United States Office of Emergencyand EPA 540-R-99-004 Environmental Protection Remedial Response OSWER 9240.0-34P Agency (5201G) PB99-963218 February, 2000 www.epa.gov/superfund Introduction to the Contract Laboratory Program ------- Introduction This document is designed to educate primarily EPA's Superfund staff and managers (e.g., Remedial Project Managers, On Scene Coordinators, Site Assessment Managers, and Risk Assessors) in obtaining laboratory analytical services for Superfund and Brownfields sites. The Contract Laboratory Program (CLP) is administered by OERR's Analytical Operations/Data Quality Center (AOC), Regional CLP Project Officers, and Regional Sample Control Center Coordinators. Other programs or agencies can "buy" into the CLP - please refer to the section on "CLP Participants" in Chapter 1 and the AOC contact list in Appendix C. CLP analytical data is used to demonstrate the nature and extent of contamination at hazardous waste sites, assess priorities for response based on risks to human health and the environment, establish appropriate cleanup actions, and determine when remedial actions are complete. Each CLP sample is properly documented to ensure timely, accurate, and complete analysis for all parameters requested, and to support the use of sample data in potential enforcement actions against responsible parties. Therefore the CLP is not available to the private sector (e.g., Potentially Responsible Parties) since it is a federally funded program and use by private parties would cause a conflict of interest. The Introduction to the Contract Laboratory Program can be obtained in Adobe Acrobat format from the CLP Web site, at the following address: http://www.epa.gov/superfund/proqrams/clp/index.htm ------- Table of Contents Chapter 1 Welcome to the Contract Laboratory Program 1 Overview of the Contract Laboratory Program 1 Background 1 Benefits of the CLP 1 Analytical Services 1 Quality Assurance 1 Enhanced Automated Services 2 Support Services 2 Cost Savings 2 Flexibility 2 CLP Successes 3 Brownfields Initiatives 3 Federal Creosote Initiatives 3 Data Assessment Tool 3 Products and Services 4 Analytical Data 4 Analytical Services 5 Expert Technical and Administrative Support 5 CLP Participants 5 Program Users 5 Program Providers 5 The CLP on the Internet 6 Chapter 2 How to Access the Contract Laboratory Program 7 CLP Services and Activities 7 Initiating CLP Analytical Services 7 Requesting CLP Analytical Services 7 Non-Superfund Support 8 Determining the Proper Statement of Work 8 CLP Software Tools 9 Data Assessment Tool 9 Contract Compliance Screening 10 Computer Aided Data Review and Evaluation 10 Data Assessment Rapid Transmittal 10 Field Operations Records Management System II Lite 10 Enforcement and Cost Recovery Support 11 Requesting Enforcement Support 11 Requesting Cost Recovery Support 11 Appendix A CLP Analytical Program Fact Sheets A-1 Appendix B CLP Documents B-1 Appendix C CLP Contacts C-1 Appendix D List of Acronyms from Chapters 1 and 2 D-1 Appendix E Glossary E-1 ------- ------- Chapter 1 - Welcome to the Contract Laboratory Program Chapter 1 Welcome to the Contract Laboratory Program The CLP is **° Superfund's preferred data quality solution for Routine Analytical Services The CLP is available ^ to local, state, and federal agencies. (A description of the CLP Program Providers may be found on page 5) The CLP provides *3° total quality assurance Overview of the Contract Laboratory Program Background Data of Known and Documented Quality: Analytical data that adheres to EPA Order 5360.1, which calls for data to withstand independent review and confirmation. Download EPA Order 5360.1 at http://es.epa.gov/ncerqa/qa/qad-docs/5360-1 ct .pdf Welcome to the Contract Laboratory Program (CLP). The CLP is a national network of Environmental Protection Agency (EPA) personnel, commercial laboratories, and support contractors whose fundamental mission is providing customers with analytical data of known and documented quality. Initiated in 1980, the CLP supports environmental data users in identifying contaminants and determining the level of contamination at Superfund hazardous waste sites prior to, during, and after site cleanup. (Note: Potentially Responsible Parties (PRPs) cannot access the CLP). Benefits of the CLP Customer satisfaction is the key factor in the design and application of all CLP services. The CLP supplies its customers with timely, high-quality, high-volume, low cost services and solutions. Customers using the CLP receive the following benefits: Analytical Services • The CLP provides a variety of analytical services for the most commonly requested organic and inorganic analytes. For a full listing of CLP target compounds and analytes, please see the Fact Sheets for the Inorganic, Organic, and Organic Low Concentration programs in Appendix A. You may also obtain the Fact Sheets from the CLP Web site at: www.epa.gov/superfund/proqrams/clp/facts.htm • The CLP provides environmental sample analysis, electronic and manual data review, and compliance with EPA specifications, giving customers a full spectrum of analytical services from a review of sample results to a full assessment of analytical raw data. Quality Assurance • The CLP provides a comprehensive quality assurance (QA) program through on-site audits, Performance Evaluation (PE) samples, quarterly performance reports, fraud detection mechanisms, performance-based scheduling, and continuous inspection of laboratory data for contractual compliance. • To simplify the Quality Assurance Project Plan (QAPP) development process, the CLP predefines elements such as: analytical methods; preventive laboratory equipment maintenance and calibration; sample shipment Chain-of-Custody procedures and forms; analytical precision and accuracy (including quantitation limits for organics and detection limits for inorganics); laboratory quality control (QC) requirements; data management; and documentation for laboratory analysis. ------- Chapter 1 - Welcome to the Contract Laboratory Program Automated «s° services streamline sample scheduling and analytical data assessment CLP's support «s° structure allows the customer to focus on site assessment activities EPA Headquarters <& assumes the costs for Regional clients CLP services are ^ becoming more flexible and responsive • CLP data is compliant with EPA Order 5360.1 quality requirements which require data to withstand independent review and confirmation. Enhanced Automated Services • The CLP captures all data produced for CLP customers. The historical data is kept for the client's future use in enforcement, litigation, and cost recovery activities. • The CLP offers Automated Data Processing (ADP) support such as automated data assessment and rapid electronic transfer of analytical data into users' databases. • The CLP provides automated sample scheduling and in certain instances can accommodate same day scheduling. Support Services • The CLP provides support services that allow managers to focus on site assessment activities without distraction from laboratory and data management issues. • CLP systems collect and disseminate financial information to EPA management for budgetary and litigation activities. (See Chapter 2, Enforcement and Cost Recovery Support, page 11). • The CLP staff has the technical expertise to resolve any questions about sample scheduling and funding and to assist EPA Regions in evaluating data quality and usability. Cost Savings • EPA Headquarters assumes the CLP costs for Regional clients in Superfund lead projects. • The CLP offers centralized high-volume purchasing of analytical services, eliminating the duplication of effort for procurement, sample tracking, invoice processing, and analytical results compilation. • The CLP offers competitive, low market prices for all projects and analytical services. The CLP's per sample prices may be viewed online at: www.epa.gov/superfund/programs/clp/prices.htm Flexibility • Customers can request a variety of data turnaround options and detection limits. • Customers can request new and/or additional methods for analysis to meet changing requirements and technological advances (currently available for organic analyses). ------- Chapter 1 - Welcome to the Contract Laboratory Program CLP Successes "Brownftelds" are abandoned, idle, or under-used industrial and commercial facilities where expansion or redevelopment is complicated by real orperceived environmental contamination. The CLP can •& accommodate a large volume of samples from multiple sites within a short time span The CLP provides "^ high-tech solutions to meet the customer's needs For more information1^ on CCS and CADRE, see the section on DAT in Chapter 2 on page 9 The following activities and products demonstrate the CLP's success in providing its customers with analytical and technical support services to achieve data of known and documented quality. Brownfields Initiatives EPA's Brownfields Initiative is an effort to identify contamination and conduct cleanup activities at various "Brownfield" sites across the United States. The objective is to make these sites safe for use in a short period of time. In FY1999, the CLP laboratories completed 84 separate projects involving the analysis of more than 4,200 field samples for 64 Brownfields sites. The CLP has provided, and continues to provide, Brownfields customers with certain advantages, such as the CLP's comprehensive QC procedures, data turnaround options, and low market prices with high quality that may not be available through other analytical programs. To learn more about the Brownfields Initiative, visit the Web site at: http://www.epa.gov/swerosps/bf/ Federal Creosote Initiatives In February 1998, EPA Region II requested assistance with the Federal Creosote site in New Jersey. Because 140 residences stand upon the site, Region II needed to quickly assess environmental damage and potential risks to human health. The CLP processed more than 2,900 soil samples during a 4 week sampling period, with 80-100 samples shipped daily to the participating laboratories. The Region required a fast turnaround of 14 days for analytical data. Analytical Operations/Data Quality Center (AOC), CLP laboratories, and CLP contractors worked in unison to provide Region II with the highest quality analytical and support services possible, successfully meeting the Region's time frame. As of January 2000, the CLP has analyzed more than 4,896 samples for the Federal Creosote site. Data Assessment Tool During the Federal Creosote site project, AOC recognized the need for an analytical tool that would facilitate the rapid transfer and storage of electronic analytical data and would streamline the data validation process. To meet this challenge, the CLP developed the Data Assessment Tool (DAT), a software- driven process designed to produce enhanced CLP deliverables and more usable reports. DAT allows Regional data users to electronically receive data that has already been assessed by Contract Compliance Screening (CCS) and Computer Aided Data Review and Evaluation (CADRE) data reviews. DAT rapidly transfers electronic analytical data into any client database, foregoing the need for manual data entry by the Regions. (Regional data validation has typically required manual data entry of post-review data). Overall, DAT has dramatically improved data turnaround times, making it possible to transmit electronic data to the data validators and the ultimate customers (e.g., Regional Project Managers (RPMs), site assessors, on-scene coordinators). DAT performed so well that AOC made it available to all Regions following the Federal Creosote site project. AOC can now provide data assessment reports to CLP customers within 24 to 48 hours of receipt of data. ------- Chapter 1 - Welcome to the Contract Laboratory Program The CLP successfully supports its customers in its routine activities as well. Please see the following figure for data on Routine CLP Activities during Fiscal Year 1999. SMO Active Laboratories: ~ 27 Samples Scheduled: 57,755 Shipment* Tracked: 2,812 Samples Shipped: 49,600 527 Sites Required Sample Analysis Customer Service Inquiries Answered: 2,734 Oata Packages Invoices Received/Reviewed: 3,645 Processed: 3,127 Technical Issues Received/Resolved: 916 Analyses Performed; 122,92ft Cost Recovery Requests: 320 (Reporting a value of $45,199,776*} * See *ie Glossary for a definition of Cost Recovery Routine CLP Activities in FY1999 CLP data is used " in all phases of the Superfund pipeline Products and Services Analytical Data The CLP provides analytical data that is used to help define the nature and extent of contamination at Superfund sites. This allows customers to: • Assess priorities for response based on the risk to human health and the environment; • Determine appropriate cleanup; and • Determine when remedial actions are complete. CLP data is used in all stages of hazardous waste site investigation, including site inspections, Hazard Ranking System (HRS) scoring, remedial investigation and feasibility studies, remedial design, treatability, remedial and removal actions, operations and maintenance, and enforcement and litigation activities. The CLP requires that any data produced within the program be of known and documented quality. ------- Chapter 1 - Welcome to the Contract Laboratory Program CLP customers *s" can combine analytical parameters and turnaround times to satisfy changing needs Complete Organic ^f Data Deliveries are available in 7, 14, and 21 days with preliminary results available in 48 and 72 hours Complete Inorganic *&" Data Deliveries are now available in 7, 14, or 21 days with preliminary results available within 72 hours The CLP is available ^ to Federal, state, territorial, and tribal agencies who need fast, reliable, environmental data (see Chapter 2, How to Access the CLP) EPA provides "^ oversight of all Program Management and Quality Assurance Activities Analytical Services Currently, the CLP offers three Routine Analytical Services (RAS): analysis of organic compounds in soils and water; analysis of metals in soils and water, and analysis of low concentration organic compounds in drinking water and groundwater. These types of analytical services ensure that the CLP is able to meet the changing needs of its clients. See Fact Sheets and other information in Appendix A for additional details. Current Services Available: * Analysis of Organic Compounds in Soils and Water (OLM04.2) * Analysis of Metals in Soils and Water (ILM04.1) » Analysis of Low Concentration Organic Compounds in Drinking Water and Groundwater (OLC02.1) Expert Technical and Administrative Support CLP's staff is comprised of experts in the fields of environmental chemistry, contract management, and automated data processing. The CLP has numerous resources within EPA Regions, EPA's own laboratories, and CLP contractors. These resources give the CLP the capability to address and overcome technical or operational issues for the CLP customer. CLP Participants Program Users CLP customers currently include 10 EPA Regions, state and tribal governments, the Army Corps of Engineers, the U.S. Bureau of Reclamation, the U.S. Geological Survey, and U.S. territories. The CLP is available to any party (except PRPs) who needs fast, reliable, environmental data of known and documented quality at reasonable prices. Program Providers The CLP is operated by a team of government offices, support contractors, and environmental laboratories. The following offices comprise the CLP: • AOC provides government oversight of all CLP activities to ensure that clients receive data of known and documented quality. • EPA Regional CLP Project Officers (CLP POs) and Regional Sample Control Center (RSCC) coordinators provide program support and oversight activities on a day-to-day basis. • The Sample Management Office (SMO), operated by the Contract Laboratory Analytical Services Support (CLASS) contractor, provides program management (e.g., scheduling, contract compliance tools, and invoice tracking) under the direction of AOC. • The Quality Assurance Technical Support (QATS) contractor provides CLP data QA (e.g., Performance Evaluation samples, data tape audits) under the direction of AOC. • CLP-contracted laboratories conduct sample analysis and provide data of known and documented quality. ------- Chapter 1 - Welcome to the Contract Laboratory Program The CLP on the Internet Find additional *&* information and new features on the Internet Current and future CLP customers can access additional information and resources at the CLP Web site on the Internet at: www.epa.gov/superfund/proqrams/clp/index.htm The pages on this Web site include more information about the CLP and its processes and procedures. Web visitors may also obtain copies of Statements of Work (SOW) and Fact Sheets for the organic, inorganic, and organic low concentration analytical protocols on the Products and Services pages. Visitors may also download the CLP's National Functional Guidelines (i.e., data assessment guidelines) and detailed points-of-contact for the CLP. Please visit the CLP Web site today for more information. ------- Chapter 2 - Accessing the Contract Laboratory Program Chapter 2 How to Access the Contract Laboratory Program The CLP can support Superfund and non-Superfund programs The Initial Process Select the CLP for your analytical needs. Contact Is your site a EPAAOC's Superfund -No* CLASS site? I Project Yj,s Officer., I Contact your Regional RSCC. Supply your RSCC with the necessary information. iCC will The RSCC will begin the Scheduling Process. The RSCC will work with the CLP Contractors and coordinate with you on the resulting activities. CLP Services and Activities This chapter provides guidance for initiating and using Contract Laboratory Program (CLP) services. It also provides information on several CLP-related software products available to CLP customers. You can begin using CLP services by contacting AOC. Please see Appendix C for contact information. Initiating CLP Analytical Services The first step in accessing CLP services is determining if the CLP is the right program for your purposes. The CLP offers numerous advantages to its customers (see Benefits of the CLP in Chapter 1) that may not be available in other programs. Also, you must determine if the site you wish to sample from is a Superfund site. If the site is part of the Superfund, then follow the steps below. If it is not a Superfund site, proceed to Non- Superfund Support on page 8. Requesting CLP Analytical Services Once you have decided to use the CLP, the next step is requesting analytical services. (Note: Each Region may have different steps for initiating analytical services. The following is only a general description.) Current and new CLP customers may request routine analytical services through an EPA Regional Sample Control Center (RSCC). The RSCC schedules all CLP analysis requests through the Sample Management Office (SMO). SMO and the RSCC work together during sampling events to ensure all samples arrive at the laboratories as scheduled and to resolve any issues that may arise during sample analysis. Each RSCC is responsible for maintaining a working knowledge of current CLP Statements of Work (SOWs) to assist the customer in choosing the proper analytical method. (Note: The CLP requires "lead time" in order to secure laboratory space for sampling projects. Routine Analytical Service projects must be scheduled with the CLP by noon on the Wednesday prior to the week of sample shipment). You will need to supply the RSCC with the following types of information (Note: There may be additional information required for your particular Region): • Site name; • Site location; • Operable unit of the site where you want the sampling to take place. (The operable unit is a specific portion of a whole site); • Type(s) of analysis you require; • Purpose of your sampling event (e.g., Site Assessment (SA), Remedial Design (RD), Remedial Action (RA), etc.); • Period of time during which the sampling will take place; • Site identification numbers (e.g., CERCLIS ID, Site Spill ID); • Data turnaround time required for your project; • Fax number for preliminary results, if required; and • Site specific Quality Assurance Project Plan (QAPP). The CLP is available to EPA Regions, state, territorial, and tribal governments, government agencies, and other EPA offices interested in receiving analytical services at reasonable costs with full QA and quality controls (QC). (Contact AOC for more information. See Appendix C.) ------- Chapter 2 - Accessing the Contract Laboratory Program Non-Superfund ** Support Services The Inorganic '^ Analytical Service The Organic ^ Analytical Service Non-Superfund Support Hie CLP also provides analytical and support activities to non- Superfund analyses customers through the transfer of funds from a non-Superfund program (e.g., RCRA, Office of Water). If you wish to utilize CLP services for non-Superfund activities, please contact the CLASS Project Officer at AOC, AOC will facilitate the funds transfer process and direct the sample analysis request to the appropriate EPA Regional Office. To contact AOC for this service, see the CLP Contacts in Appendix C or visit the CLP Web site. Determining the Proper Statement of Work The next step in accessing analytical services through the CLP is deciding which analytical services best meet your needs. The CLP currently offers three SOWs for CLP inorganic, organic, and organic low concentration analytical services. Each of the SOWs provides the technical and contractual conditions for laboratories to apply EPA/CLP analytical methods for the isolation, detection, and quantitative measurement for the most common environmental pollutants. Contact the specified AOC Program Manager for further information. Refer to the CLP Contacts in Appendix C for the appropriate contact information. NOTE: The SOWs listed below are not designed to handle radioactive samples, such as those that might come from Department of Energy sites, or samples with very high concentrations of contamination or product type samples. AOC does have some SOWs {e.g., SOW IHC01.3) that may be used to procure laboratory services for high concentration samples. However, these contracts are currently not active. Potentially radioactive samples will need to be handled on a case-by-case basis. The Inorganic SOW (ILM04.1) The Inorganic SOW sets the requirements for the analysis of 23 metal inorganic target analytes and cyanide in water and soil/sediment samples. Inorganic analysis is conducted using inductively coupled plasma (ICP), atomic absorption (AA), and colorimetric methods. Data is delivered in either 7, 14, or 21 days. The customer may specify any of the three turnaround times when requesting CLP inorganic analytical services. Preliminary results are available within 72 hours for all turnaround times. For a complete list of the inorganic target analytes and more information about the inorganic analytical service, see the Multi-Media, Multi-Concentration, Inorganic Analytical Service for Superfund (ILM04.1) Fact Sheet in Appendix A. The Organic SOW (OLM04.2) The Organic SOW sets the requirements for the analysis of 48 volatile, 65 semivolatile, and 28 pesticide/Aroclor (PCB) target compounds in water and soil/sediment samples. Organic compounds are analyzed using gas chromatography coupled with mass spectrometry (GC/MS) or an electron capture detector (GC/ECD). Data delivery is available in 7,14, or 21 days, any of which may be specified when requesting CLP organic analytical services. Preliminary results are available within 48 hours for volatiles and 72 hours for semivolatiles and pesticides/Aroclors (PCBs) underthe 7-day turnaround option. 8 ------- Chapter 2 - Accessing the Contract Laboratory Program The Low *** Concentration Organic Analytical Service DAT integrates CLP data review software and processes For a complete list of the organic volatile, semivolatile, and pesticide/Aroclor (PCB) target compounds and more information about the organic analytical service, seethe Multi-Media, Multi-Concentration, Organic Analytical Service for Superfund (OLM04.2) Fact Sheet in Appendix A. The Organic Low Concentration SOW (OLC02.1) The Organic Low Concentration SOW sets the requirements for the analysis of 41 volatile, 59 semivolatile, and 28 pesticide/Aroclor (PCB) target organic compounds in low concentration groundwaterand drinking water samples. The lowest concentration limit for volatile analysis is 1 part per billion (ppb), 5 ppb for semivolatile analysis, and 0.01 ppb for pesticide/Aroclor (PCB) analysis. Data delivery is available in 14 days. For a complete list of the low concentration target compounds and more specific information about the low concentration analytical service, please see the Low Concentration Organic Analytical Service for Superfund (Water Matrix) (OLC02.1) Fact Sheet in Appendix A. See Appendix B for a listing of CLP documents, including the SOWs, Fact Sheets, and National Functional Guidelines. Appendix B also provides information on where to obtain these documents. CLP Software Tools The CLP's commitment to quality does not end with data. In an effort to bring faster and more efficient services to our customers, the CLP has developed a number of software solutions that streamline data review and QC, contract compliance, and administrative tasks, while promoting the sharing of analytical information. Data Assessment Tool The Data Assessment Tool (DAT) is a software-driven process designed to produce enhanced CLP deliverables and more usable reports in a standard format. DAT incorporates Contract Compliance Screening (CCS), Computer Assisted Data Review and Evaluation (CADRE), and Data Assessment Rapid Transmittal (DART) to provide EPA customers with PC-compatible reports and electronic files that can be transferred into client databases and programs for end users, and to provide a complete CLP data assessment package. The electronic reports reduce the need for manual data entry and duplicate entry of information. All CLP customers receive data that has been processed through CLP data assessment tools within 24 to 48 hours after that laboratory data is received. The resultant spreadsheets are delivered directly to the data requesters (e.g., RSCCs) email addresses, in a format (e.g., Lotus) specified by the Regional customer. DAT does not include determination of data usability, qualification of data based on professional judgment, evaluation of data based on its intended use, or compliance with a site's Quality Assurance Project Plan (QAPP) or Sampling and Analysis Plan (SAP). ------- Chapter 2 - Accessing the Contract Laboratory Program DAT Components CCS and CADRE «" provide electronic data review services DART provides fast electronic data transmission FORMS II Lite *»• automates routine tasks for the sampler and streamlines data collection Contract Compliance Screening The Contract Compliance Screening (CCS) system is a data verification tool used to determine if a- laboratory's data submission is complete and contractually compliant with CLP SOW terms and conditions included in its contract. Following the evaluation, CCS produces a report detailing the evaluation results. Computer Aided Data Review and Evaluation The Computer Aided Data Review and Evaluation (CADRE) system evaluates QC results against data review criteria appropriate for the corresponding analytical method/procedure. The CADRE system has predefined CLP method information and data reyiew/QC criteria. However, it can be customized to support variations on the analytical techniques employed by the CLP and to review data according to project-specific QC criteria. CADRE uses both Regional and National Functional Guidelines as the QC criteria (e.g., holding times, percent moisture) to review and evaluate electronic analytical data. Data Assessment Rapid Transmittal Data Assessment Rapid Transmittal (DART) is an active notification system providing up-to-the-minute transmittal of the CCS and CADRE evaluation report data to CLP customers. DART also provides customers with a comprehensive audit trail and transaction record by logging reader and recipient IDs, as well as access times and dates after an email has been opened. DART is a "user-friendly" system that operates on both DOS and Microsoft Windows platforms. DART provides customers with a variety of other reports, such as Lotus/Microsoft Excel spreadsheets or an electronic file in Agency Standard Format via the Internet. Field Operations Records Management System II Lite The Field Operations Records Management System II (FORMS II Lite) is designed for customer use during the sampling event. FORMS II Lite automates the printing of labels, custody seals, Traffic Reports, and Chain-of-Custody records to improve field time management. FORMS II Lite captures critical collection information in an electronic format early in the field sampling process. FORMS II Lite enables field personnel to easily document, track, and transmit field sample information to the laboratories. In addition, by electronically capturing this information early in the tracking and reporting process, field sampling data is readily accessible for transmittal to laboratories, RSCCs, and other data users. As of February 2000 all 10 Regions, 13 states and tribal governments, and one Federal agency have received the FORMS II Lite 4.0 production version of the software. To learn more about these software tools, please visit the CLP Web site at: www.epa.gov/superfund/proqrams/clp/systems.htm 10 ------- Chapter 2 - Accessing the Contract Laboratory Program Enforcement and Cost Recovery Support The CLP provides litigation support The CLP assists «3° customers in recouping analytical and site cleanup costs The CLP has established detailed procedures and documentation to ensure that the sample data is tracked from the time of sample collection to introduction as evidence in legal proceedings. The CLP also provides documentation for program analytical costs to support Superfund cost recovery efforts. Cost recovery is designed to assist CLP customers in recouping the CLP analytical and cleanup costs they have spent on a hazardous waste site. Requesting Enforcement Support Litigation procedures often necessitate the use of CLP data generated from the analysis of samples collected. The CLP offers a variety of services to support enforcement activities, which include: • Arranging for the delivery of all laboratory and evidence documentation relating to specific sample analyses; • Augmenting customer resources for analytical data review; and • Assisting in arranging for expert testimony by laboratory or CLP personnel. Client requests for enforcement support are initially coordinated through the Cost Recovery Contact at AOC (refer to the CLP Contacts in Appendix C). AOC will review the request and determine the appropriate CLP response, including the provision of EPA Regional or contractor resources needed to respond to the request. Requesting Cost Recovery Support The CLP's cost recovery support normally consists of financial and analytical documentation. The following forms of documentation are available to support cost recovery requests: Reports which detail all CLP analytical and management costs associated with a site; Lists of CLP projects associated with a site; Sample analysis results; and Lists of each invoice associated with a particular site. Non-standard ad-hoc reports also may be prepared if necessary. Individuals interested in requesting cost recovery support should refer to the CLP Contacts in Appendix C. If necessary, the cost recovery personnel will coordinate efforts with the other EPA offices or contractor resources in order to produce or acquire cost recovery documentation. 11 ------- Appendix A CLP Analytical Program Fact Sheets Current Analytical Services SOW Concentration Matrices Fractions Turnaround Options Inorganic Multi-Media, Multi-Concentration (ILM04.1) Low, Medium Water, Soil/Sediment • 23 Metals (total or dissolved) • Cyanide • 7 Days • 1 4 Days •21 Days Preliminary Results Available (for all turnaround options): • 72 Hours Organic Multi-Media, Multi-Concentration (OLM04.2) Low, Medium Water, Soil/Sediment • 48 Volatiles • 65 Semivolatiles • 28 Pesticides/Aroclors (PCBs) • 7 Days • 1 4 Days •21 Days Preliminary Results Available (for 7-Day Turnaround only): • 48 Hours (Volatiles) • 72 Hours (Semivolatiles and Pesticide/Aroclors (PCBs)) Low Concentration (OLC02.1) Low Water • 41 Volatiles • 59 Semivolatiles • 28 Pesticides/Aroclors (PCBs) • 1 4 Days A-l ------- A-2 ------- S-EPA United States Environmental Protection Agency Office of Solid Waste and Emergency Response Publication 9240.0-09-FSD February 2000 Multi-Media, Multi-Concentration, Inorganic Analytical Service for Superfund (ILM04.1) * Office of Emergency and Remedial Response Analytical Operations/Data Quality Center (5204G) Quick Reference Fact Sheet Under the legislative authority granted to the U.S. Environmental Protection Agency (EPA) under the Comprehensive Environmental Response, Compensation, and Liability Act of -1980 (CERCLA) and the Superfund Amendments and Reauthorization Act of 1986 (SARA), EPA develops standardized analytical methods for the measurement of various pollutants in environmental samples from known or suspected hazardous waste sites. Among the pollutants that are of concern to EPA at such sites are a series of inorganic analytes and cyanide that are analyzed using inductively coupled plasma (ICP), atomic absorption (AA), and colorimetric techniques. The Analytical Operations/Data Quality Center (AOC) of the Office of Emergency and Remedial Response (OERR) offers an analytical service that provides data from the analysis of water and soil/sediment samples for inorganic analytes for use in the Superfund decision-making process. Through a series of standardized procedures and a strict chain-of-custody, the inorganic analytical service produces data of known and documented quality. This service is available through the Superfund Contract Laboratory Program (CLP). DESCRIPTION OF SERVICES The inorganic analytical service provides a technical and contractual framework for laboratories to utilize EPA/CLP analytical methods. These methods are used in the preparation, detection, and quantitative measurement of cyanide and 23 inorganic target analytes in both water and soil/sediment environmental samples. The CLP provides the methods to be used and the specific technical, reporting, and contractual requirements, including quality assurance, quality control, and standard operating procedures, by which EPA evaluates the data. This service uses ICP, AA, and colorimetric methods to analyze the inorganic target analytes and cyanide. Three data delivery turnarounds are available to CLP customers: 7,14, and 21-day turnaround after receipt of the last sample in the set. In addition, a 72- hour preliminary data submission option also is available for all turnaround times. DATA USES This analytical service provides data that EPA uses for a variety of purposes. Examples include determining the nature and extent of contamination at a hazardous waste site, assessing priorities for response based on risks to human health and the environment, determining appropriate cleanup actions, and determining when remedial actions are complete. The data may be used in all stages in the investigation of a hazardous waste site including site inspections, Hazard Ranking System scoring, remedial investigations/feasibility studies, remedial design, treatability studies, and removal actions. In addition, this service provides data that are available for use in Superfund enforcement/litigation activities. TARGET ANALYTES The analytes and detection limits for which this service is applicable are listed in Table 1. The list of target analytes for this service was originally derived from the EPA Priority Pollutant List of 129 compounds. In the years since the inception of the CLP, analytes have been added to and deleted from the Target Analyte List, based on advances in analytical methods, evaluation of method performance data, and the needs of the Superfund program. Specific detection limits are highly matrix dependent. * ILM04.1 is an interim inorganic analytical service. Further changes are expected to be released under ILM05.0 for competition during calendar year 2000. A-3 ------- Table 1. Target Analvte List and Contract Required Detection Limits (CRDLs) (ILM04.1) Abbreviation Al Sb As Ba Be Cd Ca Cr Co Cu Fe Pb Mg Mn Hg Ni K Se Ag Na Tl V Zn Cn Analyte Aluminum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Mercury Nickel Potassium Selenium Silver Sodium Thallium Vanadium Zinc Cyanide CRDL1 (n/L) 200 60 10 200 5 5 5000 10 50 25 100 3 5000 15 0.2 40 5000 5 10 5000 10 50 20 10 Sample concentration exceeding five times the detection limit of the instrument or method in use may be reported even though the instrument or method detection limit is greater than the CRDL. This is illustrated in the following example: For lead: Method in use = ICP Instrument Detection Limit (IDL) = 40 Sample Concentration = 220 CRDL =3 'The CRDL is the instrument detection limit obtained in pure water. METHODS AND INSTRUMENTATION When storing samples, the use of a cooler temperature indicator bottle and the cooler temperature must be reported on Form DC-1 and in the Sample Delivery Group (SDG) Narrative. When applying AA methods, the Contractor may analyze the sample at a dilution so long as the raw concentration or absorbence of the diluted sample falls within the upper half of the calibration range. For ICP, an undiluted analysis of the sample is required. If an insufficient sample amount (less than 90% of the required amount) is received to perform the analyses, the Contractor must contact the Sample Management Office (SMO) to report the problem. The same is required for multi-phase samples (e.g., two-phase liquid sample and oily sludge/sandy soil sample). Table 2 summarizes the methods and instruments used in this analytical service. DATA DELIVERABLES Data deliverables for this service include both hardcopy/ electronic data reporting forms and supporting raw data. The laboratory must submit data to EPA within 7,14,21- days, or preliminary data must be submitted within 72 hours after laboratory receipt of each sample in the set. EPA then processes the data through an automated Data Assessment Tool (DAT). DAT is a complete CLP data assessment package. DAT incorporates Contract Com- pliance Screening (CCS) and Computer-Aided Data Review and Evaluation (CADRE) to provide EPA Regions with PC-compatible reports, spreadsheets, and electronic files. These files can be provided to the Regions within 24 to 48 hours from the receipt of the data and can be used as a tool during the data validation process at the Region. This automated tool facili tales the transfer of analytical data into Regional databases. In addition to the Regional electronic reports, the CLP laboratories are provided with a data assessment report that documents the instances of noncompliance. The laboratory has 4 days to reconcile defective data and resubmit the data to EPA. EPA then reviews the data for noncompliance and sends a final data assessment report to the CLP laboratory and the Region. QUALITY ASSURANCE The quality assurance (QA) process consists of management review and oversight at the planning, implementation, and completion stages of the environmental data collection activity. This process ensures that the data provided are of the quality required. A-4 ------- Table 2. Methods and Instruments Analyte Al, Sb, As, Ba, Be, Cd, Ca, Cr, Co, Cu, Fe, Pb, Mg, Mn, Ni, K, Se, Ag, Na, Tl, V, Zn As, Pb, Tl, Se Ca, Mg, Na, K Hg CN Instrument Inductively Coupled Plasma (TCP) Graphite Furnace Atomic Absorption (GFAA) Flame Atomic Absorption (FAA) Cold Vapor Atomic Absorption (CVAA) Manual and Semi-automated Colorimetric Method Acid digestion followed by ICP analysis Acid digestion followed by GFAA analysis Acid digestion followed by FAA analysis Acid and permanganate oxidation followed by CVAA analysis Distillation followed by colorimetric analysis Table3. Quality Control QC Operation Instrument Calibration Initial Calibration Verification Initial Calibration Blank Continuing Calibration Verification Continuing Calibration Blank Interference Check Sample CRDL Standard for ICP CRDL Standard for AA Serial Dilution for ICP Preparation Blank Laboratory Control Sample Matrix Spike Sample Analysis Duplicate Sample Analysis Post Digestion Spike Analytical Spike Method of Standard Addition Instrument Detection Limit Determination Interelement Corrections Linear Range Analysis Freo^ency Daily or each time instrument is set up Following each instrument calibration Following each instrument calibration Every 10 analytical samples or every 2 hours during a run and at the beginning and end of each run Every 10 analytical samples or every 2 hours during a run and at the beginning and end of each run Every 20 analytical samples and at the beginning and end of each run Every 20 analytical samples and at the beginning and end of each run At the beginning of each AA analytical run For each matrix type and concentration level for each SDG For each sample preparation, analysis, and matrix per batch of prepared samples For each sample preparation and analysis procedure for each batch For each matrix type, concentration level, and method for each SDG For each matrix type, concentration level, and method for each SDG Each time matrix spike recovery is outside QC limits For each analytical sample analyzed by furnace AA When the analytical spike recovery is outside QC limits Quarterly Annually for ICP instruments only Quarterly for ICP instruments only A-5 ------- During the data collection effort, QA activities ensure that the quality control (QC) system is functioning effectively and that the deficiencies uncovered by the QC system are corrected. After environmental data are collected, QA activities focus on assessing the quality of data to determine its suitability to support enforcement or remedial decisions. Each contract laboratory prepares a quality assurance plan (QAP) with the objective of providing sound analytical chemical measurements. The QAP must specify the policies, organization, objectives, functional guidelines, and QA/ QC activities designed to achieve the data quality requirements for this analytical service. QUALITY CONTROL The QC process includes those activities required during analytical data collection to produce data of known and documented quality. The analytical data acquired from QC procedures are used to estimate and evaluate the analytical results and to determine the necessity for, or the effect of, corrective action procedures. The QC procedures required for this analytical service are shown in Table 3. PERFORMANCE MONITORING ACTWITIES Laboratory performance monitoring activities are provided primarily by AOC and the Regions to ensure that contract laboratories are producing data of the appropriate quality. EPA performs on-site laboratory audits, data package audits, and evaluates laboratory performance through the use of blind performance evaluation samples. For more information, or for suggestions to improve this analytical service, please contact: Tanya Mitchell Inorganic Program Manager EPA/AOC Ariel Rios Building (5204G) 1200 Pennsylvania Avenue, N.W. Washington, DC 20460 703-603-8872 FAX: 703-603-9112 A-6 ------- United States Environmental Protection Agency Office of Solid Waste and Emergency Response Publication 9240.0-33FS January 2000 Summary of Major Changes Made to the Multi-Media, Multi-Concentration, Organic Analytical Statement of Work (OLM03.2 to OLM04.2) Office of Emergency and Remedial Response Analytical Operations/Data Quality Center (5204G) Quick Reference Fact Sheet Under the legislative authority granted to the U.S. Environmental Protection Agency (EPA) under the Comprehensive Environmental Response, Compensation, and Liability Act of 1980 (CERCLA) and the Superfund Amendments and Reauthorization Act of 1986 (SARA), EPA develops standardized analytical methods for the measurement of various pollutants in environmental samples from known or suspected hazardous waste sites. Among the pollutants that are of concern to the EPA at such sites, are a series of volatile, semi volatile, and pesticide/Aroclor (pesticide/PCB) compounds that are analyzed using gas chromatography coupled with mass spectrometry (GC/MS) and gas chromatography with an electron capture detector (GC/ECD). The Analytical Operations/Data Quality Center (AOC) of the Office of Emergency and Remedial Response (OERR) offers an analytical service that provides data from the analysis of water and soil/sediment samples for organic compounds for use in the Superfund decision-making process. Through a series of standardized procedures and a strict chain-of-custody, the organic analytical service produces data of known and documented quality. This service is available through the Superfund Contract Laboratory Program (CLP). OVERVIEW OF MAJOR CHANGES The new organic analytical service provides a technical and contractual framework for laboratories to apply EPA/CLP analytical methods for the isolation, detection, and quantitative measurement of target compounds in water and soil/sediment environmental samples. The following service items were added or modified to better serve our customers. i. All references to 14-day and 35-day data turnaround times were removed. With OLM04.2, laboratories now have 7-, 14-, or 21- day turnaround times for analyses after laboratory receipt of the last sample in the sample delivery group (SDG). Under the 7-day turnaround option, preliminary data can be obtained within 48 hours (for volatile analyses) or 72 hours (for semivolatile and pesticide/Aroclor [pesticide/ PCB] analyses). ii. The definition of an SDG was modified to include samples received over a 7-dav period (was 14 days) regardless of contract turnaround time, and the maximum of 20 samples in an SDG now excludes Performance Evaluation (PE) samples. In addition, laboratories are now required to prepare and analyze PE samples concurrently with samples in the SDG, and all samples and sample fractions assigned to an SDG must be scheduled under the same contractual turnaround time. iii. The number of volatile and semivolatile compounds has been modified to include 10 new volatile compounds and five new semivolatile compounds. In addition, four semivolatile compounds were moved to the volatile target compound list. The compounds that have been added or moved are detailed in the Modifications To Target Compounds section and shaded in Table 1. iv. Modified the delivery schedule for Sample Traffic Reports from "5 working days" to "3 working days" to accommodate the new data turnaround requirements. v. Includes the optional use of Modified SW-846 Method 5035 using a closed system purge-and- trap method for low-level volatile soil analysis and of methanol preserved field samples for medium level volatile soil analysis. A-7 ------- VI. VII. Users may now request modifications to the specified methodologies that may include, but are not limited to, additional compounds and modified quantitation limits. SW-846 methods 3541 and 3545 (Automated Soxhlet Extraction and Pressurized Fluid Extraction) were added for optional use if laboratories demonstrate equivalence and the laboratory is approved by the EPA. These alternative extraction techniques provide the laboratories with the option to use extraction procedures that require less solvent. MODIFICATIONS TO TARGET COMPOUNDS Since the CLP began in 1980, compounds have been added and removed from the Target Compound List (TCL) based on advances in analytical methods, evaluation of method performance data, and to meet the needs of Superfund program participants. Compounds that have been added or moved in the SOW are shaded in Table 1. The following modifications were made to the organic analytical service target compounds. i. New volatile compounds include: dichlorodifluoromethane, trichlorofluoro- methane, 1,1,2-trichloro-1,2,2-trifluoroethane, methyl acetate, trans-1,2-dichloroethene, methyl tert-buytl ether, cis-1,2-dichloroethene, cyclo- hexane, methylcyclohexane, 1,2-dibromoethane, isopropylbenzene, and 1,2 dibromo-3-chloro- propane. ii. Compounds moved from semivolatiles to volatiles are: 1,2-dichlorobenzene, 1,3-di- chlorobenzene, 1,4-dichlorobenzene, and 1,2,4- trichlorobenzene. iii. New semivolatile compounds include: benz- aldehyde, acetophenone, caprolactam, 1,1'-bi- phenyl, and atrazine. MODIFICATIONS TO METHODS AND INSTRUMENTATION Current methods and instrumentations have been modified in an effort to allow CLP participants to use newer technologies or address previous issues. The following items summarize the modifications to the organic analytical service. i. The absence of a temperature indicator bottle is addressed by using an alternative procedure to determine the cooler temperature. ii. The analysis of matrix spikes and matrix spike duplicates is now optional and will be required on a case-by-case basis at the request of the customer. iii. "Gel Permeation Chromatography (GPC) Calibration" now includes "GPC Calibration and Continuing Calibration Verification (CCV)". In addition, the GPC cleanup procedures are based on manufacturer's specifications. iv. In addition to SOW specified screening procedures, laboratories may now use other EPA approved screening procedures, as well as their own in-house screening procedures, for determining if low or medium level analytical methods should be used. v. Modified methods may be performed after a written request has been approved by the Regional CLP Project Officer (PO) and laboratory Contracting Officer (CO). For example, additional compounds may be requested or quantitation limits may be adjusted. Volatiles The following items were added for volatiles. i. Specific procedures are included for the collection and weighing of low and medium level soil samples for analysis by Modified SW-846 Method 5035. ii. Procedures were incorporated to address the preparation and analysis of samples using Modified SW-846 Method 5035. iii. Guidance is provided for the analysis of storage blanks when an SDG contains only soil samples. iv. The composition of the "trap" portion of the purge-and-trap device was modified to incorporate 7 cm of coconut charcoal. This modification was made to accommodate new target compounds. Semivolatiles and Pesticides/Aroclors (Pesticides/PCBs) i. The frequency of method blanks was clarified to require that a method blank be extracted each time samples are extracted; the number of samples extracted with each method blank shall not exceed 20 samples; the method blank shall be extracted by the same procedure used to extract samples; and the method blank shall be analyzed on each GC/MS system used to analyze associated samples. A-8 ------- ii. The following items were added for the optional use of SW-846 methods 3541 and 3545 (Automated Soxhlet Extraction and Pressurized Fluid Extraction). • Language was added for the determination of method equivalency for alternative extraction procedures. • Specific instructions were provided allowing laboratories to utilize alternative extraction methods, if pre- approved by EPA. MODIFICATIONS TO REPORTING REQUIREMENTS AND DATA DELIVERABLES Data deliverables for this service include hardcopy data reporting forms and supporting raw data. In addition to the hardcopy deliverable, contract laboratories must submit the same data on diskette (or via an alternate means of electronic transmission if approved in advance by EPA). Below are modifications that affect data deliverables. i. The two most recent UV traces of the GPC semivolatile calibration solution are now required for submission. ii. Requirements were modified for reporting tentatively identified compounds (TICs) for which a library match of 85% or greater is obtained. The name of the compound with the best match must be reported as the TIC, whether or not there was a positive identification. 111. IV. v. Instructions were incorporated regarding data to be supplied in instances where no airbill is received. Additional instructions are provided for the requirements and items included on tape audits (magnetic tapes). Tape audit requirements now apply to GC/ECD data in addition to the previously required GC/MS data. Modified the assignment of an SDG number to include instructions for assigning SDG numbers for fractions of the same field samples scheduled under different turnaround times. VI. Modified the electronic reporting information to be Y2K compliant. of date For more information, or for suggestions to improve this analytical service, please contact: Terry Smith Organic Program Manager USEPA/AOC Ariel Rios Building (5204G) 1200 Pennsylvania Avenue, NW Washington, DC 20460 703-603-8849 FAX: 703-603-9112 A-9 ------- Table 1. Target Compound List and Contract Required Ouantitation Limits (CRQLs) For OLM04.2* Quantitation Limits Low Water Soil (ug/L) (ug/Kg) VOLATILES 1. Dichloroditluoromethane . . 10 10 2. Chloromethane 10 10 3, Vinyl Chloride 10 10 4. Bromomethane 10 .... 10 5. Chloroethane 10 10 6. Trichlorofluoromethanc . . 10 10 7. 1,1-Dichloroethene 10 10 8. l,U-TricMoro- 1,2,2-trifluoroethane 10 10 9. Acetone 10 ... 10 10. Carbon Bisulfide 10 ... 10 11. Methyl Acetate 10 ... 10 12 Methylene Chloride .10 10 13. trans-l,2-Dichloroethene** . . 10 10 14. Methyl tert-Butyl Ether . . 10 10 15 1 1-Dichloroethane 10 10 16. cis-l,2-Dichloroethene** ... 10 .... 10 17. 2-Butanone 10 10 18. Chloroform 10 10 19. 1,1,1-Trichloroethane 10 10 20. Cydohexane 10 10 21. Carbon Tetrachloride 10 .... 10 22. Benzene 10 . . 10 23. 1,2-Dichloroethane 10 10 24 Trichloroethene 10 10 25. Methylcyclohexane 10 10 26. 1,2-Dichloropropane 10 10 27. Bromodichloromethane .... 10 .... 10 28. cis-l,3-Dichloropropene ... 10 10 29. 4-Methyl-2-pemanone 10 10 30. Toluene 10 . . 10 31. trans- 1,3-Dichloropropene ..10 10 32. 1,1,2-Trichloroethane 10 .... 10 33 Tetrachloroethene 10 10 34 2-Hexanone 10 ... 10 35. Dibromochloromethane .... 10 .... 10 36. 1,2-Dibromoethane 10 10 37 Chlorobenzene 10 10 38. Ethylbenzene 10 ... 10 39. Xylenes (Total) 10 ... 10 40. Styrene .... 10 . . 10 41 Bromoform 10 10 42. Isopropylbenzene 10 10 43. 1,1,2,2-Tetrachloroethane ... 10 10 44. 13-Dichlorobenzene 10 .... 10 45. l,4-Dich\orobenzene 10 10 46. U-Dichlorobenzene 10 10 47. U-Dibromo- 3-chtoropropane 10 .... 10 48. 1,2,4-Triclorobenzene 10 10 Quantitation Limits Low Water Soil (ug/L) (US/Kg) SEMIVOLATILES 49. Benzaldehyde 10 ... 330 50 Phenol 10 330 51. bis-(2-Chloroethyl) ether 10 ... 330 52 2-Chlorophenol . . 10 . . 330 53 2-Methylphenol 10 330 54. 2,2'-oxybis (1-Chloropropane) 10 ... 330 55. Acetophenone 10 ... 330 56. 4-Methylphenol 10 ... 330 57. N-Nitroso-di-n-propylamine . . 10 ... 330 58 Hexachloroethane . 10 330 59 Nitrobenzene 10 330 60 Isophorone 10 330 61 2-Nitrophenol 10 330 62 2,4-Dimethylphenol .10 330 63. bis-(2-Chloroethoxy) methane .10 ... 330 64 2 4-Dichlorophenol 10 330 65. Naphthalene 10 ... 330 66. 4-Chloroaniline 10 ... 330 67. Hexachlorobutadiene 10 ... 330 68 Caprolactam 10 ... 330 69. 4-Chloro-3-methylphenol 10 ... 330 70 2-Methylnaphthalene ... 10 . 330 71. Hexachlorocyclopentadiene . . 10 ... 330 72 2 4 6-Trichlorophenol 10 330 73. 2,4,5-Trichlorophenol 25 ... 830 74. I,l'-Biphenyl 10 ... 330 75. 2-Chloronaphthalene 10 ... 330 76 2-Nitroaniline 25 830 77 Dimethylphthalate 10 330 78 2 6-Dinitrotoluene .10 . 330 79 Acenaphthylene 10 330 80 3-Nitroaniline 25 830 81 Acenaphthene 10 330 82 2 4-Dinitrophenol ... 25 . . 830 83 4-Nitrophenol 25 830 84 Dibenzofuran . 10 330 85 2 4-Dinitrotoluene 10 330 86 Diethylphthalate . 10 . . 330 87 Fluorene 10 ... 330 88. 4-Chlorophenyl-phenyl ether . . 10 ... 330 89 4-Nitroaniline 25 830 90. 4,6-Dinitn>2-methylphenol . . 25 ... 830 91. N-Nitrosodiphenylamine 10 ... 330 92. 4-Bromophenyl-phenyl ether .10 ... 330 93 Hexachlorobenzene 10 330 94 Atrazine 10 . 330 95 Pentachlorophenol 25 830 96 Phenanthrene . . 10 . 330 97 Anthracene . 10 . 330 Quantitation Limits Low Water Soil (ug/L) (HR/Kg) 98 Carbazole 10 330 99 Di-n-butylphthalate 10 330 100 Fluoranthene 10 330 101 Pyrene 10 . 330 102 Butylbenzylphthalate 10 330 103. 3,3'-Dichlorobenzidine .... 10 ... 330 104 Benzo(a)anthracene 10 330 105. Chrysene 10 . . 330 106. bis-(2-Ethylhexyl) phthalate 10 ... 330 107 Di-n-octylphthalate 10 330 108 Benzo(b)fluoranthene 10 330 109 Benzo(k)iluoranthene 10 330 110 Benzo(a)pvrene 10 330 111. Indeno(l,2,3-cd)pyrene ... 10 ... 330 112. Dibenzo(a,h)anthracene ... 10 ... 330 113. Benzo(g,h,i)perylene 10 ... 330 PESirdDES/AROCLORS (PESXICIDES/PCBs) Water Soil (ug/L) (ug/Kg) 1 14. alpha-BHC 0.05 .... 1.7 115 beta-BHC 005 17 116 delta-BHC 005 .. 1.7 117. gamma-BHC (Lindane) . . 0.05 .... 1.7 118 Heptachlor 005 17 119 Aldrin 005 17 120. Heptachlor epoxide 0.05 1.7 121 EndosulfanI . . .005 .. 1.7 122 Dieldrin 010 33 123 44'-DDE 010 .. 3.3 124 Endrin ... ... 0 10 ... 3.3 125 Endosulfan n 010 33 126 44'-DDD 010 .. 33 127. Endosulfan sulfate 0.10 3.3 128. 4,4'-DDT 0.10 3.3 129 Methoxychlor .050 ... 17 130. Endrin ketone 0.10 3.3 131 Endrin aldehyde . . 0 10 . .3.3 132. alpha-Chlordane 0.05 1.7 133. gamma-Chlordane 0.05 1.7 134 Toxaphene 5.0 ... 170 135 Aroclor-1016 .10 . .33 136 Aroclor-1221 2.0 .... 67 137 Aroclor-1232 1.0 33 138 Aroclor-1242 1 0 33 139 Aroclor-1248 10 33 140 Aroclor-1254 1 0 33 141 Aroclor-1260 10 . 33 * For volatiles, quantitation limits for medium soils are approximately 120 times the quantitation limits for low soils. For semi volatile medium soils, quantitation limits are approximately 30 times the quantitation limits for low soils. ** 1,2-Dichloroethene (total) has been changed to cis-l,2-Dichloroethene and trans- 1,2-Dichloroethene. Compounds that have been added or moved in the SOW are shaded. A-10 ------- SEPA United States Environmental Protection Agency Office of Solid Waste and Emergency Response Publication 9240.0-08-FSD January 2000 Multi-Media, Multi-Concentration, Organic Analytical Service for Superfund (OLM04.2) Office of Emergency and Remedial Response Analytical Operations/Data Quality Center (5204G) Quick Reference Fact Sheet Under the legislative authority granted to the U.S. Environmental Protection Agency (EPA) under the Comprehensive Environmental Response, Compensation, and Liability Act of 1980 (CERCLA) and the Superfund Amendments and Reauthorization Act of 1986 (SARA), EPA develops standardized analytical methods for the measurement of various pollutants in environmental samples from known or suspected hazardous waste sites. Among the pollutants that are of concern to the EPA at such sites, are a series of volatile, semivolatile, and pesticide/Aroclor (pesticide/PCB) compounds that are analyzed using gas chromatography coupled with mass spectrometry (GC/MS) and gas chromatography with an electron capture detector (GC/ECD). The Analytical Operations/Data Quality Center (AOC) of the Office of Emergency and Remedial Response (OERR) offers an analytical service that provides data from the analysis of water and soil/sediment samples for organic compounds for use in the Superfund decision-making process. Through a series of standardized procedures and a strict chain-of-custody, the organic analytical service produces data of known and documented quality. This service is available through the Superfund Contract Laboratory Program (CLP). DESCRIPTION OF SERVICES The new organic analytical service is available as of September 1999. It provides a technical and contractual frame work for laboratories to apply EPA/CLP analytical methods for the isolation, detection, and quantitative measurement of 48 volatile, 65 semivolatile, and 28 pesticide/Aroclor (pesticide/PCB) target compounds in water and soil/sediment environmental samples. The CLP provides the methods to be used and the specific technical, reporting, and contractual requirements, including quality assurance (QA), quality control (QC), and standard operating procedures (SOPs), by whichEPA evaluates the data. This service uses GC/MS and GC/ECD methods to analyze the target compounds. Three data delivery turnarounds are available to CLP customers: 7,14,and21- day turnaround after laboratory receipt of the last sample in the set. In addition, there are 48 (for volatiles) and 72-hour [for semivolatiles and pesticides/Aroclors (pesticides/PCBs)] preliminary data submission options available. New options under this service include a closed system purge-and-trap method for low level volatile soil analysis and methanol preservation for medium level volatile soil analysis. In addition, users may request modifications to the specified methodologies that may include, but are not limited to, additional compounds and modified quantitation limits. DATA USES This analytical service provides data which EPA uses for a variety of purposes, such as determining the nature and extent of contamination at a hazardous waste site, assessing priorities for response based on risks to human health and the environment, determining appropriate cleanup actions, and determining when remedial actions are complete. The data may be used in all stages in the investigation of a hazardous waste site including site inspections, Hazard Ranking System scoring, remedial investigations/feasibility studies, remedial design, treatability studies, and removal actions. In addition, this service provides data that will be available for use in Superfund enforcement/litigation activities. TARGET COMPOUNDS The compounds for which this service is applicable and the corresponding quantitation limits are listed in Table 1. For water samples, the lowest quantitation limits reportable are 10 ppb for the volatile compounds, 10 ppb for the semivolatile compounds, and 0.05 ppb for the pesticide/Aroclor (pesticide/PCB) compounds. For soil samples, the lowest quantitation limits reportable are 10 ppb for the volatile compounds, 330 ppb for the semivolatile compounds, and 1.7 ppb for the pesticide/ A-ll ------- Table 1. Target Compound List and Contract Required Quantitation Limits (CRQLs) For OLM04.2* Quantitation Limits Low Water Soil (MS/L) (us/Kg) VOLATILES 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. Dichlorodifluoromethane Chloromethane Vinyl Chloride Bromomethane Chloroethane . Trichlorofluoromethane . 1,1-DichJoroethene 1,1,2-Trichloro- 1,2,2-trifluoroethane .... Acetone Carbon Disulfide Methyl Acetate Methylene Chloride . trans- 1 ,2-Dichloroethene Methyl tert-Butyl Ether . . 1 1 -Dichloroethane cis-l,2-Dichloroethene . . 2-Butanone Chloroform 1,1,1-Trichloroethane . . Cyclohexane . . Carbon Tetrachloride . . . Benzene 1 ,2-Dichloroethane . . . Trichloroethene Methylcyclohexane 1 ,2-Dichloropropane . . . Bromodichloromethane . cis- 1 ,3-Dichloropropene 4-Methyl-2-pentanone Toluene trans- 1 ,3-Dichloropropene 1,1,2-Trichloroethane . . . 2-Hexanone Dibromochloromethane . 1 2-Dibromoethane Chlorobenzene Ethylbenzene . . . Xylenes (Total) Styrene 1 , 1 ,2,2-Tetrachloroethane 1,3-Dichlorobenzene . . . 1,4-Dichlorobenzene . . . 1,2-Dichlorobenzene . . . 1,2-Dibromo- 3-chloropropane 1,2,4-Triclorobenzene . . . ...10 . . . 10 10 10 . . 10 . . . 10 ...10 ...10 10 . . . 10 10 . . 10 . . . 10 .. 10 10 . . . 10 . . . 10 10 ...10 . . . 10 ...10 10 . 10 . . . 10 10 ...10 . . . 10 . . . 10 . 10 10 . . 10 ...10 10 10 ...10 10 10 . 10 10 10 10 10 ...10 . .. 10 ...10 ...10 10 ...10 .... 10 10 10 10 10 .... 10 .... 10 .... 10 .... 10 .... 10 10 10 .... 10 .... 10 10 .... 10 .... 10 10 .... 10 ... 10 .... 10 10 .... 10 .... 10 10 .... 10 .... 10 .... 10 .... 10 10 .... 10 .... 10 10 ... 10 .... 10 . 10 10 10 10 . 10 10 10 .... 10 .... 10 .... 10 .... 10 10 .... 10 Quantitation Limits Low Water Soil (ug/L) (ug/Kg) SEMIVOLATILES 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77. 78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 88. 89. 90. 91. 92. 93. 94. 95. 96. 97. Benzaldehyde . . Phenol bis-(2-Chloroethyl)ether 2-Chlorophenol 2-MethyIphenoI 2,2'-oxybis ( 1 -Chloropropane) Acetophenone 4-Methylphenol N-Nitroso-di-n-propylamine . Hexachloroethane Nitrobenzene Isophorone 2-Nitrophenol 2,4-Dimethylphenol bis-(2-Chloroethoxy) methane 2,4-Dichlorophenol Naphthalene 4-Chloroaniline Hexachlorobutadiene Caprolactam 4-ChJoro-3-methylphenol . . . 2-Methylnaphthalene Hexachlorocyclopentadiene . 2,4,6-Trichlorophenol 2 4 5-Trichlorophenol 1 l'-Biphenyl 2-Chloronaphthalene 2-Nitroaniline Dimethylphthalate 2 6-Dinitrotoluene Acenaphthylene . . 3-Nitroaniline 2 4-Dinitrophenol Dibenzofuran 2 4-Dinitrotoluene Diethylphthalate 4-Chlorophenyl-phenylether . 4,6-Dinitro-2-methylphenol . N-Nitrosodiphenylamine . . . 4-Bromophenyl-phenylether . Atrazine Pentachlorophenol Phenanthrene . Anthracene 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 25 10 10 25 10 10 10 25 10 25 25 10 10 10 10 10 25 25 10 10 10 10 25 10 10 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 830 ... 330 ... 330 ... 830 ... 330 ... 330 . . 330 ... 830 ... 330 ... 830 ... 830 ... 330 ... 330 ... 330 ... 330 ... 330 ... 830 ... 830 ... 330 ... 330 ... 330 ... 330 ... 830 ... 330 ... 330 Quantitation Limits Low Water Soil (ug/L) (ug/Kg) 98. 99. 100. 101. 102. 103. 104. 105. 106. 107. 108. 109. 110. 111. 112. 113. PEST Carbazole Di-n-butylphthalate Fluoranthene Butylbenzylphthalate . 3,3'-Dichlorobenzidine Benzo(a)anthracene . . Chrysene . . . . . . 10 10 10 10 . . . . 10 . . . . 10 ... . 10 10 bis-(2-Ethylhexyl)phthalate . 10 Di-n-octylphthalate 10 Benzo(k)fluoranthene Indeno( 1 ,2,3-cd)pyrene Dibenz(a,h)anthracene Benzo(g h i)perylene nCIDES/AROCLORS (PESTICIDES/PCBst 114. 115. 116. 117. 118. 119. 120. 121. 122. 123. 124. 125. 126. 127. 128. 129. 130. 131. 132. 133. 134. 135. 136. 137. 138. 139. 140. 141. alpha-BHC beta-BHC delta-BHC 10 10 . . . . 10 .... 10 10 Water (ug/L) 005 005 . . 0.05 gamma-BHC (Lindane) . . 0.05 Heptachlor . . . . 0 OS Aldrin . . Heptachlor epoxide . . Endosulfan 1 Dieldrin 4 4'-DDE Endrin Endosulfan n 4,4'-DDD Endosulfan sulfate . . . 4 4'-DDT Methoxychlor . . Endrin ketone Endrin aldehyde alpha-Chlordane gamma-Chlordane . . . Toxaphene Aroclor-1016 ArocIor-1221 Aroclor-1232 Aroclor-1242 Aroclor-1248 Aroclor-1254 Aroclor-1260 * For volatiles, quantitation limits for medium soils are approximately 120 times the quantitation limits for low soils. For semivolatile medium soils, approximately 30 times the quantitation limits for low soils. . . . 0.05 . . . 0.05 0.05 . . 0.10 0 10 . . . 0.10 0 10 0.10 . . . 0.10 0 10 0.50 0 10 . . . 0.10 005 . . . 0.05 5.0 ... 1.0 20 10 ... 1.0 1 0 1.0 ... 1.0 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 ... 330 Soil (ug/Kg) 1 7 1.7 1.7 .... 1.7 . . 1.7 1.7 .... 1.7 . . 1.7 .... 3.3 3.3 .... 3.3 33 .... 3.3 .... 3.3 33 17 33 .... 3.3 17 .... 1.7 . 170 .... 33 . 67 33 33 33 . . 33 .... 33 quantitation limits are A-12 ------- Aroclor (pesticide/PCB) compounds. Specific sample quantitation limits will be highly matrix dependent. Compounds identified with concentrations below the quantitation limit will be reported as estimated concentration values. The list of target compounds for this service was originally derived from the EPA Priority Pollutant List of 129 compounds. In the years since inception of the CLP, compounds have been added to and removed from the Target Compound List (TCL), based on advances in analytical methods, evaluation of method performance data, and the needs of the Superfund program. For drinking water and groundwater type samples, use of the low concentration organic analytical service is recommended. METHODS AND INSTRUMENTATION For semivolatile and pesticide/Aroclor (pesticide/PCB) water samples, a 1-L aliquot is extracted with methylene chloride using a continuous liquid-liquid extractor or separatory funnel [for pesticides/Aroclors (pesticides/PCBs) only]. For low level semivolatile soil and pesticide/Aroclor (pesticides/PCBs) soil samples, a 30-g soil/sediment sample is extracted with methylene chloride/acetone using sonication, automated soxhlet, or pressurized fluid extraction techniques. For medium level semivolatile soil samples, a 1 -g aliquot is extracted with methylene chloride using the techniques mentioned above for low level soil samples. For both water and soil samples, the extract is concentrated, subjected to fraction-specific cleanup procedures, and analyzed by GC/MS for semivolatiles or GC/ECD for pesticides/Aroclors (pesticides/PCBs). For volatile water samples, 5 mL of water is added to a purge and trap device and purged with an inert gas at room temperature. For volatile low level soil samples, a 5-g aliquot of soil is added to a purge and trap device with 5 mL of reagent water then purged with an inert gas at 40°C; or a 5-g aliquot (pre-weighed in the field) is purged from a closed-system purge and trap device at 40°C. For volatile medium level soil samples, a measured amount is collected/extracted with methanol and an aliquot of the methanol extract is added to reagent water and purged at room temperature. For both water and soil samples, the volatiles purged from the sample are trapped on a solid sorbent. They are subsequently desorbed by rapidly heating the sorbent and then introduced into a GC/MS system. Table 2 summarizes the methods and instruments used in this analytical service. DATA DELIVERABLES Data deliverables for this service include hardcopy data reporting forms and supporting raw data. In addition to the hardcopy deliverable, contract laboratories must also submit the same data electronically. The laboratory must submit data to EPA within 7, 14, or 21-days [or preliminary data within 48 hours (for volatiles)] or 72 hours [for semivolatiles and pesticides/Aroclors (pesticides/PCBs)] after laboratory receipt of the last sample in the set. EPA then processes the data through an automated Data Assessment Tool (DAT). DAT is a complete CLP data assessment package. DAT incorporates Contract Compliance Screening (CCS) and Computer-Aided Data Review and Evaluation (CADRE) review to provide EPA Regions with PC-compatible reports, spreadsheets, and electronic files within 24 to 48 hours from the receipt of the data for data validation. This automated tool facilitates the transfer of analytical data into Regional databases. In addition to the Regional electronic reports, the CLP laboratories are provided with a data assessment report that documents the instances of noncompliance. The laboratory has 10 days to reconcile defective data and resubmit the data to EPA. EPA then reviews the data for noncompliance and sends a final data assessment report to the CLP laboratory and the Region. QUALITY ASSURANCE The quality assurance (QA) process consists of management review and oversight at the planning, implementation, and completion stages of the environmental data collection activity. This process ensures that the data provided are of the quality required. During the implementation of the data collection effort, Q A activities ensure that the quality control (QC) system is functioning effectively and that the deficiencies uncovered by the QC system are corrected. After environmental data are collected, QA activities focus on assessing the quality of data to determine its suitability to support enforcement or remedial decisions. Each contract laboratory prepares a quality assurance plan (QAP) with the objective of providing sound analytical chemical measurements. The QAP must specify the policies, organization, objectives, and functional guidelines, as well as the QA and QC activities designed to achieve the data quality requirements for this analytical service. QUALITY CONTROL The QC process includes those activities required during analytical data collection to produce data of known and documented quality. The analytical data acquired from QC procedures are used to estimate and evaluate the analytical results and to determine the necessity for, or the effect of, corrective action procedures. The QC procedures required for this analytical service are shown in Table 3. A-13 ------- Table 2. Methods and Instruments Fraction Volatiles Semivolatiles Pesticides/Aroclors (Pesticides/PCBs) Water Purge-and-trap followed by GC/MS analysis Continuous liquid-liquid extraction followed by GC/MS analysis Continuous liquid-liquid or separatory funnel extraction followed by dual column GC/ECD analysis Soil Purge-and-trap or closed-system purge- and-trap followed by GC/MS analysis Sonication, automated soxhlet, or pressurized fluid extraction followed by GC/MS analysis Sonication, automated soxhlet or pressurized fluid extraction followed by dual column GC/ECD analysis Table 3. Quality Control QC Operation System Monitoring Compounds (volatiles) Surrogates [for semivolatiles and pesticides/Aroclors (pesticides/PCBs)] Method Blanks (volatiles) Method Blanks [semivolatiles and pesticides/Aroclors (pesticides/PCBs)] Instrument Blank (volatiles) Instrument Blank [pesticides/Aroclors (pesticides/PCBs)] Storage Blanks (volatiles) GC/MS mass calibration and ion abundance patterns (volatiles and semivolatiles) GC Resolution Check [pesticides/Aroclors (pesticides/PCBs)] Initial Calibration Continuing Calibration Internal Standards (volatiles and semivolatiles) Matrix Spike and Matrix Spike Duplicate Frequency Added to each sample, standard, and blank Added to each sample, standard, and blank Analyzed at least every 12 hours for each matrix and level Prepared with each group of 20 samples or less of same matrix and level, or each time samples are extracted by the same procedure Analyzed after a sample which contains compounds at concentrations greater than the calibration range Every 12 hours on each GC column used for analysis Prepared and stored with each set of samples Every 12 hours for each instrument used for analysis Prior to initial calibration, on each instrument used for analysis Upon initial set up of each instrument, and each time continuing calibration fails to meet the acceptance criteria Every 12 hours for each instrument used for analysis Added to each sample, standard, and blank Once every 20 or fewer samples of same fraction, matrix, and level in an SDG PERFORMANCE MONITORING ACTIVITIES Laboratory performance monitoring activities are provided primarily by AOC and the Regions to ensure that contract laboratories are producing data of the appropriate quality. EPA performs on-site laboratory audits, data package audits, GC/MS and/or GC/ECD tape audits, and evaluates laboratory performance through the use of blind performance evaluation samples. For more information, or for suggestions to improve this analytical service, please contact: Terry Smith Organic Program Manager USEPA/AOC Ariel Rios Building (5204G) 1200 Pennsylvania Avenue, NW Washington, DC 20460 703-603-8849 FAX: 703-603-9112 A-14 ------- United States Environmental Protection Agency Office of Solid Waste and Emergency Response Publication 9240.0-32FSA January 2000 Low Concentration Organic Analytical Service for Superfund (Water Matrix) (OLC02.1) Office of Emergency and Remedial Response Analytical Operations/Data Quality Center (5204G) Quick Reference Fact Sheet Under the legislative authority granted to the U.S. Environmental Protection Agency (EPA) under the Comprehensive Environmental Response, Compensation, and Liability Act of 1980 (CERCLA) and the Superfund Amendments and Reauthorization Act of 1986 (SARA), EPA develops standardized analytical methods for the measurement of various pollutants in environmental samples from known or suspected hazardous waste sites. Among the pollutants that are of concern to the EPA at such sites, are a series of volatile, semivolatile, and pesticide/Aroclor (pesticide/PCB) compounds that are analyzed using gas chromatography coupled with mass spectrometry (GC/MS) and gas chromatography with an electron capture detector (GC/ECD). The Analytical Operations/Data Quality Center (AOC) of the Office of Emergency and Remedial Response (OERR) offers an analytical service that provides data from the analysis of groundwater and drinking water type samples for organic compounds for use in the Superfund decision-making process. Through a series of standardized procedures and a strict chain-of-custody, the low concentration organic analytical service produces data of known and documented quality. This service is available through the Superfund Contract Laboratory Program (CLP). DESCRIPTION OF SERVICES The low concentration organic analytical service provides a technical and contractual framework for laboratories to apply EPA/CLP analytical methods for the isolation, detection, and quantitative measurement of 41 volatile, 59 semivolatile, and 28 pesticide/Aroclor (pesticide/PCB) target compounds in low concentration groundwater and drinking water type samples. The CLP provides the methods to be used and the specific technical, reporting, and contractual requirements, including quality assurance, quality control, and standard operating procedures, by which EPA evaluates the data. The data turnaround time for this contract is 14 days after laboratory receipt of the last sample in the set. DATA USES This analytical service provides data which EPA uses for a variety of purposes, such as determining the nature and extent of contamination at a hazardous waste site, assessing priorities for response based on risks to human health and the environment, determining appropriate cleanup actions, and determining when remedial actions are complete. The data may be used in all stages of a hazardous waste site including site inspections, Hazard Ranking System scoring, remedial investigations/ feasibility studies, remedial design, treatability studies, and removal actions. In addition, this service provides data that are available for use in Superfund enforcement/litigation activities. TARGET COMPOUNDS The compounds and quantitation limits for which this service is applicable are listed in Table 1. The lowest quantitation limits reportable are 1 ppb for the volatile compounds, 5 ppb for the semivolatile compounds, and 0.01 ppb for the pesticide/Aroclor (pesticide/PCB) compounds. Specific sample quantitation limits are highly matrix dependent. The list of target compounds for this service was originally derived from the EPA Priority Pollutant List of 129 compounds. In the years since the inception of the CLP, compounds have been added to and deleted from the Target Compound List (TCL), based on advances in analytical methods, evaluation of method performance data, and the needs of the Superfund program. A-15 ------- Table 1. Target Compound List and Contract Required Quantitation Limits (CRQLs) in ug/L (OLC02.1) VOLATILES 1. Chloromethane 1 2. Bromomethane 1 3. Vinyl Chloride 1 4. Chloroethane 1 5. Methylene Chloride 2 6. Acetone 5 7. Carbon Bisulfide 1 8. 1,1-Dichloroethene 1 9. 1,1-Dichloroethane 1 10. cis-l,2-Dichloroethene 1 11. trans-1,2-Dichloroethene 1 12. Chloroform 1 13. 1,2-Dichloroethane 1 14. 2-Butanone 5 15. Bromochloromethane 1 16. 1,1,1-Trichloroethane 1 17. Carbon Tetrachloride 1 18. Bromodichloromethane 1 19. 1,2-Dichloropropane 1 20. cis-l,3-Dichloropropene 1 21. Trichloroethene 1 22. Dibromochloromethane 1 23. 1,1,2-Trichloroethane 1 24. Benzene 1 25. trans-1,3-Dichloropropene 1 26. Bromoform 1 27. 4-Methyl-2-pentanone 5 28. 2-Hexanone 5 29. Tetrachloroethene 1 30. 1,1,2,2-Tetrachloroethane 1 31. 1,2-Dibromoethane 1 32. Toluene 1 33. Chlorobenzene 1 34. Ethylbenzene 1 35. Styrene 1 36. Xylenes (total) 1 37. 1,3-dichlorobenzene 1 38. 1,4-Dichlorobenzene 1 39. 1,2-Dichlorobenzene 1 40. l,2-dibromo-3-chloropropane 1 41. 1,2,4-Triclorobenzene 1 SEMTVOLATILES 42. Phenol 5 43. bis-(2-Chloroethyl)ether 5 44. 2-Chlorophenol 5 45. 2-Methylphenol 5 46. 2,2'-oxybis(l-Chloropropane) 5 47. 4-Methylphenol 5 48. N-Nitroso-di-n-propylamine 5 49. Hexachloroethane 5 50. Nitrobenzene 5 51. Isophorone 5 52. 2-Nitrophenol 5 53. 2,4-Dimethylphend 5 54. bis-(2-Chloroethoxy)methane 5 55. 2,4-Dichlorophenol 5 56. Naphthalene 5 57. 4-Chloroaniline 5 58. Hexachlorobutadiene 5 59. 4-Chloro-3-methylphenol 5 60. 2-Methylnaphthalene 5 61. Hexachlorocyclopentadiene 5 62. 2,4,6-Trichlorophenol 5 63. 2,4,5-Trichlorophenol 20 64. 2-Chloronaphthalene 5 65. 2-Nitroaniline 20 66. Dimethylphthalate 5 67. Acenaphthylene 5 68. 2,6-Dinitrotoluene 5 69. 3-Nitroaniline 20 70. Acenaphthene 5 71. 2,4-Dinitrophenol 20 72. 4-Nitrophenol 20 73. Dibenzofuran 5 74. 2,4-Dinitrotoluene 5 75. Diethylphthalate 5 76. 4-Chlorophenyl-phenylether 5 77. Fluorene 5 78. 4-Nitroaniline 20 79. 4,6-Dinitro-2-methylphenol 20 80. N-Nitrosodiphenylamine 5 81. 4-Bromophenyl-phenylether 5 82. Hexachlorobenzene 5 83. Pentachlorophenol 20 84. Phenanthrene 5 85. Anthracene 5 86. Di-n-butylphthalate 5 87. Fluoranthene 5 88. Pyrene 5 89. Butylbenzylphthalate 5 90. 3,3'-Dichlorobenzidine 5 91. Benzo(a)anthracene 5 92. Chrysene 5 93. bis-(2-Ethylhexyl)phthalate 5 94. Di-n-octylphthalate 5 95. Benzo(b)fluoranthene 5 96. Benzo(k)fluoranthene 5 97. Benzo(a)pyrene 5 98. Indeno(l,2,3-cd)pyrene 5 99. Dibenz(a,h)anthracene 5 100. Benzo(g,h,i)perylene 5 PESTICIDES/AROCLORS (PESTICIDES/PCBs) 101. alpha-BHC 0.01 102. beta-BHC 0.01 103. delta-BHC 0.01 104. gamma-BHC (Lindane) 0.01 105. Heptachlor 0.01 106. Aldrin 0.01 107. Heptachlor epoxide 0.01 108 Endosulfanl 0.01 109. Dieldrin 0.02 110. 4,4'-DDE 0.02 111. Endrin 0.02 112. Endosulfan D 0.02 113. 4,4'-DDD 0.02 114. Endosulfan sulfate 0.02 115. 4,4'-DDT 0.02 116. Methoxychlor 0.10 117. Endrin ketone 0.02 118. Endrin aldehyde 0.02 119. alpha-Chlordane 0.01 120. gamma-Chlordane 0.01 121. Toxaphene 1.0 122. Aroclor-1016 0.20 123. Aroclor-1221 0.40 124. Aroclor-1232 0.20 125. Aroclor-1242 0.20 126. Aroclor-1248 0.20 127. Aroclor-1254 0.20 128. Aroclor-1260 0.20 If the compound concentration for water samples other than low concentration groundwater and drinking are suspected of containing higher than 25 ng/L, then it is recommended that the sampler use the multi-media, multi-concentration organic analytical service. PREPARATION METHODS AND INSTRUMENTATION For semivolatile and pesticide/Aroclor (pesticide/PCB) water samples, a 1-L aliquot is extracted with methylene chloride using continuous liquid-liquid extraction or separatory funnel [for pesticides/Aroclors (pesticides/PCBs) only]. The extract is concentrated, subjected to fraction-specific cleanup procedures, and analyzed by GC/MS for semivolatiles or GC/ECD for pesticides/Aroclors (pesticides/PCBs). For volatiles, 25 mL of water is added to a purge-and-trap device and purged with an inert gas at room temperature. The volatiles purged from the sample are trapped on a solid sorbent. They are subsequently desorbed by rapidly heating the sorbent and then introduced into a GC/MS system. Table 2 summarizes the preparation methods and instruments used in this analytical service. A-16 ------- DATA DELIVERABLE^ Data deliverables for this service include both hardcopy data reporting forms and supporting raw data. The laboratory must submit data to EPA within 14 days after laboratory receipt of the last sample in the set. EPA then checks the data for compliance with contract requirements. A report of instances of noncompliance is distributed to the laboratory and the Region within 10 days from the receipt of the data. The laboratory has 10 days to reconcile defective data and resubmit the data to EPA. EPA then screens the data and sends a final data assessment report to the laboratory and the Region. QUALITY ASSURANCE The quality assurance (QA) process consists of management review and oversight at the planning, implementation, and completion stages of the environmental data collection activity. This process ensures that the data provided are of the quality required. During the implementation of the data collection effort, QA activities ensure that the quality control (QC) system is functioning effectively and that the deficiencies uncovered by the QC system are corrected. After environmental data are collected, QA activities focus on assessing the quality of data to determine its suitability to support enforcement or remedial decisions. Each contract laboratory prepares a quality assurance plan (QAP) with the objective of providing sound analytical chemical measurements. The QAP must specify the policies, organization, objectives, and functional guidelines, as well as the QA and QC activities designed to achieve the data quality requirements for this analytical service. QUALITY CONTROL The QC process includes those activities required during analytical data collection to produce data of known and documented quality. The analytical data acquired from QC procedures are used to estimate and evaluate the analytical results and to determine the necessity for, or the effect, of corrective action procedures. The QC requirements for this analytical service are shown in Table 3. Table 2. Preparation Methods and Instruments Fraction Volatiles Semivolatiles Pesticides/Aroclors (Pesticides/PCBs) Preparation Method Purge-and-trap Continuous liquid-liquid extraction Continuous liquid-liquid or separatory runnel extraction • Analytical Instrument GC/MS analysis GC/MS analysis GC/ECD analysis Table3. Quality Control QC Operation System Monitoring Compound (volatiles) Method Blanks (volatiles) Method Blanks [semivolatiles and pesticides/Aroclors (pesticides/PCBs)] Instrument Blank (volatiles) Surrogates [semivolatiles and pesticides/Aroclors (pesticides/PCBs)] Instrument Blank [pesticides/Aroclors (pesticides/PCBs)] Storage Blank (volatiles) GC/MS mass calibration and ion abundance patterns (volatiles and semivolatiles) GC Resolution Check [pesticides/Aroclors (pesticides/PCBs)] Frequency Added to each sample, standard, and blank Analyzed at least every 12 hours Prepared with each group of 20 samples or less, or each time samples are extracted Analyzed after a sample which contains compounds at concentrations greater than the calibration range Added to each sample, standard, and blank Every 12 hours on each GC column used for analysis Prepared and stored with each group of samples Every 12 hours for each instrument used for analysis Prior to initial calibration on each GC column used for analysis A-17 ------- Table 3. Quality Control (Continued) QC Operation Initial Calibration Continuing Calibration Internal Standards (volatiles and semivolatiles) Laboratory Control Sample (LCS) Laboratory Evaluation Sample Frequency Upon initial set up of each instrument, and each time continuing calibration fails to meet the acceptance criteria Every 12 hours for each instrument used for analysis Added to each sample, standard, and blank Prepared and analyzed with each group of 20 samples or less Prepared and analyzed (if provided) with each set of 20 samples or less PERFORMANCE MONITORING ACTIVITIES Laboratory performance monitoring activities are provided primarily by AOC and the Regions to ensure that contract laboratories are producing data of the appropriate quality. EPA performs on-site laboratory audits, data package audits, and GC/MS tape audits, and evaluates laboratory performance through the use of blind performance evaluation samples. For more information, or for suggestions to improve this analytical service, please contact: Terry Smith Organic Program Manager USEPA/AOC Ariel Rios Building, NW (5204G) 1200 Pennsylvania Avenue, NW Washington, DC 20460 703-603-8849 FAX: 703-603-9112 A-18 ------- Appendix B CLP Documents ANALYTICAL METHODS (WWW.EPA.GOV/SUPERFUND/PROGRAMS/CLP/PRODSERV.HTM) Title Publication No./Date Fact Sheets Multi-Media, Multi-Concentration, Inorganic Analytical Service for Superfund (ILM04.1) Quick Reference Fact Sheet * Summary of Major Changes Made to the Multi-Media, Multi- Concentration Organic Analytical Statement of Work (OLM03.2 to OLM04.2), Quick Reference Fact Sheet Multi-Media, Multi-Concentration, Organic Analytical Service for Superfund (OLM04.2), Quick Reference Fact Sheet Low Concentration Organic Analytical Service for Superfund (Water Matrix) (OLC02.1), Quick Reference Fact Sheet 9240.0-09FSC January 2000 9240.0-33FS January 2000 9240.0-08-FSD January 2000 9240.0-32FSA January 2000 Analytical USEPA Contract Laboratory Program Statement of Work for Methods Inorganics Analysis, Multi-Media, Multi-Concentration USEPA Contract Laboratory Program Statement of Work for Organics Analysis, Multi-Media, Multi-Concentration USEPA Contract Laboratory Program Statement of Work for Organics Analysis, Low Concentration Water ILM04.0, February 1995 OLM04.2, May 1999 OLC02.1, February 1996 CLP National Functional Guidelines USEPA Contract Laboratory Program National Functional Guidelines EPA-540/R-99/008 (PB99- for Organic Data Review 963506), October 1999 USEPA Contract Laboratory Program National Functional Guidelines EPA-540/R-94-013 (PB94- for Inorganic Data Review 963502), February 1994 (Most of the documents may be obtained via Acrobat Reader, which is available from the Web site.) * ILM04.1 is an interim inorganic analytical service. Further changes are expected to be released under ILM05.0 for competition during calendar year 2000. B-l ------- B-2 ------- Appendix C AOC CLP Contacts USEPA Analytical Operations/Data Quality Center (AOC1 Mailing Address: Ariel Rios Building (5204G) 1200 Pennsylvania Ave., NW Washington, DC 20460 FAX 703-603-9112 Street Address (For Fed-Ex Delivery and Visits): 1235 Jefferson Davis Hwy Crystal Gateway I, 12th Floor Arlington, VA 22202 Name Dana S. lulls Edward Brosnan Jacqueline Eaton Michael Johnson Tanya Mitchell Terry Smith Lucinda Taylor Willie Wong Responsibilities Director of the Analytical Operations/Data Quality Center Scheduling, Tracking, Reporting, and Invoicing of CLP Samples AOC Project Officer for CLP Funding CLP Document Officer CLP Budget Analyst Automated Data Processing Project Coordinator Data Assessment Tools Project Coordinator Contract Compliance Screening for CLP CLP Inorganic Program Manager CLP Organic Program Manager CLP Organic Low Concentration Program Manager SMO Project Officer Cost Recovery Contact FORMS II Lite (Sample Tracking Software) Electronic Commerce (EC) for Laboratories Phone Number/Email address 703-603-8993 email: tulis.dana@epa.gov 703-603-8866 email: brosnan.edward@epa.gov 703-603-8813 email: eaton.jacqueline@epa.gov 703-603-0266 email: johnson.michaels@epa.gov 703-603-8872 email: mitchell.tanya@epa.gov 703-603-8849 email: smith.terry@epa.gov 703-603-8818 email: tayjor.lucinda@epa.gov 703-603-8846 email: wong.willie@epa.gov For the latest contact information, please see the CLP Web site at: http://www.epa.gov/superfund/proqrams/clp/contact.htm C-l ------- USEPA CLP Contact List Regional Designations Region 1 ME, NH.VT, MA, Rl, CT II NY, NJ, PR, VI III PA, DE, MD, VA, WVA, DC IV NC, SC, KY, TN, GA, FL, AL, MS V OH, IL, IN, Ml, Wl, MN VI LA, AR, OK, TX, NM VII IA, MO, KS, NE VIII ND, SD, MT, WY, CO, UT IX CA, AZ, NV, HI, Guam X WA, OR, ID, AK Title CLPPO RSCC CLPPO RSCC CLPPO RSCC CLPPO RSCC CLPPO RSCC CLPPO RSCC CLPPO RSCC CLPPO RSCC CLPPO RSCC CLPPO RSCC Name Jennie Han-Liu Christine Clark Jennifer Feranda Jennifer Feranda Dan Slizys Jon Kwedar Edward Messer Debbie Colquit Cecilia Moore Howard Pham Ray Flores (alt. Marvelyn Humphrey) Myra Perez (alt. L.C. Miner) Larry Marchin Nicole Roblez Carol Beard Carol Beard Steve Remaley Rich Freitas Bruce Woods Melody Walker Phone Number 781-860-4379 781-860-4615 732-321-6687 732-321-6687 410-305-2734 410-305-3021 706-355-8560 706-355-8804 312-886-1488 312-353-2310 281-983-2139 (281-983-2140) 281-983-2130 (281-983-2116) 913-551-5170 913-551-5130 303-312-6687 303-312-6687 415-744-1496 415-744-2315 206-553-1193 206-553-1106 Fax Number 781-860-4397 781-860-4397 732-906-6622 732-906-6622 410-305-3095 410-305-3095 706-355-8803 706-355-8803 312-886-0186 312-886-0186 281-983-2248 281-983-2248 281-983-2248 281-983-2248 913-551-5218 913-551-5218 303-312-6897 303-312-6897 415-744-1476 415-744-1476 206-553-8210 206-553-8210 C-2 ------- Appendix D List of Acronyms from Chapters 1 and 2 AA Atomic Absorption AOC Analytical Operations/Data Quality Center (EPA) ADP Automated Data Processing CADRE Computer Aided Data Review & Evaluation CCS Contract Compliance Screening CERCLA Comprehensive Environmental Response Compensation and Liability Act CLASS Contract Laboratory Analytical Services Support CLP Contract Laboratory Program CLP PO Contract Laboratory Program Project Officer DART Data Assessment Rapid Transmittal DAT Data Assessment Tool EPA Environmental Protection Agency GC/ECD Gas Chromatography/Electron Capture Detector GC/MS Gas Chromatography/Mass Spectrometry HRS Hazard Ranking System ICP Inductively Coupled Plasma PE Performance Evaluation PCBs Polychlorinated Biphenyls PO Project Officer PRP Potentially Responsible Party QA Quality Assurance QAPP Quality Assurance Project Plan QATS Quality Assurance Technical Support QC Quality Control RAS Routine Analytical Service RCRA Resource Conservation and Recovery Act RSCC Regional Sample Control Center (EPA Region) SAP Sampling and Analysis Plan SARA Superfund Amendments and Reauthorization Act SMO Sample Management Office SOW Statement of Work D-l ------- D-2 ------- Appendix E Glossary Analyte: The element, ion, or parameter an analysis seeks to determine; the element of interest. Analytical Protocol: See Statement of Work (SOW). Analytical Operations/Data Quality Center (AOC): The US EPA Center which directs the national Contract Laboratory Program. Atomic Absorption (AA): A procedure for inorganic analysis based on the absorption of radiation by mercury vapor (Cold Vapor), flame, or graphite furnace Brownfields: Abandoned, idle, or under-used industrial and commercial facilities where expansion or redevelopment is complicated by real or perceived environmental contamination. Computer Aided Data Review and Evaluation (CADRE): The CADRE system evaluates QC results against data review criteria appropriate for a specified corresponding analytical method or procedure. Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA): Initiated in December 1980, CERCLA provided broad federal authority to respond directly to the release or possible release or hazardous substances that may endanger human health or the environment. CERCLA also established a trust fund to provide for cleanup when no responsible party could be identified, hence CERCLA is commonly referred to as "Superfund". Contract Compliance Screening (CCS): The screening of electronic and hardcopy data deliverables for completeness and compliance with the contract. This screening is done under EPA direction by the SMO Contractor. Contract Laboratory Analytical Services Support (CLASS): Contract that operates the Sample Management Office (SMO) and is awarded and administered by EPA. The contractor-operated SMO office provides management, operations, and administrative support to the CLP. The SMO contractor schedules and tracks sample shipments for CLP analytical services requests. Contract Laboratory Program (CLP): Supports the EPA's Superfund effort by providing a range of chemical analytical services to produce environmental data of known quality. This program is directed by the Analytical Operations/Data Quality Center of EPA. Contract Required Detection Limit (CRDL): Minimum level of detection acceptable under the contract Statement of Work. Contract Required Quantitation Limit (CRQL): Minimum level of quantitation acceptable under the contract Statement of Work. Cost Recovery. A legal process by which potentially responsible parties who contributed to contamination at a Superfund site can be required to reimburse the Trust Fund for money spent during any cleanup actions by the federal government. Cost Recovery Request A request issued by an Authorized Cost Recovery Requestor for detailed cost and sample documentation associated with a Superfund site. Cyanide (Total): Cyanide ion and complex cyanides converted to hydrocyanic acid (HCN) by reaction in a reflux system of a mineral acid in the presence of magnesium ion. Data Assessment Rapid Transmittal (DART): DART is an active notification system providing up-to-the- minute transmittal of the CCS and CADRE evaluation report data to CLP customers. Data Assessment Tool: A software driven process that incorporates CCS, CADRE, and DART designed to produce enhanced CLP deliverables and more usable reports in a standard format. E-l ------- Data Turnaround Time: The maximum length of time allowed for laboratories to submit analytical data to EPA in order to avoid financial penalties (i.e., liquidated damages). Data turnaround time begins at the validated time of sample receipt (VTSR) at the laboratory. Data Validation: Data validation is based on Region-defined criteria and limits, professional judgement of the data validator, and (if available) the Quality Assurance Project Plan (QAPP) and Sampling and Analysis Plan (SAP). Feasibility Study: A description and analysis of potential cleanup alternatives for a site such as one on the National Priorities List. The feasibility study usually recommends selection of a cost-effective alternative. It usually starts as soon as the remedial investigation is underway. Together, they are commonly referred to as the "RI/FS". Gas Chromatography (GC): The instrument used to separate analytes on a stationary phase within a chromatographic column. Gas Chromatography is frequently used with other instruments for analyzing organic compounds: a). Mass Spectrometry. In volatile and semivolatile analysis, the compounds are detected by a Mass Spectrometer (MS). b). Electron Capture: In pesticide/Aroclor analysis, the compounds are detected by an Electron Capture Detector (ECD). Hazard Ranking System (MRS): A numerically based screening system that uses information from initial, limited investigations to assess the relative potential of sites to pose a threat to human health or the environment. MRS is the principal mechanism EPA uses to place uncontrolled waste sites on the National Priorities List (NPL). Hazardous Waste Site: A site contaminated with substances that can pose a substantial or potential hazard to human health or the environment. Inductively Coupled Plasma - Atomic Emission Spectroscopy (ICP-AES): A technique for the simultaneous or sequential multi-element determination of elements in solution. The basis of the method is the measurement of atomic emission by an optical spectroscopic technique. Characteristic atomic line emission spectra are produced by excitation of the sample in a radio frequency inductively coupled plasma. ILM04.1: The current inorganic analytical protocol. National Functional Guidelines (NFG): Documents designed to offer guidance on inorganic, organic, and organic low concentration CLP analytical data evaluation and review. National Priorities List (NPL): A list of sites for hazardous waste cleanup under the Superfund program. Office of Solid Waste and Emergency Response (OSWER): The EPA office that provides policy, guidance, and direction for the EPA's solid waste and emergency response programs, including Superfund. OLC02.1: The current organic low concentration water analytical protocol. OLM04.2: The current organic analytical protocol. OSCs: On-Scene Coordinators for the Superfund's Removal Program. Performance Evaluation (PE) Sample: A sample of known composition provided by EPA for contractor analysis. Used by EPA to evaluate contractor performance. Pesticides: Substances intended to repel, kill, or control any species designated a "pest", including weeds, insects, rodents, fungi, bacteria, and other organisms. E-2 ------- Polychlorinated Biphenyls (PCBs): A group of toxic, persistent chemicals used in electrical transformers and capacitors for insulating purposes, and in gas pipelines systems as a lubricant. The sale and new use of PCBs were banned by law in 1979. Quality Assurance (QA): An integrated system of management activities involving planning, implementation, assessment, reporting, and quality improvement to ensure that a process, item, or service is of the type and quality needed and expected by the customer. Quality Control (QC): The overall system of technical activities that measures the attributes and performance of a process, item, or service against defined standards to verify that they meet the stated requirements established by the customer; operational techniques and activities that are used to fulfill requirements for quality. Quality Assurance Technical Support (QATS) Laboratory: A contractor-operated facility operated under the QATS contract, awarded and administered by EPA. Remedial Action: The construction or clean-up phase of a Superfund site cleanup. Remedial Design: A phase of remedial action that follows the remedial investigation/feasibility study and includes development of engineering drawings and specifications for a site cleanup. Remedial Investigation: An in-depth study designed to gather data needed to determine the nature and extent of contamination at a Superfund site, establish site cleanup criteria, identify preliminary alternatives for remedial action, and support technical and cost analyses of alternatives. The remedial investigation is usually done with the feasibility study. Together they are usually referred to as the "RI/FS". Remedial Project Manager (RPM): The EPA or state official responsible for overseeing on-site remedial action. Remedial Response: Long-term action that stops or substantially reduces a release or threat of a release of hazardous substances that is serious but not an immediate threat to public health. Remediation: Cleanup or other methods used to remove or contain a toxic spill or hazardous materials from a Superfund site. Routine Analytical Service (RAS): The standard inorganic, organic, and organic low concentration high volume, multi-component analyses available through the CLP. Regional Sample Control Center (RSCC): The RSCC coordinates Regional sampling efforts. Sample: A single, discrete portion of material to be analyzed, which is contained in single or multiple containers and identified by a unique sample number. Sample Management Office (SMO): A contractor-operated facility operated by the Contract Laboratory Analytical Services Support (CLASS) contract, awarded and administered by the EPA. Statement of Work (SOW): A document which specifies how laboratories analyze samples under a particular CLP analytical program. Superfund: The program operated under the legislative authority of CERCLA and SARA that funds and carries out EPA removal and remedial activities at hazardous waste sites. These activities include establishing the National Priorities List, investigating sites for inclusion on the list, determining their priority, and conducting and/or supervising cleanup and other remedial actions. Superfund Amendments and Reauthorization Act (SARA): The 1986 amendment to CERCLA. E-3 ------- E-4 ------- |