments
Unacceptable, Action Pending
Unacceptable
I
"Volatiles
11
B/N/A
111
Pesticide
Data Reviewed by:
Review Authorized By:
Signature:
Area Code/Phone No.:
FTS Line:
Date:
Date:
P.O. Box 818, Alexandria, Virginia 22313. Phone: (703) 557-2490/FTS-8-557-2490
D-7
-------
NARRATIVE
Case No.
Site Name
Laboratory Name
Introduction
The laboratory's portion of this Case consisted of
samples collected on , 1985.
The laboratory reported problem(s) with the receipt of these
samples.
The laboratory reported problems with the analyses of
compounds.
The evaluator has commented on the criteria specified under each fraction head-
ing. All criteria have been assessed, but no discussion is given where the evaluator has
determined that criteria were adequately performed or require no comment. Details
relevant to these comments are given on the forms in Appendix A. Amounts of detected
compounds are summarized in Appendix B.
D-8
-------
Evaluation by Fraction
I. Volatiles (VOAs)
Holding Times
GC/MS Tuning
Calibration, Initial
Calibration, Continuing
Blank
Surrogate Recovery
Comments:
MS/MSD
Compound ID (HSL, TIC)
Spectra Quality
Standards
Chromatography
Data Completeness
D-9
-------
II. Base/Neutral/Acids
Holding Times
GC/MS Tuning
Calibration, Initial
Calibration, Continuing
Blank
Surrogate Recovery
Comments:
MS/MSD
Compound ID (HSL, TIC)
Standards
Chromatography
Data Completeness
D-10
-------
III. Pesticides/PCBs
Holding Times
Instrument Performance
DDT RT/12 Minute?
Retention Time Window
Analytical Sequence
DDT/Endrin Degradation
RT Check for DBC
Resolution Check
Comments:
Calibration Linearity
Calibration, Continuing
Blank
Surrogate Recovery
MS/MSD
Compound ID (HSL, TIC)
Standards
Chromatography
Data Completeness
D-ll
-------
REVIEW MATRIX
APPENDIX B - VOA COMPOUNDS
Page of
Case No. _______ Laboratory Name
Compoind*
Samples
Blanks
Chloromethane
Bromomethane
Vinyl Chloride
Chloroe thane
Methylene Chloride
Acetone
¦
Carbon Disulfide
1,1-Dichloroethene
1,1 -Dichloroethane
T rans-1,2-DichIoroethene
Chloroform
1,2-Di chloroe thane
2-Butanone
1,1,1 -T richloroethane
Carbon Tetrachloride
Vinyl Acetate
Bromodichloromethane
1,2-Dichloropropane
T rans-1,3-Dichloropropene
T richloroethene
Dibromochloromethane
1,1,2-T richloroethane
Benzene
cis-1,3-Dichloropropene
2-Chloroethylvinylether
Bromoform
-------
REVIEW MATRIX
APPENDIX B - PESTICIDE/PCB COMPOUNDS
Page of
Case No. ____________ Laboratory Name
Com poinds
Samples
Blanks
Alpha-BHC
Beta-BHC
Delta-BHC
Camma-BHC
Heptachlor
Aldrin
Heptachlor Epoxide
Endosulfan I
Dieldrin
M-DDE
Endrin
Endosulfan 11
~,0-DDD
Endosulfan Sulfate
*.
-------
REVIEW MATRIX
APPENDIX B - BNA COMPOUNDS
Page of
Cue No. Laboratory Name
Cam poinds
Samples
Blanks
Phenol
bis(2-Chloroethyl)Ether
2-Chiorophenol
1,3-Dichlorobenzene
1 ,-Dinitrophenol
O-Nitrophenol
Dlbenzoluran
2,4-Dinitrotoluene
2.6-Dinitrotoluene
Diethylphthalate
4-ChlorophenvI-phenylether
Fluorene
f-Nitroaniline
-------
REVIEW MATRIX
APPENDIX B - TIC COMPOUNDS
Laboratory Name
D-15
-------
CONTRACT COMPLIANCE SCREENING
D-16
-------
CONTRACT COMPLIANCE SCREENING FOR 0R6ANIC VOA
PAGE:
OF
CASE:
LAB NAME:
SAMPLES:
DATE:
.LOG NO.
PREPARED BY:
©
I
SAMPLE
NO
C/M
DATE
RECEIVED IANALYSIS
ANALYSIS
TIME
ASSOC-
IATE
TUNE
ASSOC-
IATE
BLANK
CALIBRATION
INITl CONT
HITS
HSLlTIC
NO
OF
SPCS
SURR.
OUT
LIERS
PROBLEMS
-------
CONTRACT COMPLIANCE SCREENING FOR ORGANIC B/N/A PAGE: OF
CASE:
LAB NAME:
SAMPLES:
DATE:
.LOG NO.
PREPARED BY:
©
I
00
SAMPLE
NO
C/M
DATE
RECD. I EXT. I ANAL.
ANALY-
SIS
TIME
ASSOC-
IATE
TUNE
ASSOC-
IATE
BLANK
CALIBRATION
INIT ICCNT
HITS
HSLlTIC
NO
OF
SPCS
SURR
OUT
L1ERS
PROBLEMS
-------
CONTRACT COMPLIANCE SCREENING FOR ORGANIC PESTICIDES/ PCBS PA6E: OF
CASE:
LAB NAME:
SAMPLES:
DATE:
PREPARED BTt
LOS NO.
I
SAMPLE
NO.
C/M
DATE
RECO.
EXT.
COLUMN 1
ANALYSIS
DATE
TIME
ASSO-
CIATE
BLANK
CALIBRATION
INIT
CONT
COLUMN 2_
ANALYSIS
DATE
TIME
ASSO-
CIATE
BLANK
CALIBRATION
INIT
CONT
NO.
OF
HITS
PROBLEMS
-------
CASE:
LAB NAME:
CONTRACT COMPLIANCE SCREENING SUMMARY FOR 0R6ANICS PAGE _
SAMPLES: DATE: LOS NO._
REGION:
OF
V 0 A
B N A
PREPARED BY:
PESTICIDES
S
A
M
P
L
E
B
I CALIB I
C I D E I F
H
HlTlBlllClSlMlC
0 I U I L I N I 0 I U I S I 0
LlNlKlIlNlRl/lM
DlElSlTlTlRlDlP
B
I CALIB I
C I D E I F
HlHlTlBlIIClSlMlC
OlOlUlLlNlOlUlSlO
LlLlNlKlIlNlRl/lM
DlDlElSlTlTlRlDlP
B
I CALIB I
H I I J | K
HlHlBlDlRlAlOlDlMlIIClC
OlOlLlDlTlNlElBlSiNlOlO
LlLlKlTl |A|G|C|/|I|N|M
DlDlSl IMILI I IDITITIP
0
1
N)
O
~
~
~
PROBLEM CODE: EX = EXPLAIN, RS = RESUBMIT, SU = SUBMIT» NC = NONCOMPLIANT
-------
CONTRACT COMPLIANCE SCR
CASE:
LAB NAME:
EENZN6 FOR INORGANICS
SAMPLES:
REGION:
WORKSHEET A - ICAP PAGE OF
OATE:
PREPARED BY:
SAMPLE
NO.
7
SJ
C/M
DATE
RECD. ANAL.
CALIBRATION
INIT. CONT.
BUNKS
ICS
LINEAR
RANGE
LCS
SERIAL
DILUTION
PROBLEMS
-------
CONTRACT COMPLIANCE SCREENING FOR INORGANICS WORKSHEET B: AA AND CYANIDE PAGE
CASE: SAMPLES: DATE:
LAB NAME: REGION: PREPAREO BT:
ANALTTES
OF
SAMPLE
C/M
DATE
PROBLEMS
O
fo
M
! I I I I
-------
CONTRACT COMPLIANCE SCREENING SUMMARY FOR IN0R6ANICS PAGE OF
CASE: SAMPLES: DATE:
LAB NAME: REGION: PREPARED BY:
SAMPLE
NO.
A
COVER
PAGE
B
OATA
SHEETS
CALIBRATION
INIT. CONT.
D
BLANKS
E
ICS
F
MATRIX
SPIKE
DUP.
ID L
LCS
I
MSA
J
HOLD
TIME
K
RAH
DATA
L
n?
M
SER.
OIL.
N
LIN.
RAN6E
0
1
N)
W
PROBLEM CODE: EX = EXPLAIN, RS = RESUBMIT, SU = SUBMIT, NC = NONCOMPLIANT
-------
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
-------
ANALYTICAL REFERENCES
American Public Health Association, American Water Works Association, Water Pollution
Control Federation, Standard Methods for Examination of Water and Wastewater,
14th Ed., (1975).
American Society for Testing and Materials, Annual Book of ASTM Standards, Part 31,
"Water", Standard D3223-73, p. 343 (1976^
Bishop, 3.N., 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,
USEP A-600/4-79-019.
EPA, Handbook for Monitoring Industrial Wastewater, USEPA Technology Transfer, 1973.
EPA, Methods for Chemical Analysis of Water and Wastewater, USEPA Technology
Transfer, 1974.
EPA, Methods for Chemical Analysis of Water and Wastes, EPA Pub. 600/4-79-02, March
1979.
EPA Office of Solid Waste and Emergency Response, Modification (By Committee) of
Method 3050, SW-846, 2nd Ed., Test Methods for Evaluating Solid Waste, July 1982.
EPA, Procedures Manual for Groundwater Monitoring at Solid Waste Disposal Facilities,
EPA 530/SW-611, 1977.
EPA EMSL, Users Guide for the Continuous Flow Analyzer Automation System,
Cincinnati, Ohio, 1981.
Garbarino, J.R. and Taylor, H.E., "An Inductively-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 40, 2085 (1968).
E-2
-------
ANALYTICAL REFERENCES
(continued)
Kopp, J.F., Longbottom, M.C. and Lobring, L.B., "Cold Vapor Method for Determining
Mercury," AWWA, Vol. 64, p. 20, Jan. 1972.
Martin, T.D., Kopp, J. F., and Ediger, R.D., "Determining Selenium in Water, Wastewater,
Sediment and Sludge by Flameless Atomic Absorption Spectroscopy", Atomic
Absorption Newsletter 14, 109, 1975.
Organochlorine Pesticides and PCBs, Method 608; 2,3,7,8-TCDD, Method 613; Purgeables
(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 (CNI) as a Stabilizing Agent for 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 IIC System,
Technical Pub. #TA9-0460-00, Tarrytown, 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 Inorganic Data/Protocol Review Committee.
Winefordner, J.D., "Trace Analysis: Spectroscopic Methods for Elements," Chemical
Analysis, Vol. 46, pp. 41-42.
Winge, R.K., Peterson, V.J., 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 Organics in Sludges, USEPA, Municipal
Environmental Research Laboratory; Cincinnati, Ohio 45268.
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).
E-3
-------
SAMPLING REFERENCES
EPA Environmental Response Team, Field Monitoring and Analysis of Hazardous
Materials, EPA Training Manual, Course No. 165.f, Cincinnati, Ohio, 1980.
Huibregtse, K.R., and Moser, J.H., Handbook for Sampling and Sample Preservation of
Water and Wastewater, USEPA-600/4-76-049, 1976.
Municipal Environmental Research Laboratory, USEPA, Samplers and Sampling Procedu-
res for Hazardous Waste Streams, EPA-600/280-018, Cincinnati, Ohio, 1980.
National Enforcement Investigations. Center, Enforcement Considerations for Evaluation
of Uncontrolled Hazardous Waste Sites by Contractors, EPA Office of Enforcement,
Denver, Colorado, 1980.
Olson, D.M., Berg, E.L., Christensen, R., Otto, H., Ciancia, 3., 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.I., Biological Field and Laboratory Methods for Measuring the Quality of Surface
Waters and Effluents, USEPA-670/W3-001, 1973.
SHIPPING REFERENCES
Federal Express Corporation, Hazardous Materials Department, Telephone: 1-800-238-
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, 49
CFR Parts 100 - 199, October 1, 1978.
E-4 «U. S.GOIKRMENT PRINT INC OFflCE :19B7-716-002 i606«9
------- |