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Quality Assurance Manual Frontier Analytical Laboratory 5172 Hillsdale Circle El Dorado Hills, CA 95762 916-934-0900 This Quality Assurance Manual contains confidential and proprietary information and may not be copied or distributed without the written permission of Frontier Analytical Laboratory. QA Officer: Dan Vickers QA No.1A-Rev.12 Effective: 3/30/2010 -Cover Page- Uncontrolled

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Page 1: Quality Assurance Manual - Frontier Analytical · Quality Assurance Manual Frontier Analytical Laboratory 5172 Hillsdale Circle El Dorado Hills, CA 95762 916-934-0900 This Quality

Quality Assurance Manual

Frontier Analytical Laboratory 5172 Hillsdale Circle

El Dorado Hills, CA 95762 916-934-0900

This Quality Assurance Manual contains confidential and proprietary information and may not be copied or distributed without the written permission of Frontier Analytical Laboratory.

QA Officer: Dan Vickers

QA No.1A-Rev.12 Effective: 3/30/2010 -Cover Page-

Uncontrolled

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QA No. 1A Revision: 12 Effective: 3/30/2010 Replaces: Rev.11

Section 2

INTRODUCTION

This manual describes the quality assurance and quality control program for Frontier Analytical Laboratory. It provides the information necessary to maintain an effective quality assurance program. This program was established to ensure that analytical data is within acceptable method-specific control limits and to verify that all data complies with project-specific quality guidelines. The QA manual describes various aspects of the laboratory, our quality objectives, and how we intend to achieve these quality objectives throughout the analytical process.

The policies described in this manual are written and detailed in Standard Operating

Procedures (SOPs). The SOPs are used to implement the activities described in this manual. Frontier Analytical Laboratory staff maintain and follow all SOPs thus ensuring quality, consistency, and reliability throughout our laboratory processes. The QA manual and the SOPs furnish detailed documentation to clients, employees and agencies so they may fully comprehend quality control and quality assurance as it pertains to Frontier Analytical Laboratory.

Frontier Analytical Laboratory specializes in GC/MS analysis of polychlorinated dioxins and

furans (PCDDs/PCDFs), polychlorinated biphenyls (PCBs), and polycyclic aromatic hydrocarbons (PAHs) utilizing an array of governmental analytical methods. Our mission is to provide high quality data, immediate responsive customer service and short turnaround times to every client.

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Section 3

QUALITY POLICY STATEMENT

The Quality Assurance Officer is responsible for the publication and distribution of the Quality Assurance Manual. The manual is routinely reviewed by personnel. In the event of significant changes in the quality procedures, the manual is revised then reviewed and authorized by the senior management team. New revisions are immediately put into practice and the previous revisions are stored and archived accordingly. The signatures of the senior management team in Section 1 verify authorization and approval of the Quality Assurance Manual. Quality Assurance Manuals are available for Frontier Analytical Laboratory staff and are updated as new revisions arise.

Mission Statement

Frontier Analytical Laboratory’s mission is to provide our clients with the highest quality scientific data possible that is both legally defensible and scientifically valid. In addition, we will develop long-term relationships with customers based on mutual trust and respect by consistently delivering the highest quality service with the shortest possible turnaround times in the industry.

Quality Assurance Policies

Frontier Analytical Laboratory Standard Operating Procedures (SOPs) are based on method requirements and accurately reflect each laboratory operation. SOPs are followed to ensure sample and data integrity and security. Personnel receive extensive hands-on training on laboratory functions ensuring consistent and high quality work throughout the process. Initial and ongoing validation studies are performed for each analytical method to prove reliability whenever extensive modifications or personnel changes occur. Frontier Analytical Laboratory uses a quality control system, including but not limited to method blanks, OPRs, LCS, IPRs, MS/MSDs, QCs, and audit samples, which verifies ongoing precision and accuracy of analytical results. Extensive documentation and records of each step of the process are maintained to ensure accountability, traceability and repeatability. Laboratory equipment and materials used throughout the analytical process are properly maintained and verified to meet applicable requirements.

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Corrective actions will be implemented if testing discrepancies occur, or upon departure from documented policies or operating procedures. It is assumed that all samples received could potentially be used for evidentiary purposes. Therefore the chain of custody and all associated data records are treated as legal documents. Policies for data reduction and storage shall satisfy applicable NELAC standards. Method-specific criteria ensure the proper functioning of the equipment used to capture, manipulate, and record analytical data. Management regularly reviews all upcoming bids and projects to ensure that Laboratory capacity is not overburdened and that proper attention to quality is maintained at all times. Under no circumstances will fraudulent or illegal actions be tolerated. We will hold ourselves to the highest ethical standards at all times. Annual ethics training ensures adherence to these policies. All principals and employees will be bound to the policies and procedures outlined in this document and our SOPs.

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Section 4

THE LABORATORY

Frontier Analytical Laboratory, Inc. 5172 Hillsdale Circle

El Dorado Hills, CA 95762

Tel: (916) 934-0900 Fax: (916) 934-0999

Email: [email protected]

Frontier Analytical Laboratory is located in a custom designed 5,000 square foot laboratory in El Dorado Hills, California. The laboratory has an open floor plan to enhance communication between all facets of laboratory operations.

Frontier Analytical Laboratory has a spacious sample login and storage area. Samples are stored in freezers and refrigerators that are kept under lock and key and are accessible only by authorized personnel. Freezer and refrigerator temperatures are regularly monitored.

The sample preparation laboratory is designed to maximize efficiency and productivity while maintaining a safe work environment.

The instrument room accommodates two magnetic sector instruments. The instrument room is climate controlled and designed to maintain proper instrument operating conditions. Rotary pump emissions are evacuated and instrument chillers are isolated from the instrument room to maximize safety and comfort.

There is a common data review area that promotes communication between analysts interpreting and reviewing data. This helps accommodate our multi-tiered review process.

Frontier Analytical Laboratory has a secure data archive room designed to meet USEPA Good Laboratory Practices guidelines regarding data security (40 CFR sec.160). The data archive room contains raw data, manual and electronic data used to generate final reports, archived SOPs, logbooks, and electronic backup files.

During business hours, entrances and exits to the facility remain locked unless monitored by

Frontier Analytical Laboratory personnel. Visitors are required to sign the Visitor Logbook and are accompanied by Frontier Analytical Laboratory personnel. After business hours, all entrances and exits are locked and require a key or entry code to gain access. The alarm system is monitored twenty-four hours a day by an offsite security company.

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Chemicals are stored in accordance with local fire and environmental regulations. This includes flameproof solvent cabinets and flameproof fifty-five gallon drum cabinets for solvent and laboratory waste. The building is equipped with an overhead sprinkler system as well as safety eye wash and drench hose stations. The disposal of hazardous waste is done in accordance with EPA guidelines (40 CFR part 261). Frontier Analytical Laboratory contracts with an authorized waste carrier to dispose of hazardous waste.

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Section 5

Company Structure

Brad Silverbush

Director of Operations

Dan Vickers Quality Assurance Officer

Director of Technical Services Safety Officer

Tom Crabtree

Director of Mass Spectrometry

Kathy Zipp Accounting

Administrator

Gabby Navarro Associate Scientist Extraction Chemist

Gordon Gregory Associate Scientist Extraction Chemist

Quality Assurance Officer/ Director of Technical Services/Safety Officer Responsibilities include technical guidance and support for routine analysis and research and

development of new methodologies. Reviews and interprets analytical data and final reports. Responsibilities also include client management and personnel training. As Quality Assurance Officer, he manages the QA activities of the entire laboratory. As Safety Officer he is responsible for monthly/annual equipment and facility inspections, ensures that employees follow written safety procedures at all times and provides safety training on an as needed basis.

Director of Operations Responsibilities include technical guidance and support for instrument operations, routine analysis

and research and development of new methodologies. Additional responsibilities include personnel training, client and project management, sales and marketing, reviewing and interpreting analytical data, and preparing and reviewing final reports. He is also responsible for the daily operations of the laboratory.

Director of Mass Spectrometry Responsibilities include documenting, performing, and/or supervising all preventative and on demand

maintenance of mass spectrometers. He maintains an ample supply of mass spectrometer consumables and spare parts for preventative and on demand maintenance. In addition, he is responsible for routine analysis, client and project management, reviewing and interpreting analytical data as well as preparing and reviewing final reports.

Accounting Administrator Responsibilities include providing bookkeeping services for the laboratory. This includes performing

accounts payable, invoicing and payroll. Responsible for administrative support to the Directors including phone routing, office supply inventory, final report packaging, marketing programs and client correspondence.

Associate Scientist/Extraction Chemist The chemist is responsible for following Frontier Analytical Laboratory’s standard operating

procedures used in the extraction of Dioxins/Furans, polychlorinated biphenyls and polyaromatic hydrocarbons from a variety of matrices. The chemist will also adhere to Frontier Analytical Laboratory’s ethics policy and safety policy at all times while performing their duties. The chemist will coordinate their work within the extraction lab to meet all extraction hold times and to prioritize samples based on their project due date. The chemist will perform routine tasks such as reagent preparation, glassware cleaning, kiln loading/unloading, inventory stocking and waste disposal. The chemist will also perform non-routine duties such as laboratory cleaning, laboratory equipment preventative maintenance and expired sample disposal. The chemist will coordinate with other laboratory personnel in performing sample control duties.

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Daniel P. Vickers

Director of Technical Services/Quality Assurance Officer/Safety Officer

EDUCATION B.S. Biochemistry, University of California, Davis, CA (1987) Minor in Entomology EXPERIENCE Present Director of Technical Service/Quality Assurance Officer/Safety

Officer, Frontier Analytical Laboratory Mr. Vickers, a founder, is responsible for maintaining and operating the sample preparation laboratory. He supplies technical guidance and support for routine analysis and development of new methodologies. He is also responsible for routine analysis, reviewing and interpreting data, training personnel, client and project management, preparing and reviewing final reports. In addition, he manages the QA activities of the entire laboratory. He works with the other Directors to ensure that the QAPP and SOP guidelines are followed. As Safety Officer, he is responsible for verifying that laboratory safety procedures are being followed by the staff at all times. This verification includes monthly safety inspections, yearly equipment checks, safety training and routine safety SOP review.

1994-2001 Senior Scientist, ALTA Analytical Laboratory

As Senior Scientist at ALTA Analytical Laboratory Mr. Vickers managed and trained employees on various methodologies. He developed, tested and implemented procedures that increased productivity and quality. He successfully met all sample hold times and client deadlines.

1990-1994 Senior Field Service Engineer, Millipore/Waters Corporation As Senior Field Service Engineer, Mr. Vickers performed new equipment startup, customer training and both preventative and on demand maintenance on all Waters equipment.

1987-1990 GCMS Operator, Enseco-Cal Lab As lead chemist, Mr. Vickers assigned projects and provided technical assistance. He performed all EPA Methods for PCDD/F analysis. In addition, he interpreted data and provided troubleshooting experience.

QUALIFICATIONS Mr. Vickers has over twenty-two years experience in production analytical laboratories including nineteen years experience in the field of environmental mass spectrometry. Much of this experience has involved PCDD/PCDF analysis in a variety of matrices. PROFESSIONAL AFFILIATIONS American Chemical Society The NELAC Institute (TNI) Member

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Bradley B. Silverbush

Director of Operations EDUCATION B.S. Biochemistry, University of California, Davis, CA (1988) EXPERIENCE Present Director of Operations, Frontier Analytical Laboratory

Mr. Silverbush, a founder, directs and performs routine analysis and method development work in the Mass Spectrometry department. He is responsible for routine maintenance and operation of the HRMS instruments, as well as the preparation, QC, etc. of all standards. In addition Mr. Silverbush is responsible for personnel training, reviewing and interpreting data, client and project management, sales and marketing, and preparing and reviewing final reports.

1991-2001 Senior Scientist, ALTA Analytical Laboratory

As Senior Scientist at ALTA Analytical Laboratory Mr. Silverbush performed analysis and method development work in the High Resolution Mass Spectrometry department. He was responsible for routine maintenance of HRMS instruments and for the preparation, QC, etc. of all standards. In addition, Mr. Silverbush trained new staff, supervised other Senior Scientists, reviewed and interpreted data, prepared final reports, and interfaced with clients.

1990-1991 GC/MS Chemist, Enseco-Cal Lab As GC/MS Chemist at Enseco-Cal Lab Mr. Silverbush was responsible for the operation and maintenance of quadrupole GC/MS instruments. His duties entailed sample analysis by EPA methods for volatiles. He was also responsible for the training of the staff in the department.

1988-1990 Extraction Chemist, Enseco-Cal Lab Duties entailed sample extraction for Dioxin/Furan Analysis by High Resolution Mass Spectrometry. In addition, he was responsible for training new staff, and the development of new extraction techniques.

QUALIFICATIONS Mr. Silverbush has over twenty-two years experience in production analytical laboratories and environmental mass spectrometry. Most of this experience has involved PCDD/PCDF, PCB, and PAH analysis using HRMS instrumentation on a variety of matrices. PROFESSIONAL AFFILIATIONS American Society for Mass Spectrometry American Chemical Society California Water Environment Association Technical Association for the Pulp and Paper Industry

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Thomas C. Crabtree

Director of Mass Spectrometry

EDUCATION Present Computer Science, Business Administration EXPERIENCE Present Director of Mass Spectrometry, Frontier Analytical Laboratory

Mr. Crabtree, a founder, is responsible for maintenance, repairs and product development of all mass spectrometers. In addition, he performs routine analysis and method development. He is also responsible for personnel training, reviewing and interpreting data, client and project management, sales and marketing, and preparing and reviewing final reports.

2000-2001 Chemist/Analyst 5, Severn Trent Laboratory

Mr. Crabtree was responsible for routine maintenance and operation of the HRMS instruments. In addition, he performed HRMS analysis using an array of EPA, CARB, and NCASI methods.

1991-2000 Product Manager, GB Scientific, Inc.

Mr. Crabtree developed and maintained the Spares Department, and was responsible for all product development. He developed and maintained a network of computers as well as the Access Database to track customers, inventory, sales and shipping information. He also provided technical support to customers, field service and instrument re-location.

1979-1991 Senior Research Assistant, Chevron Research Company Mr. Crabtree was responsible for operating and maintaining mass spectrometers, and associated DEC, PDP, VAX, and Alpha mini computers. This included general laboratory functions, chemical analysis, separation sciences, wet chemistry, record keeping, database maintenance, ordering of lab supplies, and maintaining service contracts with vendors. He maintained VG 7070H, 7070E, 70VSE, ZAB, HP 5970A,B, 5971, Finnigan 4500, 5100, TSQ70, ITD, Varian Saturn, CEC & Nuclide mass spectrometers.

QUALIFICATIONS Mr. Crabtree has over thirty years experience in the mass spectrometry field. He has serviced and maintained a broad range of mass spectrometers. He also has extensive knowledge of operating systems as well as a great deal of technical experience.

Professional Affiliations American Society for Mass Spectrometry American Chemical Society

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Section 6

ANALYTICAL SERVICES

The focus of Frontier Analytical Laboratory is to provide state-of-the-art high-resolution mass spectrometry services to our private and governmental clients. Frontier Analytical Laboratory operates with the intent of providing data of the highest quality, responsive customer service and short turnaround times.

Frontier Analytical Laboratory’s expertise lies in the analysis of semivolatile organic compounds such as Dioxin/Furans (PCDDs/PCDFs), Polychlorinated Biphenyls (PCBs), and Polycyclic Aromatic Hydrocarbons (PAHs).

Frontier Analytical Laboratory represents a diverse and experienced group of mass spectrometry specialists with over fifty years of combined experience. This diversity in experience and unique size enables Frontier Analytical Laboratory to provide a variety of expertise as well as personal service. Client inquiries and requests can be discussed with the specialist working on the project. Frontier Analytical Laboratory staff have participated in and had hands on experience in the development of such methods as USEPA Methods 8290, 1613A/1613B and California Air Resources Board (CARB) Method 428.

Frontier Analytical Laboratory scientists have actively participated in interlaboratory round robin studies and certification programs such as the USEPA (ITD) study of PCDD’s/PCDF’s in pulp and paper; Cambridge Isotopes Lab (CIL) study on Coplanar PCBs and PCDD/PCDF’s in fish; the National Council for Air and Stream Improvement (NCASI) lab certification program study and the NCASI/USEPA variability study on PCDD/PCDF’s in pulp and paper.

Frontier Analytical Laboratory provides integrity, reliability and accountability unsurpassed in the environmental industry. Frontier Analytical Laboratory offers a vast amount of experience and expertise in EPA Methods 8280, 8290, 1613A/1613B, 1668, TO-9, 0023, NCASI 551, CARB Method 428.

When laboratory services other than PCDD/PCDF, PCB, or PAH analyses are required, we

will notify the client, in writing, of our intention to sub-contract the requested services. Prior to commencing work, we will attempt to get written approval from the client regarding the use of a subcontracting lab. We will only subcontract to laboratories that are NELAP certified in that specific area of testing (See Table 6.1 for Register of NELAP Subcontractors). Reputation, experience, and/or the customer’s request will determine which laboratory will be chosen to fulfill these needs. The original reports from subcontracted analytical work will be submitted to the client. In all cases, work must be performed at a level consistent with Frontier Analytical Laboratory’s rigorous quality standards.

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Table 6.1

Register of NELAP Accredited Subcontractors 1.) Air Toxics Limited

180 Blue Ravine Road Folsom, CA 95630 Phone: (916) 985-1000 Fax: (916) 985-1020 Contact: Jennifer Miller e-mail: [email protected]

2.) California Laboratory Services (CLS) 3249 Fitzgerald Road Rancho Cordova, CA 95742 Phone: (800) 638-7301 Contact: Mark Smith e-mail: [email protected]

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Section 7

ANALYTICAL STANDARDS

Receipt, inventory, storage, and preparation of reference standards and standard solutions are summarized in SOPs that comply with EPA guidelines set forth in 40 CFR 160. The traceability of these standards to known reference values represents a cornerstone of the entire analytical process. Whenever possible, Frontier Analytical Laboratory employs reference materials that are traceable to national standards, such as NIST or EPA certified reference materials.

Standards Receipt

Frontier Analytical Laboratory procures standards from approved chemical suppliers. All standards received by Frontier Analytical Laboratory are required to meet specified criteria before they are accepted and classified as reference standards. The acceptance criteria include the physical condition of standards as well as associated standards documentation. Once standards are deemed acceptable, they are logged in and all pertinent information is documented on a Reference Standard Tracking Log (Figure 7.1). Once a standard is properly logged in, it is labeled with the unique reference log number (Ryy/mm/dd), reference standard name, lot number, concentration, and expiration date. All reference standards are stored separately from samples and extracts in designated cabinets, refrigerators, or freezers. This is determined by the manufacturer’s recommendation. Acceptable refrigerator and freezer temperatures are 0o C to 4o C and from –10o C to –20o C respectively. Refrigerator and freezer temperatures are monitored on a regular basis.

Standards Preparation

Reference standards are used to prepare standard solutions. Standard solutions are used as stock solutions, calibration solutions, and spiking solutions. Standard solutions are documented on the Standards Solutions Tracking Log (Figure 7.2). Once the standard solutions are properly prepared and logged, they are labeled with the unique reference log number (yy/mm/dd), standard solution name, concentration, and expiration date. All standard solutions are stored separately from samples, extracts, and reference standards in designated cabinets and refrigerators. This is determined by the manufacturer’s recommendation. Acceptable refrigerator temperatures are 0o C to 4o C. Standard refrigerator temperatures are monitored on a regular basis. All standard solutions are deemed acceptable once their accuracy and precision have been verified to be within a given analytical methods guidelines.

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Figure 7.1

Reference Standards Tracking Log Reference No.: R____________ Chemist: ___________ Date Received: _____________ Standard Description: ___________________________________________________________________ Catalog No.: _______________ Lot No.: ___________ Expiration Date: ____________ Company: _________________ Solvent: ___________ Concentration: _____________ Condition: _________________ Purity: ____________ Storage Location: ___________ Amount Received: __________

Solution Prepared

Amount Used

Amount Remaining

Initials and Date

Passed QC

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Figure 7.2

Standard Solutions Tracking Log Standard Solution No.: ________ Chemist: ___________ Date Prepared: _____________ Standard Solution Name: ________________________________________________________________ Storage Location: ____________ Solvent: ___________ Expiration Date: ____________ Solution Application: _________ Solvent Lot Number: _______ Final Volume: ______________

Reference Number

Name Initial Concentration

Amount Used

Final Concentration

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Section 8

SAMPLE MANAGEMENT

Sample Receipt

All samples received by Frontier Analytical Laboratory go through a sample receipt procedure ensuring the proper handling of samples, from their acceptance to eventual return. A unique project number is assigned to each sample and an in-house chain of custody is initiated. The analyst logging in the samples examines the shipping containers, their contents, and corresponding client information for problems. Information about the condition of the COC seals (if present) is noted as well as the state of preservation. Any discrepancies in documentation or other anomalies are noted and brought to the attention of the client, who may provide further instructions. The sample login SOP describes our procedures for sample acceptance and login.

Once the samples are properly logged in, they are stored in a manner which best ensures their

integrity and security. Each sample is stored according to method-specific requirements, either in a lockable freezer at -10oC to-20oC or a lockable refrigerator at 0-4oC. Each sample refrigerator or freezer is temperature monitored regularly (either manually or automatically).

Sample Preparation

Sample preparation is method and matrix specific. Environmental samples must be prepared within a specified period of time after sampling. Frontier Analytical Laboratory will comply with method specific hold times to the most practical extent possible. In the event samples are received near or beyond the hold time expiration date, the client will be notified and analysis will be continued at the client’s discretion. Sample preparation and cleanup procedures are detailed in the appropriate method and matrix specific SOPs.

Sample extracts are placed in appropriate storage for at least 30 days after analysis. After that

time, the extracts are placed in labeled boxes and stored for a period of one year prior to disposal. Written procedures describe routine storage and disposal procedures.

Sample Disposal, Return

Samples are stored at Frontier Analytical Laboratory for at least ninety days from their receipt date prior to disposal. DLM/CBC samples are stored for at least six months from the date the final report is submitted. If a client would like their samples returned or their sample storage times extended, they should contact us within ninety days from receipt of their sample to arrange this. Extended storage times may incur an additional storage fee. Returned samples are temperature preserved and packaged properly to insure safe shipment by a commercial carrier. Sample extracts are held for at least one year prior to disposal unless otherwise directed by the client.

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SAMPLE MANAGEMENT

Method Holding Times

Method Holding Time Pre-Spike to

Sampling

Holding Time Sampling to Extraction

Holding Time Extraction to Analysis

CARB Method 428 30 days (D/F & PCBs) 30 days 30 days EPA Method 23/23A 14 days (D/F) 30 days 45 days EPA Method TO-9 30 days (D/F) 7 days 40 days NCASI Method 551 NA 30 days 45 days

EPA Method 613 NA 7 days 45 days EPA Method 8280 NA 30 days 45 days EPA Method 8290 NA 30 days 45 days EPA Method 1613 NA 1 year 45 days

EPA DLM02.0/DLM02.2

NA *10 days 30 days

EPA CBC01.0/CBC01.2

NA *10 days 30 days

EPA Method 1668 NA 1 year 1 year

Sample Delivery

Aqueous – Certified, pre-cleaned one-liter narrow mouth amber glass bottle. Total of two liters desired. Preservative – Sodium Thiosulfate Solid – Certified, pre-cleaned wide mouth amber glass jar/bottle. No preservative necessary. Minimum of 20 grams dry weight equivalent desired. Sample bottle must be glass. Fish and other tissue samples – may be wrapped in aluminum foil. All sample matrices are to be sent between 0-40 Celsius, preferably using overnight delivery. Fish and other tissue samples may be sent frozen. Fish and other tissue samples are frozen once received by the laboratory. All other matrices are refrigerated between 0-40 Celsius once received by the laboratory. Most matrices extraction hold times can be extended up to one year if the sample is frozen (<-100 Celsius) upon arrival at the laboratory. *All DLM or CBC samples shall be extracted within 10 days of the Validated Time of Sample Receipt (VTSR).

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Section 9

INSTRUMENTATION

Traceability of Measurements

The quality of the analytical data depends upon the precision and accuracy of the equipment making the measurements. This includes the GC/MS, balances, pipets, syringes, etc. Any piece of equipment upon which the quantitative results are dependent should be checked for measurement capability against a traceable measurement standard. Frontier Analytical Laboratory uses NIST traceable standards whenever possible. Extensive documentation is kept on the maintenance and use of all instrumentation and equipment.

Verification of instrumentation and equipment performance is essential in order to provide the highest quality scientific data possible. Frontier Analytical Laboratory has implemented numerous procedures to ensure legally defensible and scientifically valid data.

Gas Chromatography/Mass Spectrometry (GC/MS)

Frontier Analytical Laboratory is equipped with two magnetic sector instruments. The Waters/Micromass Autospec M Series Ultima and the VG Analytical 70 S magnetic sector mass spectrometer provide routine picogram analysis. Both instruments are equipped with OpenVMS operating systems with OPUS Quan data handling software, HP5890 Series II gas chromatographs and CTC auto-samplers that provide twenty-four hour capabilities.

The gas chromatograph operating conditions are established to meet the requirements of each

analytical method. Conditions may include minimum retention times of internal standards, relative retention times of target analytes, and minimum absolute retention times of specific compounds. Verification of first and last eluters may be applicable. Other requirements may include the ability to peak resolve specific target analytes from other analytes. Once the operating conditions are established, the same conditions must be used for the analysis of all standards, blanks, QC samples, IPRs, OPRs, LCS, and samples.

The mass spectrometer is tuned and calibrated according to the specific method of analysis.

Perfluorokerosene (PFK) is introduced into the ion source and used to tune and calibrate the mass spectrometer. The instrument is tuned to meet the minimum required resolving power according to the analytical method being performed. Initially, the analyst does this visually. It is then confirmed, recorded and printed by the data system. Next, mass calibration of the instrument is performed by the data system. Mass calibration is continuously adjusted by the data system, at a rate of approximately once per second throughout the analysis.

Initial calibration is performed for each analytical method. The initial calibration consists of

five to seven calibration solutions. Each solution contains the target analytes along with the corresponding labeled analytes at method specified concentrations. New initial calibrations are performed whenever a new set of spiking calibration standards is made, or if six months has passed since the last initial calibration was run, or if the continuing calibration consistently falls outside the

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specified acceptance criteria. The method specific criteria must be met prior to the analysis of any samples. Failure to meet the corresponding criteria will require corrective action prior to sample analysis.

Continuing calibration is performed at the beginning of each twelve-hour window. The

continuing calibration is a mid-range standard from the initial calibration standards that may also contain window defining analytes and peak resolution analytes. The method-specific criteria must be met prior to the analysis of any samples. Failure to meet the corresponding criteria will result in corrective action prior to sample analysis.

Qualified on-site personnel will perform routine preventative and non-routine instrument

maintenance. In the event on-site personnel cannot perform the maintenance, Frontier Analytical Laboratory will utilize an authorized service dealer. Routine and non-routine service is recorded in corresponding maintenance logbooks. These logbooks define routine and non-routine maintenance. Each logbook is instrument-specific and is maintained by the analyst. Quality spare parts are kept on-site in order to prevent instrument down time.

General Laboratory Equipment

Balances are checked and calibrated, if necessary, prior to use. The check consists of three weights that encompass the range of weight to be measured. The calibration weights used are NIST certified class S weights, which are certified annually. Each balance is professionally serviced and calibrated annually. Each balance has its own maintenance and calibration logbook that also contains the acceptance criteria. In addition, each balance has its own general maintenance and calibration SOP.

Laboratory Thermometers are checked for accuracy against NIST certified thermometers that

are calibrated professionally and recertified periodically. All laboratory mercury or alcohol-in-glass thermometers are checked annually, and metal thermometers are checked quarterly. Other types of thermometers (e.g., electronic) are calibrated on an as-used basis. In addition, sample-receiving thermometer accuracy is routinely verified using a second source. Correction factors are applied when necessary. Maintenance and calibration procedures are described in the laboratory thermometer SOP.

Other equipment, such as pipets, syringes, volumetric glassware, etc. is checked for accuracy

against manufacturer’s specifications and rejected if it falls outside of acceptable criteria.

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Section 10

DATA MANAGEMENT

Data Production

Analytical data shall be retained for a minimum of five years. Analytical data is acquired both manually and electronically. Raw data is the principal source of information used to generate the final report. The raw data will have unique identifiers that distinguish each sample and batch of samples. In addition, the data will contain pertinent information that enables verification of the authenticity of the results. This may include but not be limited to Laboratory ID, analytical method, instrument ID, sample preparation protocol, etc.

Manual data is an observation that is recorded, in permanent ink, by an analyst. The

observations can be recorded on such documentation as logbooks, data sheets, chain-of-custody documents, as well as other types of standard documentation that require an analyst’s observation. The reason for each observation is clearly stated. Each entry is dated and signed or initialed by the analyst and must be logged at the time of the observation.

Electronic data may consist of chromatograms, data printouts, temperature logs, and raw quantitation reports. It must include the date of acquisition, and the analyst’s name or initials. The electronic data shall have hard copy or write-protected backup copies. In addition, the electronic data has a uniform naming scheme so that each piece of the electronic data can easily be retrieved.

Manual and/or electronic entries shall not be obliterated by methods such as erasures or

markings. Corrections to record-keeping errors shall be made by one line marked through the error and the individual making the correction shall date and sign or initial the correction.

Method evaluation and data validation are essential for successful data management. Frontier

Analytical Laboratory routinely analyzes an array of quality control samples including method blanks, ongoing precision and recovery samples, laboratory control samples, matrix spike and matrix spike duplicates, duplicate samples, initial precision and recovery samples, resin and filter QC samples, and method detection limit study samples. The frequency and purpose of all quality control samples are reviewed and discussed in the Quality Control portion of Section 11, Quality Systems.

Accepted analytical methods guide the data review and reduction process. Data review is a

three-tiered system that is originated by the instrument analyst. Once the instrument analyst has reviewed the data, a second thorough peer review is completed before a final report is prepared. Once the final report has been prepared, a thorough review of the entire report is performed. In addition, the Quality Assurance Officer reviews approximately ten percent of the final reports. This multi-tiered review process ensures data of the highest quality and integrity. Instrument data acquisition and reduction is performed via DEC PWS 500AU Alpha Work Stations. The instrument data and other pertinent data used for the final report are acquired and reduced via PC based software. This allows for a complete and thorough final report that is easily read and understood.

Analytical data and records are safely archived and retrievable for a minimum of five years.

Retrieval of such information is documented in the archive access log (Figure 10.1) and is restricted

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to a few authorized personnel. All data that has been deemed appropriate for disposal will be shredded. In the event that Frontier Analytical Laboratory (FAL) transfers ownership of the business, the owners of FAL shall make arrangements for continued archive and retrieval of all data for up to five years by the new owners. In the unlikely event that FAL goes out of business, the owners shall arrange to transfer data directly to the client if desired.

In the event additions or corrections to the final report are required, authorized personnel

must first verify and substantiate the addition or correction. The authorized personnel must then sign and retrieve the report from the archive area. The addition or correction is then made and sent to the customer as soon as possible. The addition or correction is clearly noted in the final report and the entire report is returned to the archive area.

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Figure 10.1

Archive Access Log

This log monitors and restricts the access to completed final reports. Only authorized personnel are allowed access to the completed final reports and must sign out and sign in each report. Authorized personnel are listed below. Authorized Personnel:

Name Title Signature Dan Vickers Director of Technical Services

Quality Assurance Officer Safety Officer

Brad Silverbush Director of Operations Tom Crabtree Director of Mass Spectrometry Kathy Zipp Accountant/Office Administration Maria Gabriella Navarro Extraction Chemist

Authorized Personnel

Frontier Project Number

Check-out Time and Date

Check-in Time and Date

Signature

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Section 11

QUALITY SYSTEMS

Frontier Analytical Laboratory’s Quality Assurance program provides a system of activities ensuring that quality control takes place at each step of production. This program includes the administration, management and evaluation of all SOP documents, internal and external facility audits, corrective action reports, quality control procedures, statistical analysis and charting of quality indicators.

Quality Assurance:

SOPs: Frontier Analytical Laboratory provides various types of SOPs describing procedures performed throughout the laboratory. General laboratory procedures (LPs) document procedures such as XAD cartridge preparation, glassware cleaning, balance calibration, etc. Method specific extraction procedures (EPs) and instrumentation procedures (IPs) document standard operating procedures for the methodologies performed at Frontier Analytical Laboratory. Safety procedures (SPs) document safety awareness and safety policies, safety equipment inspection and maintenance and hazardous waste handling and disposal procedures. The SOPs are maintained and followed by Frontier Analytical Laboratory staff. Updates and modifications are made when necessary. This may include but is not limited to new methodology, new instrumentation, etc. The revision number and effective date is documented and an archive of the outdated SOP is maintained. The SOPs are clearly written and provide adequate detail to perform the procedure. SOPs are located in the area where the equipment and procedures are utilized. This provides a reference for staff and ensures proper utilization.

Quality records: Frontier Analytical Laboratory maintains quality records that verify control

procedures and ensure traceability. Quality records are maintained and archived by Frontier Analytical Laboratory. These include sample receipt records, sample preparation records, sample and QC sample analysis data, logbooks (run-logs, temperature logs, balance calibration logs, etc.), certificates of analysis and other records for standards, reagents, and other media, method validation records (MDL, IPR, etc.), quality indicator data (QC charts), system audit reports, corrective action reports, and QA reports. Logbooks are located in the area where the equipment and procedures are utilized. This enables entries to be made at the time of observation and ensures that logbooks are properly utilized.

Audits and inspections: System audits can be either internally or externally initiated. The QA

department performs internal audits on an annual basis. Clients and agencies can initiate and perform external audits as per their requirements. The purpose of these audits (either internal or external) is to verify that operations continue to comply with the requirements of the laboratory’s quality systems and policies. In the event of non-compliance, the qualifying event is noted, management is notified and corrective action is initiated, if necessary. Corrective actions should be completed as soon as possible. All findings from QA audits are subject to management review.

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Performance audits: A Performance Evaluation (PE) Sample is analyzed and reported by the laboratory and can be internally or externally driven. The concentration is not known by the analyst or laboratory but is known by the Performance Evaluation Sample source. The purpose of performance audits is to monitor the quality of the laboratory’s analytical activities. Performance Evaluation Samples are used for accreditation, round-robin studies, analyst proficiency testing, as well as evaluating laboratory system modifications. PE sample testing is performed twice yearly for each matrix and Method as required for accreditation.

Data audits: Data audits are careful evaluations of randomly selected data reports. The

Quality Assurance Officer performs an exhaustive and thorough review of the entire report. Both technical and clerical accuracy is verified. Data audits are conducted to identify areas for improvement to determine if the report satisfies the needs of the customer. Approximately ten percent of all finalized reports undergo data audits.

Management Review: The entire Quality System, including this document and all SOPs shall

be annually reviewed by management and updated in conjunction with the laboratory’s annual internal audit. Management review of this document shall take into account outcomes from internal audits, assessments by external authorities, interlaboratory studies, performance evaluation tests, SOPs, method manuals, laboratory polices, training records, changes in volume of or type of work, feedback from clients and corrective actions.

Quality Control: The analytical data produced for Frontier Analytical Laboratory clients must meet defined quality standards. These defined quality standards include accuracy, precision, completeness, and comparability. Numerous quality control procedures are implemented at each stage of production throughout the laboratory. The purpose of these procedures is to guarantee consistent and verifiable analytical results. In the event defined quality standards are not met, corrective actions are initiated.

Quality Control Samples and Spikes:

Cleanup Surrogate Standard (CSS) A known amount of isotopic labeled standard that is added to every sample and is present at the same concentration in every blank, quality control sample, and concentration calibration solution. It is added after extraction and prior to cleanup. The cleanup surrogate standard recovery serves as an indicator of the performance of the cleanup procedure. In certain air sampling procedures, impinger waters are required to be extracted separately. If this is required, the cleanup surrogate standard is added to the impinger water prior to extraction. In this particular case, the cleanup surrogate standard recovery serves as an indicator of the overall performance of the impinger extraction.

Duplicate Samples (DUP) Duplicate samples are analyzed to demonstrate laboratory precision. Duplicate samples are two separate aliquots taken from the same sample source. Duplicate samples are prepared and analyzed using the same procedures as the rest of the analytical batch.

Initial Precision and Recovery (IPR) IPRs are analyzed to demonstrate acceptable precision and recovery. A known quantity of native standard is added to four reference matrix method blanks. The IPRs are then prepared

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and analyzed following the laboratory procedure for processing samples. IPRs are performed annually or prior to the first time a method is used and any time a method, personnel or instrumentation is significantly modified or changed.

Internal Standard (IS) A known amount of isotopic labeled standard that is added to every sample and is present at the same concentration in every blank, quality control sample, and concentration calibration solution. It is added prior to extraction and is used to measure the concentration of the target analytes and the surrogate pre-sampling standard. The internal standard recovery serves as an indicator of the overall performance of the analysis.

Matrix Spikes (MS/MSD) Duplicate matrix spike samples are analyzed to demonstrate method precision and accuracy on a particular sample matrix. A known quantity of native standard is added to duplicate samples. These MS/MSD samples are then prepared and analyzed using the same procedures as the rest of the analytical batch. MS/MSD samples are performed per client request.

Method Blanks (MB) Reference matrix method blanks are analyzed to demonstrate freedom from laboratory contamination. The method blank is prepared and analyzed using the same procedures as the rest of the analytical batch. A method blank is run with each sample batch, not to exceed 20 samples total in a given 12-hour period.

Method Detection Limits (MDL) MDLs are performed to determine the minimum concentration of an analyte that can be measured and reported with 99% confidence. A known quantity of native standard is added to seven reference matrix method blanks. These spiked matrix method blanks are then prepared and analyzed following the laboratory procedure for processing samples. MDLs are performed annually or prior to the first time a method is used and any time a method or instrumentation is significantly modified.

Native Standard (NS) A known amount of unlabeled standard that is added to reference method blanks and samples in association with OPRs, LCSs, MDLs, IPR, and MS/MSDs. It is also used in conjunction with isotopic labeled standards to calculate native response factors, verify the linearity and performance of the instrumentation, and to assess the accuracy of the analytical method.

Ongoing Precision and Recovery/Laboratory Control Spikes (OPR/LCS) An OPR/LCS is analyzed to demonstrate method precision and accuracy. A known quantity of native standard is added to a reference matrix method blank. This OPR/LCS is then prepared and analyzed using the same procedures as the rest of the analytical batch. All results are reported in ng/mL of final extract. An OPR/LCS is run with each sample batch, not to exceed 20 samples total in a given 12-hour period.

Percent Recovery Percent recovery is the calculated recovery of any known amount of labeled or unlabeled analyte. If known background levels exist, they must be accounted for. Percent recovery is a quantitative measure of the accuracy of an analytical process.

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Performance Evaluation Samples (PE) PE samples are analyzed to demonstrate laboratory accuracy. PE samples are prepared and analyzed following the laboratory procedure for processing samples. PE samples usually contain a known concentration of target analytes. Multiple laboratories analyze PE samples in order to determine statistically the accuracy and precision that can be expected when a competent analyst performs a method. Analyte concentrations are unknown to the analyst.

Pre-Sampling Standard (PSS) A known amount of isotopic labeled standard that is added to every air sample and is present at the same concentration in every blank, quality control sample, and concentration calibration solution. It is added during sampling media preparation and prior to sampling. The pre-sampling standard recovery serves as an indicator of the performance of the sampling event.

Recovery Standard (RS) A known amount of isotopic labeled standard that is added to the final extract prior to analysis. The response of the internal standards relative to the recovery standards is used to calculate the percent recovery of the internal standards.

Relative Percent Deviation (RPD) The relative percent difference is a comparison of target analytes from LCS or MS/MSD pair recoveries. The RPD is calculated as the difference in percent recoveries of the target analyte, divided by the average percent recovery of the target analyte, times 100%.

Quality Control Acceptance Criteria

The acceptance criteria for analytical data are method specific. Refer to each IP for the specific requirements.

Corrective Action

Corrective Action is initiated when QC limits are exceeded, as specified in the particular method. This may include re-injection of the extract, or re-extraction of the sample or sample set.

Corrective Action Reports (CAR)

Corrective action reports are initiated when major non-routine irregularities arise, or as a result of customer complaint. The purpose of a CAR is to determine the cause of a problem, to monitor the progress of any corrective action activities, and to implement measures to prevent the problem from re-occurring in the future. For example, if persistent method blank contamination occurs, corrective action is implemented to determine the source of the contamination. In this particular case, the analyst would initiate decontamination procedures. The initiation, progress and outcome of any corrective action are documented on the corrective action report form (Figure 11.1).

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A corrective action report can be initiated by anyone who detects a significant quality problem and is monitored by the QA department.

Quality Assessment Quality assessment is a means to determine whether the laboratory’s ongoing quality systems are functioning properly. Assessments include but are not limited to: peer reviews, system audits, performance evaluations, data quality audits, statistical tracking of analytical quality indicators (QC charts) and subsequent management review. The assessment procedures and their implementation are outlined throughout the Quality Manual.

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Figure 11.1

Summarized by: __________________

QA Department Approval: __________

Management review: ______________

Corrective Action Performed by: __________

Problem Reported by: _________________

Corrective Action Report

FAL Report ID: _______________ Samples Affected: _________________ Method Requested: __________________

Date Received: _______________ Date Extracted: __________________ Date Analyzed: ____________________

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Problem Description

Date Problem Detected: ______________

__

/2

ra

Corrective Action

_____ Date of Corrective Action: ______________

Corrective Action Summary

_____ Date Summarized: _____________

_____ Date Approved: _______________

_____ Date Approved: _______________

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Appendix 1

Laboratory Procedure Table of Contents

QA 1A Quality Assurance Manual QA 2A Ethics / Data Integrity Program QA 2B Organizational Conflict of Interest Plan

Section 1

LP 1A Sample Login Procedure LP 1B Document Development and Change Procedure

LP 1C Report Review and Packaging Procedure LP 1D Project Management LP 1E Laboratory Information Management System (LIMS)

Section 2

LP 2A Receipt and Preparation of Analytical Standards LP 2B Internal Laboratory System Audit Procedure/Management

Review LP 2C Corrective Action Report Procedure LP 2D Data Recording Procedure LP 2E Proficiency Test Sample Preparation and Reporting

Section 3

LP 3A Glassware Washing, Solvent Rinsing and Kilning Procedure

Section 4

LP 4A Sample Control Thermometer Calibration Procedure LP 4B Refrigerator/Freezer Thermometer Calibration Procedure

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LP 4C Toploader Balance Calibration/Operation Procedure LP 4D Analytical Balance Calibration/Operation Procedure LP 4E Refrigerator/Freezer Monitoring Procedure

Section 5

LP 5A Filter Cleaning and Contamination Check Procedure LP 5B XAD-2 Cleaning and Contamination Check Procedure

LP 5C PUF Cartridge Preparation Procedure

LP 5D MM-5 Air Cartridge Preparation Procedure

Section 6

ML 3 Master List of Laboratory Procedures/Current Revisions

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Appendix 1

Extraction Procedure Table of Contents

Section 1

EP 1A Extraction and Cleanup Procedure for Polychlorinated Biphenyls

(PCBs) by Modified EPA Method 1668 EP 1B Extraction and Cleanup Procedure for Coplanar Polychlorinated

Biphenyls by Modified EPA Method 1668 EP 1C Extraction and Cleanup Procedure for Mono through Deca

Polychlorinated Biphenyls by Modified EPA Method 1668 in an MM5 Air Train

EP 1D Extraction and Cleanup Procedure for Coplanar Polychlorinated Biphenyls by Modified EPA Method 1668 in an MM5 Air Train

EP 1E Extraction and Cleanup Procedure for Coplanar Polychlorinated Biphenyls by Modified EPA Method 1668 in an Ambient Air Sample

EP 1F Extraction and Cleanup Procedure for Coplanar Polychlorinated Biphenyls by Modified EPA Method CBC01.0

EP 1G Extraction and Cleanup Procedure for Coplanar Polychlorinated Biphenyls by Modified EPA Method CBC01.1

Section 2

EP 2A Extraction and Cleanup Procedures for Polychlorinated Dibenzo-

p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method 1613

EP 2B Extraction and Cleanups Procedure for Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method 8290

EP 2C Extraction and Cleanup Procedure for Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method DLM02.0

EP 2D Extraction and Cleanup Procedure for Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method DLM02.1

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Section 3

EP 3A Extraction and Cleanup Procedure for Polychlorinated Dibenzo-

p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method 8280

Section 4

EP 4A Extraction and Cleanup Procedure for Polychlorinated Dibenzo-

p-Dioxins and Polychlorinated Dibenzofurans by Modified CARB Method 428

EP 4B Extraction and Cleanup Procedure for Polychlorinated Biphenyls by Modified CARB Method 428

EP 4C Extraction and Cleanup procedure for Polychlorinated Dibenzo-p-Dioxins/Dibenzofurans and Polychlorinated Biphenyls by Modified CARB Method 428

Section 5

EP 5A Extraction and Cleanup Procedure for Polychlorinated Dibenzo-

p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method 23

EP 5B Extraction and Cleanup Procedure for Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method 23A

Section 6

EP 6A Extraction and Cleanup Procedure for Polychlorinated Dibenzo-

p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method TO-9

EP 6B Extraction and Cleanup Procedure for Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method 23A and Polyaromatic Hydrocarbons by Modified EPA Method TO-13 in a MM5 train

EP 6C Extraction and Cleanup Procedure for Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method TO-9 and Polycyclic Aromatic Hydrocarbons by Modified EPA Method TO-13

EP 6D Extraction and Cleanups for Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans by Modified EPA Method 23A and Semi Volatile Organic Compounds by Modified EPA Method 8270 in a MM5 Train

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EP 6E Extraction and Cleanup Procedure for Polychlorinated Dibenzo-p-Dioxins and Dibenzofurans by Modified EPA Method TO-9A and Pesticides by Modified EPA Method TO-4A

EP 6F Extraction and Cleanup Procedure for Mono through Deca Polychlorinated Biphenyls by Modified EPA Method 1668 in an Ambient Air Sample

Section 7

EP 7A Extraction and Cleanup Procedure for Polycyclic Aromatic

Hydrocarbons by Modified EPA Method 429 EP 7B Extraction and Cleanup Procedure for Polycyclic Aromatic

Hydrocarbons by FAL Method 15

Section 8

EP 8A Extraction and Cleanup Procedure for Polycyclic Aromatic

Hydrocarbons by Modified EPA Method TO-13

EP Master List

ML 1 Master List of Extraction Procedures/current revisions

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Appendix 1

Instrument Procedure Table of Contents

Section 1

IP 1A GC/MS Analysis for Polychlorinated Biphenyls by Modified EPA

Method 1668 IP 1B GC/MS Analysis for Coplanar Polychlorinated Biphenyls by

Modified EPA Method 1668 IP 1C GC/MS Analysis for Mono through Deca Polychlorinated

Biphenyls by Modified EPA Method 1668 in an MM5 Air Train IP 1D GC/MS Analysis for Coplanar Polychlorinated Biphenyls by

Modified EPA Method CBC01.0 IP 1E GC/MS Analysis for Coplanar Polychlorinated Biphenyls by

Modified EPA Method 1668 in a PUF Sample or a MM5 Sample IP 1F GC/MS Analysis for total Mono through Deca Polychlorinated

Biphenyls by Modified EPA Method 1668 IP 1G GC/MS Analysis for Coplanar Polychlorinated Biphenyls by

Modified EPA Method CBC01.1

Section 2

IP 2A GC/MS Analysis for Polychlorinated Dibenzo-p-Dioxins and

Dibenzofurans by Modified EPA Method 1613 IP 2B GC/MS Analysis for Polychlorinated Dibenzo-p-Dioxins and

Dibenzofurans by Modified EPA Method 8290 IP 2C GC/MS Analysis for Polychlorinated Dibenzo-p-Dioxins and

Dibenzofurans by Modified EPA Method DLM02.0 IP 2D GC/MS Analysis for Polychlorinated Dibenzo-p-Dioxins and

Dibenzofurans by Modified EPA Method DLM02.1

Section 3

IP 3A GC/MS Analysis for Polychlorinated Dibenzo-p-Dioxins and

Dibenzofurans by Modified EPA Method 8280

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Section 4

IP 4A GC/MS Analysis for Polychlorinated Dibenzo-p-Dioxins and

Dibenzofurans by Modified CARB Method 428 IP 4B GC/MS Analysis for Polychlorinated Biphenyls by Modified

CARB Method 428

Section 5

IP 5A GC/MS Analysis for Polychlorinated Dibenzo-p-Dioxins and

Dibenzofurans by Modified EPA Method 23 IP 5B GC/MS Analysis for Polychlorinated Dibenzo-p-Dioxins and

Dibenzofurans by Modified EPA Method 23A

Section 6

IP 6A GC/MS Analysis for Polychlorinated Dibenzo-p-Dioxins and

Dibenzofurans by Modified EPA Method TO-9

Section 7

IP 7A GC/MS Analysis for Polycyclic Aromatic Hydrocarbons by

Modified EPA Method 429

Section 8

IP 8A GC/MS Analysis for Polycyclic Aromatic Hydrocarbons by

Modified EPA Method TO-13

Section 9

IP 9B GC/MS Analysis for Polycyclic Aromatic Hydrocarbons by FAL

Method 15

IP Master List

ML 2 Master List of Instrument Procedures/current revisions

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Appendix 1

Safety Procedure Table of Contents

Section 1

SP 1A Safety Awareness and Safety Policies

SP 1B Safety Equipment and Inspection Procedure SP 1C Hazardous Waste Handling and Disposal Procedures SP 1D Spill Prevention Control and Countermeasure Plan

Section 2

Monthly Safety Equipment Inspection Log Annual Safety Equipment Inspection Log Monthly Hazardous Waste Area Inspection Log Safety Training records

Section 3

ML 4 Master List of Safety Procedures/Forms/current revisions

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