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70-92 Boston Street & 61 Ward Street Brownfields Quality Assurance Project - Attachment B - April 2004 ATTACHMENT B LABORATORY QUALITY ASSURANCE MANUAL L2004-123 I s QUALITY ASSURANCE PLAN -Date Revised: 1109103 Revision 4 COKtOL HUMBER UNCONTROL T D Approved By: lowmEN �QA/QC Director Date Lab iredor Date MITKEM Corporation 175 Metro Center Boulevard,Warwick,RI 02886 Phone Number: (401) 732-3400,Fax Number: (401) 732-3499 QA Plan Section No.2 tev_4 Date Initiated:OU151% Date revised:U"103 Page 1 of 6 2.0 Table of Contents Section Page 1 Title Page 1.1 2 Table of Contents 2.1 3 Introduction 3.1 4 Quality Assurance Policy Statement 4.1 5 Quality Assurance Management Organization and Responsibility 5.1 6 Quality Assurance Objectives for 6.1 Measurement Data in Terms of Precision, Accuracy,Representativeness,Completeness and Comparability 6.1 Precision and Accuracy 6.1 6.2 Representativeness 6.2 6.3 Completeness 6.2 6.4 Comparability 6.2 7 Sampling Procedures 7.1 8 Sample Custody 8.1 8.1 Chain of Custody 8.1 8.2 Laboratory Security 8.1 8.3 Duties and Responsibilities of Sample Custodian 8.2 I QA Plan Section No.2 rev.4 Dabs Initiated:01/15/94 NatorcWv&1/07/03 E 2.0 Table of Contents(Cont'd) Page 2 of 6 Section Page 8.4 Sample Receipt 8.3 8.5 Sample Log-in and Identification 8.4 8.6 Sample Storage and Disposal 8.6 8.7 Sample Tracking 8.7 9 Calibration Procedures and Frequency 9.1 9.1 Instruments 9.1 9.2 Standards and Reagents 9.4 10 Analytical Procedures 10.1 E 10.1 Analytical References 10.11 '11 Data Reduction, Validation and Reporting 11.1 11.1 Data Reduction 11.1 11.2 Data Validation 11.1 11.3 Data Verification 11.1 11.4 Data Interpretation and Reporting 11.2 11.4.1 Report Formats 11.2 11.4.2 Data Reporting for Massachusetts Drinking Water Samples 11.2 11.5 Levels of Review 113 11.5.1 Level 1 11.3 11.5.2 Level 2 11.3 11.5.3 Level 3 11.5 QA Plan Section Na 2 rev.4 Date Initiated 01/15/94 Date revised 1/07/d3 Page 3 of 6 2.0 Table of Contents(Cont'd) Section Page 11.5.4 Level 4 11.6 11.5.5 Level 5 11.6 11.6 Document Control 11.7 11.6.1 Logbooks 11.7 11.6.2 Project/Data Files 11.7 11.6.3 Standard Operating Procedures(SOPs) 11.7 11.6.4 Method Updates 11.8 12 Laboratory Quality Control Checks 12.1 12.1 Detection Limit Determination/Verification 12.1 12.2 Personnel Training 12.1 12.3 Control Charts 12.1 12.4 General QC Protocols 12.3 13 Quality Assurance Systems Audits, Performance Audits and Frequencies 13.1 13.1 Systems Audits 13.1 13.2 Performance Audits 13.1 14 Preventive Maintenance 14.1 15 Specific Routine Procedures Used to Assess Data Precision,Accuracy,Completeness,Methods Detection Limits and Linear Dynamic Range 15.1 15.1 Precision 15.1 QA Man Seddon No.2 mv.4 Date tniCmkd-MOM Date revised:1/07M Page 4 of 6 2.0 Table of Contents(Cont'd) Section Page 15.2 Accuracy 15.2 15.3 Completeness 15.3 15.4 Method Detection Limit 15.3 15.5 Linear Dynamic Range 15.4 16 Corrective Action 16.1 17 Quality Assurance Reports to Management 17.1 18 Safety 18.1 Tables Table 7-1 Recommended Containers,Preservation Techniques and 7.2 Holding Times for SW846 Analyses Table 7-2 Recommended Containers,Preservation Techniques and 7.4 Holding Times for CLP/ASP Analyses Table 7-3 Recommended Containers,Preservation Techniques and 7.6 Holding Times for Other Analyses Table 10-1 Potable Water Analytical Methods 10.2 Table 10-2 Non-potable Water Priority Pollutant Analytical Methods 10.3 Table 10-3 SW-846 Inorganic Analytical Methods 10.5 Table 10-4 SW-846 Organic Analytical Methods 10.7 Table 10-5 CLP-Type Analytical Methods 10.9 Table 10-6 Other Analytical Methods 10.10 Figures Figure 5-1 MITKEM Corporation's Organization Chart 5.3 QA Plan Section No.2 rev.4 Date faitiate&01/15/94 Date revised:1107103 Page 5 of 6 2.0 Table of Contents(Cont'd) Figures Page Figure 8.4-1 Sample Receipt Tracking Logbook Form 8.9 Figure 8.4-2 USEPA CLP Sample Login Form 8.10 Figure 8.4-3 Sample Condition Form 8.11 Figure 8.4-4 Sample Condition Notification Form 8.12 Figure 8.4-5 MITKEM Chain-of-custody Form 8.13 Figure 8.5-1 Project Information Form 8.14 Figure 8.6-1 Volatile Organic Tracking Logbook Form 8.15 Figure 8.6-2 Temperature Log Form 8.16 Figure 8.6-3 Extracts Transfer Log Form—Semivolatile Analysis 8.17 Figure 9.6-4 Extracts Transfer Log Form—Pesticide/PCB Analysis 8.18 Figure 9.2-1 Metals Primary Standard Receipt Logbook Form- 9.5 Instrument Laboratory Figure 9.2-2 Semivolatile Primary Standard Receipt Logbook Form- 9.6 Instrument Laboratory Figure 9.2-3 Pesticide/PCB Working Standard Receipt Logbook Form- 9.7 Instrument Laboratory Figure 9.24 Reagent Preparation Logbook Form Preparation Laboratory 9.8 Figure 11.5-1 Data Review Checklist 11.9 Figure 11.5-2 CLP and CLP-type Data Review Checklist-Organics 11.10 Figure 11.5-3 CLP and CLP-type Data Review Checklist—Inorganics 11.11 i Figure 11.54 Data Review Flow Diagram 11.12 I 1 QA Plan Sxtium No.2 mv.4 Date JnWatad:01115M Date revised:1/07103 Page 6 of 6 Table of Contents(Cont'd) Figures page Figure 12.3-1 Example Control Chart 12.5 Figure 13.1-1 QA Systems Audit Checklist 13.2 Figure 14-1 Example Instrument Maintenance Logbook Form 14.4 Figure 14-2 Instrument Maintenance Schedule 14.5 Figure 16-1 QA Corrective Action Request Form 16.3 Figure 17-1 Quality Assurance Report to Management Format 17.1 Appendices Appendix A Major Instrumentation Listing Appendix B Confidentiality;Ethics and Data Integrity Agreement Qk Pion SectionNo.3 rev.4 Date liddated:1/151'94 Date Revised:IM6103 Pagel of 1 3.0 INTRODUC.""TION M=M Corporation is an 8(a)minority-owned environmental services company, incorporated in the State of Rhode Island. Offices and laboratories are located in Warwick,Rhode Island. The laboratory occupies Approximately 11,000 square feet of laboratory space. This Quality Assurance Plan(QAP)describes the policies,organization,objectives, quality control activities and specific quality assurance functions employed at MITKEK and demonstrates MITKEM's dedication to the production of accurate,consistent data of known quality. This QAP is developed by following the guidelines discussed in the EPA Requirements for Quality Assurance Project Plans for Environmental Data Operations, EPA QA/R-5,Interim Final,Jan., 1994. In the event the Laboratory transfers ownership all records will be transferred to the new owner/owners and all clients will be notified.The new ownership will be responsible for the records and will carry out all client instructions for the maintenance of the records.In the event the Laboratory goes out of business,an outside party will be designated to maintain the records and complete all instructions pertaining to the records per all client instructions. 1 i QA Plan Section No.4 rev.4 Date Wdatei 1/15/94 Date Revised 1/08/03 Page 1 of 2 4.0 QUALITY ASSURANCE POLICY STATEMENT MITKEM is firmly committed to the production of valid data of known quality through the use of analytical measurements that are accurate,reproducible and complete. To ensure the production of such data,MITKEM has developed a comprehensive Quality Assurance/Quality Control Program that operates throughout the entire organization MITKEM Management considers Quality Assurance/Quality Control to be of the highest importance in the success of its Analytical Testing Laboratory and therefore fully supports the staff in the implementation and maintenance of a sound and thorough Quality Assurance Program. MITKEM's corporate success is based on its participation in the most rigorous and quality-focussed environmental testing programs,such as the EPA Contract Laboratory Program,US Department of Defense programs and nationwide and state-specific certification and approval programs. These programs require consistent application of the QA/QC procedures described in this document. MITKEM's ability to demonstrate and document that analyses were performed in this manner is one of the foundations of its business. The other foundation of its business is to provide superior levels of customer service,above and beyond the norm for laboratories performing at this level of quality. MITKEM's approach to customer service is to aggressively meet or exceed customer expectations,particularly in terms of turnaround time for results. While the production of rapid turnaround time data may require MITKEM employees to"go the extra mile"for the customer,without quality,the data are useless. MITKEM constantly manages its business to rapidly provide data meeting all the requirements.of its quality program. MITKEM management works to insure: • that employees understand the primary importance of quality in its day to day operations, • that employees will not be subjected to pressure to sacrifice quality for turnaround, financial or other considerations, • that employees understand the importance of their ethical responsibilities in terms of data manipulation,falsification or other illegal or improper actions, • that employees maintain all client information in a confidential manner,and • that employees understand that any short-term gain realized by disregarding the QA/QC program will be more than wasted by the serious penalties for these actions. All employees receive training in these issues as part of the initial orientation process, and are required to acknowledge that they understand their responsibilities in these areas. These issues are also discussed among all laboratory staff at frequent company meetings and re-training sessions. The QA Officer,Technical Director and other senior company management are readily available to all staff through their daily presence, "open door" QA Plan . Samson No.4 rev.4 Date IdMited:1/1S 4 Date RcviR d:l/OM Page 2 of policy and approachable manner. This allows any employee to readily discuss any questions,concerns or issues that may occur. Quality Control is defined as an organized system of activities whose purpose is to demonstrate that quality data are being produced through documentation_ Quality Assurance is more broadly defined as a system of activities designed to ensure that the quality control program is actually effective in producing data of the desired quality. Quality Control is included as part of Quality Assurance. In supporting government regulatory and enforcement proceedings, a high degree of attention to quality is essential. Thorough application of quality control principles and routine quality assurance audits is required. The basic components of the MITKEM QA/QC Program are control,evaluation and correction. Control ensures the proper functioning of analytical systems through the implementation of an orderly and well-planned series of positive measures taken prior to and during the course of analysis including quality control practices,routine maintenance and calibration of instruments,and frequent validation of standards. Evaluation involves the assessment of data generated during the control process. For example,precision and accuracy are determined from the results of duplicates and spikes, and other check samples. Long-term evaluation measures include performance and systems audit conducted by regulatory agencies,as well as the MI TKEM quality assurance group. Correction includes the investigation,diagnosis and resolution of any problems detected in an analytical system. Proper functioning of the system may be restored through method re-evaluation,analysis of additional check samples,trouble-shooting and repair of instrumentation or examination and comparison with historical data. Corrective actions are documented and reviewed to make sure they are implemented. Certain situations may occur when there are occasional departures or exceptions from documented policies and procedures or standard specifications due to client or project specific protocols,unusual sample matrix,or special non-target analyte or non-routine analyses. MITKEM's policy is to fully document all such procedures and their associated QC,and notify the client or regulatory agency. If the situation is to continue,a Standard Operating Procedure will be written and implemented. QA Plan Section No.5 rev.4 Date Initiated.1/15M Date Revised:VOM3 Page i of 6 5.0 QUALITY ASSURANCE MANAGEMENT,ORGANIZATION AND RESPONSIBILITY Quality Assurance at MITKEM is a company:wide function that depend on: (1) cooperative working relationships at all levels within the laboratory and (2) multi-level review through all working levels of responsibility. Responsibilities for QA/QC functions begin with the bench scientist and extend to the chief executive officer. The primary level of quality assurance resides with the bench scientist. After completion of the documented training program,his/her responsibilities include: • complying with all aspects of formally approved analytical methods and SOPS, • carefully documenting each step of the analytical process, • conscientiously obtaining peer review as required, • promptly alerting laboratory supervisors and/or QA staff members to problems or anomalies that may adversely impact data quality,and • participation in corrective actions as directed by the laboratory supervisor or QA Director. The supervisor of each laboratory is responsible for ensuring thorough oversight of the quality of the data generated by the bench scientists. The laboratory supervisor implements and monitors the specific QC protocols and QA programs with the laboratory to ensure a continuous flow of data meeting all control protocols and Mitkem QA requirements. The laboratory supervisor's responsibilities include providing the bench chemist with adequate resources to achieve the desired quality of performance. The MIT'KEM organizational structure is shown in the Organization Chart. Resumes of the CEO/Technical Director,Vice President,Quality Assurance Director, Operations Manager,Organic and Inorganic Managers,Chief Financial Officer,Marketing Director, Account Director,Project Managers,supervisors for the Inorganic Laboratory,GC Laboratory,Semi-volatile Organic Laboratory,Volatile Organic Laboratory and Sample Preparation Laboratory are included. Implementation of the entire Quality Assurance Program is the responsibility of the QA Director. While interacting on a daily basis with laboratory staff members,the QA Director remains independent of the laboratories and reports directly to the Chief Executive Officer. The QA Director evaluates laboratory compliance with respect to the QA program through informal and formal systems and performance audits as described in Section 13.0. Remedial action,to alleviate any detected problems,is suggested, discussed with the appropriate parties and implemented where necessary. QA Plan SeationNo.S rev.4 Date]nitrated:.915194 Date Revised:L e103 " Page 2 of 6 With input from the appropriate staff members,the QA Director writes,edits and archives QA Plans,QC protocols,safety procedure,and Standard Operating Procedures (SOPS)in accordance with US EPA approved methodologies,and GLP procedures. If site specific or project specific QA Plans and/or QC protocols are needed,these will be generated as needed. An essential element of the QA program is record keeping and archiving all information pertaining to quality assurance including QA/QC data,pre award check sample results and scorm performance test sample results and scores,state certifications of the laboratory,external and internal audits and resolution of EPA and other audit team comments,recommendations and reports are also included. The QA Director also plays an important role in the corrective action mechanism described in Section 16. In addition,the QA Director works with scientists and management to continually upgrade procedures and systems to improve the laboratory's efficiency and data quality. Ultimately,the success of the QA program depends on the cooperation and support of the entire organization. The hGTKEM laboratory's most valuable resource is its staff of dedicated professionals who take personal pride ill the quality of their performance. Mitkem Corporation's personnel job descriptions: Responsibilities of each staff area in the laboratory include: Bench Scientist/Preparation Laboratory Areas: • Analysis of samples through compliance with all aspects of formally approved analytical methods and laboratory SOPS • Carefully documenting each step of the analytical process • Noting in the appropriate logbook area any unusual occurrences or sample matrix problems • Conscientiously obtaining peer review as required • Promptly alerting laboratory supervisors and/or QA staff members to problems or anomalies that may adversely impact data quality • Routine housekeeping duties for their laboratory area Bench Scientist/Instrument Laboratory Areas: • Analysis of samples through compliance with all aspects of formally approved analytical methods and laboratory SOPs • Routine maintenance of instrumentation • Preparation of analytical standards and spiking solutions which are documented and traceable to their original source • Carefully documenting each step of the analytical process " • Noting in the appropriate logbook area any unusual occurrences or sample matrix problems QA Plan Section No.S mv.4 Date Initiated:I115/94 Date Revise&1/08/03 Pago3 of G • Conscientiously obtaining peer and supervisor review as required • Promptly alerting laboratory supervisors and/or QA staff members to problems or anomalies that may adversely impact data quality • Documenting the initial review of analysis data to determine compliance with established company QA/QC protocols and any project-specific QA criteria,and noting any unusual occurrences or discrepancies on the data review checklist. • Routine housekeeping duties for their laboratory area Supervisor: • Oversight of bench scientists in their laboratory areas • Monitors the status of all work in their laboratory area to insure compliance with holding time and turnaround time requirements • Training new scientists in the appropriate procedures and methods in the laboratory • Works with laboratory managers and the QA staff to review,revise and implement SOPS • Insures adequate resources to perform the needed tasks by working with administrative personnel to order needed supplies • Insures all supplies and reagents meet the QC requirements of their intended task prior to their use in the laboratory • Insures all staff are using proper safety protocols • Works with laboratory managers on the annual review of personnel performance • Interviews prospective new employees to insure they have the minimal level of qualifications,experience, education and skills necessary to perform their tasks,as well as the appropriate work ethic and social skills necessary for proper teamwork and productivity • Review of analytical data to insure compliance with method/SOP requirements prior to release to the client • Documents any non-compliance or other unusual occurrences noted during sample analysis and data review such that these can be included in the report narrative and*explained to the client Senior Scientists: • Review of analytical data to insure compliance with method/SOP requirements prior to release to the client • Documents any non-compliance or other unusual occurrences noted during sample analysis and data review such that these can be included in the report narrative and explained to the client • Assist laboratory Managers and Supervisors in other tasks as required Laboratory Managers: • Review of analytical data to insure compliance with method/SOP requirements prior to release to the client 0 Oversight of Supervisors and Senior Scientists in their laboratory areas QA Plan Section No.5 rev.4 Date Initiated:1/15/94 Date Revised:1/oa/03 Page 4 of 6 • Assists analysts and Supervisors in the troubleshooting and maintenance of instrumentation • Works with instrument suppliers to insure appropriate instruments are available in the laboratory • Provides technical assistance to other laboratory staff Operations Manager_ • Prioritizes work in the laboratory areas to insure projects are completed on a timely basis • Works with laboratory Managers and Supervisors to coordinate laboratory areas in the completion of analytical projects • Review of analytical data to insure compliance with method/SOP requirements prior to release to the client • Writes project report narratives to document any unusual occurrences noted during sample analysis • Works with management and supervisory staff to continuously improve the quality and efficiency of all company procedures • Works with clients to insure all questions and concerns are addressed and answered • Assists laboratory Managers and Supervisors in the annual review of personnel performance • Supervises laboratory Managers and Supervisors to insure compliance with company QA policies and other company procedures Project Manager: • Works with the client to completely understand the requirements of all incoming work • To evaluate the client's requirements-as compared to the abilities of the laboratory as stated in Mitkern's Standard Operating Procedure(SOP);Project Coordination,#G19. • To communicate the customer's requirements to all laboratory staff working on the project • Works with the customer to determine the number and type of sample containers required for the project • Works with the Sample Custodian to resolve and communicate to the client any problem or discrepancies with incoming samples • Maintains open,responsive and continuous communication with the customer. • Follows up with the client to assess level of satisfaction,and insure all project goals have been accomplished. QA Director: • Implements the entire QA program • Interact on a daily basis with laboratory staff • Evaluates compliance with the QA program through formal and informal reviews of data and processes • Implements the corrective action system • Works with laboratory Managers and Supervisors to implement new SOPS and to annually review and revise existing SOPS QA Plan Section No.5 rev.4 Date Wtiated-1115/94 Date Revised 1/08/03 Page 5 of 6 • Interfaces with certification authorities and agencies to maintain existing certifications and obtain new certifications • Maintains records of employee training and certification Technical Director. • Review of analytical data to insure compliance with metho&SOP requirements prior to release to the client • Supervises all Management,QA and Supervisory staff to insure compliance with company QA policies and other company procedures • Provides technical assistance to all areas of the laboratory staff • Works with clients to insure their understanding of complex technical issues The personnel training records are located in the QA department.All individual training is documented including new employee training, individual training,and Health and Safety training. i QA Plan . Scc ioallo.5my.4 Date lftWed_1115/94 Date Revised:IM/03 Page 6 of 6 Figure 5-1 MTTKEM Corporation's Organizational Chart I . �II T�� Sal r 8 � a r P—1 a O � r E $l - ' ° .. . ro b -- I ra m 6 ION S.CHIU Chief Executive Oftloerfrechnical Director Dr.Chiu is a MIT trained mass spec tmeopist with extensive experience in the trace level analyses of organic and hazardous waste compounds in environmental samples. He has over twenty years of experience in using GCJMS,HPLC and OC with various detectors. He has been involved with research and development on con-routine analytical .approaches to environmental chemistry problems. Dr.Chiu has been the lead chemist responsible for analytical laboratory operations_at several of the most respected laboratory facilities in the northeast. Dr.Chiu has extensive program management experience through positions of high responsil ility in Contract Laboratory Program(CLP)laboratories. He also has sigmficant experience with the management ofprograms involving Army Corps of Engineers,Navy and Air Force analytical rnquiremerits. Dr.Chiu also has extensive experience with the financial and business management responsibilities of small and medium size corporations,as well as the public sector. MITKEM is his second environmental laboratory start-up.The first,CE1M[C Corporation was also highly successful.He was an active partner in both the tcbnical and business aspects of both companies. EDUCATION MASSACHUSETTS INSTITUTE OF TECHNOLOGY Cambridge,Massachusetts Chemistry,PhD RUTGERS UNIVERSITY New Bnmswid:,New Jersey Environmental Sciences,US ! UNIVERSITY OF MARYLAND College Park,Maryland Chemisty,BS RELATED EXPERIENCE 1994-Present MF=K CORPORATION Wanyick,Rhode Island Chief Executive Officer Technical Director 1993 COAST TO COAST ANALYTICAL Westboro*Maine • -Di ector of LObor tort'Operations 1991-1993 MASSACHUSETTS WATER RESOURCES ! AUTHORITY Boston,Massachusetts Laboratory Superir&ndent 1988-1992 CEMUC CORPORATION Nmnansd#,Rhode Island -Vice President Organic Laboratory Operations and Technical Director 1983-1988 ENSECOlERCO DIVISION Cambridge,Massachusetts- -Head of Research and Development i - I REINTER A.COURANT Vice President a Mr.Courant has over twenty five years of experience in environmental chemistry. fle has managed a number of large scale multi-disciplinary and international ea►vironmeatal baseline studies. Tbese studies involved the collection and analysis of samples for a wide variety of parameters,evaluation and interpretation of the generated data,and writing of the final report. Mr.Courant leas authored 25 scientific papers,taught chemistry at the university level add held senior scientist and project-manager positions as well as upper management and partner positions in several environmental firms. Mr.Courant has extensive experience im many phases of environmental chemistry,with particular concentration in laboratory design and automation,specifically m electromie transfer of data and set-up of infon nation management systexus.- Mr.Courant also has considerable experience in sample analysis,data review and data package preparation for EPA Contract Laboratory Program inorganic sample analyses. Mr.Courant's experience with chemical analysis instrumentation is rvidcgwie hg,with a primary focus on elemental and trace metals analyses. In the past ten years he has been involved in the start-up and senior management of several environmental testing laboratories. EDUCATION UNIVERSITY OF RHODE ISLAND Graduate School of Oceanography Kingston,Rhode Island Chemical Oceanography,MS NORTHEASTERN UNIVERSITY Bostoa,Massachusetts Mathematics,MS DELFT INSTITUTE OF TECHNOLOGY Delft,Netherlands RELATED EXPERIENCE 1994-Present MITKEM CORPORATION Warwicir,Rhode Island -Vice President 1 1991-1994 CC CORPORATION Lacingtoo,Massachusetts -President 1987-1991 CBILvIIC CORPORATION Narragansett,Rhode Island -Woe President 1985-1987 ENERGY AND ENVIRONMENTAL 19WI983 ENGWEERJNG,INC. Cambridge,Massachusetts -Vice President 1983-1985 RESEARCH PLANNING INSTITUTE Columbia,South Carolina -Senior Chemist Niger Delta Baseline Studies 1978-1984 ENTERSTATE ELECTRONICS CORPORATION Anaheim,California -Senior Oceanographer US EPA Studies of US Offshore Dumpsites 1976-I978 ENERGY RESOURCES COMPANY-ERCO Cambridge.MassachusdU -Field Operation Manager and Senior Oceanographer Georges Bank Region Environmental Baseline Studies 1972-1976 IONTVLRSITY OF RHODE ISLAND Kingston,Rhode Island -Research Spedalis Graduate Student 1969-1972 WOODS HOLE OCEANOGRAPHIC INSTITUTE Woods Hole,Massachusetts -Research AssistantlGraduatc Student I Thomas A.McConnell Quality Assurance Director Mr.McConnell has over ten years experience within the environmental industry as well as several years in other areas as manufacturing,medical device and phaimaceuticaLs.Mr.McConnell has gained his technical knowledge working for several environmental laboratories beginning as a Chemical Toxicologist,QC Chemist, Batch Chemist for a pharmaceutical company,and a Lab Director for a waste recycling company.Through his years as a Chemist he has a working knowledge of GC,ICP,AA, and HPLC imtrumentation.As a Toxicologist,he acquired the knowledge of how chemicals and other pollutants impact the environment. Mr.McConnell has over eight years experience within the quality field.Working as a QC Chemist for a manufacturing company,a Quality Assurance Officer for a medical device company,QA Manager for a Environmental Testing Lab,and as a Quality Consultant for several domestic clients.He has course certifications for Hazardous Waste Management,GMPs,GLPs,GCPs and ISO standards. Mr.McConnell's current responsibilities include the overall function of Mitkem's quality program.This would include training,document control,change control, corrective action,track and trending,certifications,laboratory reviews,internal and external audits,and personnel review. As the Hazardous Waste/Health and Safety Officer,it is his responsibility to oversee Mitkem's hazardous waste program including chemical training,safety training, accident reportinglinvestigation,and compliance with government laws and regulations. - Education ' .1976-1980 Southeastern Massachusetts University- Dartmouth,MA BS,Chemistry Business Law(Contracts) 1975-1976 Bristol Community College-Fall River,MA - Lair Enforcement Related Experience 2002-Present Mitkem Corporation ' Warwick,RI Quality Director - 2000-2002 Quality Consultants_ N Dartmouth,MA Consultant I 1998 2000 ESS Laboratory Cranston,RI '- •` Quality Manager 1994-1997 American Red Cross,NHQ Dedham,MA Quality Assurance Officer 1992-1994 Armstrong Pharmaceuticals W.Roxbury,MA Batch Chemist 1991-1992 Sanborn,Inc Wrentham,MA Laboratory Manager 1990-1991 Benjamin Moore E Milford,MA QC Chemist '19874999 Springborn Laboratory Wareham,MA F=' Chemianoxicologist 3.t.. , r 1983-1989 CAMBRIDGE ANALYTICAL ASSOCIATES,INC. Boston,Mamadwsetts Project Manager VoWe Organic Laboratary Manager 1978-1983 ENERGY RESOURCES COMPANY,INC- ERCO Cambridge,,Massachusetts, -Volatile Organics(Gq Manager Analytical Chemist-Volatile Organics Lab -Analytical C hwmistOrg c preparation Lab 1978 LAPUCK LABORATORIES,INC Watertown,Massachusetts -Analytical C hcui t-Wet C h emis(xy&Metals -Microbiologist i EDWARD A.LAWLER Operations Manager Mr.Lawler has over twenty years of experience in environmental UboratotY oPeratioas• extensive axperieace is�&8 Laboratory workflow and in establiding and He has _ • _:.:.,� u:9t.has considerable experience in a wide mega inant�airing Customer of ea*onineatai chemical analyses,with a concentration in trace level volatile organics anslysir. Mr.Lawler's responsMties include coordination and Prioritization of an analytical r. chcmistrY testing at Mitkem. 'this includes daily ni,eetings with the organic and inorganic wry pervisors and mamgers to ia�all tediinicalLabora and schedule rbquire are met Mr.Lawler also reviews laboratory data to insure QAlQC wteria bave,been vides final review Of data reports prior to delivexY to clients. I41r. achieved and ° significant a nalytical testing pro!' aactingas principalLawler all so manages certain l tecbnical liaison with the client previous oxperieace includes various staid;management and senior W.Lawles's p Laboratories. Direct project QiaAagement positions at several environmental BSA and 1�II?t?SC,DOD experien ce includes EPA CLP.Army Wm.Navy NF- HAZWRAP and New York DEC ASP pmgrams. Mr.Lawler has also provided expert testimony at several Superfund trials including Pre-trial consulting and trial witness services. EDUCATION: UNIVERSITY OF MASSACHUSETTS Amherst,Massachusetts Environmental Sciences,BS RELATED MERIENCE. 1997-Present 11IITUM CORPoRATIUN Warwick,Rhode island -Operations Manager II f I I989-I997 NATIONAL ENV R0NME�ITAL IySMG, CAMBRIDGE DIMION BeMrd,Massachusetts Divisioa Manager .proposaUCoutract Manager IDirector of Project Management I I _ YIHAI DING Chemist,GGMS and GC Laboratories Mr.Ding has experience in a wide variety of analytical chemistry techniques,including GC, GCUS,HPLC and FTM His expertise includes the operafion,calibration and maintenance of sophisticated,computer controlled instrumentation. Mr.Ding's responsibilities include the daily tuning and calibration of analysis instrumentation, monitoring QC criteria,sample analysis,review of results and mass spectra data,use of CLP forms generation software and other statistical data evaluation software. Mr.Ding's prior experience includes research into the mechanisms and ldnedcs of various biochemical processes. A large portion of this research has required the analysis of reactants and products using state-of-the-art chemical instrumentation. I& Ding has also taut chemistry and biochemistry laboratory courses at the university level- EDUCATION MIDDLE TENNESSEE STATE UNIVERSITY Murfreesbr%Tennessee Chmistry,MS JILIN UNIVERSITY Changchun,China i - Biochemistry,BS RELATED EXPERIENCE 1998-Present bffrKEM CORPORATION Warwick,Rhode Island - GC/MS Analyst 1994-1998 MIDDLE TENNESSEE STATE UNIVERSITY Murfreesbro,Tennessee - Researcher - Laboratory instructor,chemistry and biochemistry 1993-1994 NATIONAL ENZYME ENGINEERING LAB Changchun,China - Researcher I l i KAREN M.GAVrrr Inorganic Laboratory Manager Ms.Gavitt has neady ten years of experience in the analysis of enviromental and hazardous waste samples for both organic and inorganic analytess. A large portion of this experience has involved the use of axial ICP,radial 1CP,cold vapor AA and graphite furnace AA for trace metals analysis. Ms.Gavitt's responsibilities at Mitkem include management of the inorganic chemistry laboratories including metals and oonvenhoW wet dwaucal analyses. Her duties include the day-to-day scheduling of all analytical work in her dqwtnent to med program, turnaround and method holding time requirements. Ms.Gavin is also responsible for the technical and QC performance of a wide variety-of methods,as well as development and implementation ofStandard Operating Procedures,method and instrument performance measures, daily review of sample and QC data,training of laboratory staff and discussion. of program requirements and project status with Mitkan s project managers and clients. She was a GC/MS analyst during her most recent employment before joining Wtkem. Ms.Gavitt also has experience in the analysis of samples for inorganic and organic analyses by US EPA CL,P protocols,New York State ASP protocols and various DOD analytical programs. EDUCATION DUQUESNE UNIVERSITY Pittsburgh Pwnsylvarda Chemistry,$S RELATED LXPERIENCE 1994-Present MLTKEM CORPORATION warwidk Rhode Island u -Inorganic Laboratory Manager 1994 ENMONMENTAL SCIENCES SERVIOES Provide me,Rhode Island -GCYMS Analyst 1990-1994 CEIMIC CORPORATION Narragansett,Rhode Island -Trace Metals Laboratory Supervisor . Organic Prep Lab Technician ROBERTA A.CARVALHO Semivolatile Organic Laboratory Supervisor Ms.Carvalho has experience with Malysis of environmental samples by a variety of analytical t.dwques. Her responsibilities at mtkem involve the coordination of seanivolatile organics analyses using GC/MS instrumentation. Her duties in this role include instrument calibration and maintemancc,sample analysis,review of sample and.QC data,implementation of Standard Operating Procedures,documentation of msttummt and.method QC criteria and-coordination with other laboratory sections. Ms.Carvalho'S experience includes GOMS,ICP/MS,CTq IC and AA techniques. She has used this equipment im routine analysis and research roles. She has also taught chemical instrumentation courses in a university setting. Ms.Carvalho has experience with tho analysis of a wide variety of terrestrial and marine sample matrices,as well as atmospheric samples. She has participated in 20 offshore rwmrh cruises involving various responsibilities including co- chief scientist. Her knowledge of chemical analysis of environmental media is wide-ranging and I diverse. EDUCATION TEXAS A&M UNIVERSITY College Station,Texas Chemicd Ooeanography,MS TEXAS A&M UNIVERSITY Galveston,Tom - Marine Biology,BS { i RELATED EXPERIENCE 1998-Present MITKEM CORPORATION Warwick,Rhode Mud - QCMS Analyst i 1998 LAWLER,MATUSKY&SKELLY ENGINEERS Somerset,Massachusetts Environmental Field Technic= I 1997 U.S.GEOLOGICAL SURVEY Woods Hole,Massadumdts Todhnical Consultor,Marine Geochemistry Division 1990—1997 TEXAS A&M UNIVERSITY College Station,Texas Gla&ate Swdent Teacher,Analytical Inshmentation - Researcher,-OceanowvWc and Havironmental Research Laboratory {1 1 YDLU DING Chemist;GOO and GC Laboratories Mr.Ding has experience in a wide variety of analytical chemistry techniques,including GC, GClMS,B PLC and MR. His expertise includes the operation,calibration,and mainteteanoe of I sophisticated,computer controlled instrumentation. W.Ding's responsibilities include fbe daily tuning and calibration of analysis instnm►entation, monitoring QC criteria,sample.analysis,review of results and mass spectra data,use of CLP forms generation software and other statistical data evaluation software. I&Ding's prior.mperieuce includes research into the mechanisms and kinetics of various biochemical processes. A large portion of this research has required the analysis of reactants and products using state-of-the-art chemical instrumentation. Mr.Ding has also taught chemistry and biochemistry laboiatory courses at the university level. I EDUCATION MIDDLE TENNESSEE STATE UNIVERSITY Murfivesbro,Tennessee - Chemistry,MS JILIN UNIVERSITY i Changchun,China Biochemistry,BS t RELATED EXPERIENCE 1998-Present MI ERM CORPORATION Warwick,Rhode Island GGMS Analyst i 1994-1998 MIDDLE TENNESSEE STATE UNIVERSITY + Mur ftoc6ro,Twnessee j - Researcher - Laboratory Instructor,chemistry and biochemistry 1993-1994 NATIONAL ENZYME ENGINEERING LAB Changchun,China Researcher I GONGMIN LEI Gas Chromatography Lab Manager Mr.Lei has several years of experience in the analyses of samples for Pesticide and PCBs. He also has experience in the extraction of analyses of hydrocarbons is water and sediments by CG PID and GC-MS techniques. As mannw of MitkoWs gas chromatography laboratory Mr.Lei is responsible for the daily scheduling of all GC-analyzes including pestiddes,PCBs:herbicides,.petroleum hydmcartbous, and specialty testing. Mr.Lei iS also responsible for the implementation of Standard Operating Procedures,the production and review of sample and QC results,the documentation of instrument and method perfounance data and the training of analytical stalE Mr.Lei is familiar with the use of the Target software package to provide EPA CLP and New York State ASP deliverables on a wide variety of GC analysis methods. Prior to joining Mitkem W.Lei-gained extensive experience in the application of analytical chemistry techniques to a wide variety of environmental problems,both in the US and in China. He has worked as a researcher in both university and government organizations dedicated to managing environmental issues. EDUCATION UNIVERSITY OF MASSACHUSETTS Boston},Massachusetts Environmental Sciences,MS NANKAI UMVERSIT'Y Tianjin,China - Environmental Analytical Chemistry,MS - Chemistry,BS RELATED EXPERIENCE 1996-1'ceseut MITKEM CORPORATION Warwick,Rhode Island Pestieide/PCB Lab Manager 1993-1996 UNIVERSITY OF MASSACHUSETTS Boston,Massachusetts Research and Teading Assistant 1987-1993 TIANJIN INSTITUTE OF ENVIR,PROTECTION Tianjin,China - F.avima�ntal F.agiuoa 19841987 NANKAI UNIVERSITY 114in,Chin -Research Assistant 1 PAUL T.BOUDRIA Organic Preparation Laboratory Sapervlsor Mr.Boudria is responsible for the daily workflow management and supervision of the organic sample preparation laboratory. In this role he evaluates incoming sample analysis requests,schedules sample and QC analyses,reviews data,interfaces with the supervisors of the GC and GONS laboratories to iasm all technical and schedule requirements are met: He also provides training to laboratory staff,develops and reviews Standard Operating Procedures,implements new methods,performs and evaluates method performance documentation. Mr.Boudda is thoroughly familiar with U.S.EPA and SWW methodologies and sample extraction and cleanup protocols. He has also worked on a contract basis for a major pbArmaceutical company specializing in hazardous'and other chemical waste' management,including OSHA hazardous waste operators duties and training. EDUCATION BRIDGEWATER STATE COLLEGE Bridgewater,Massachusetts Chemistry/Geology;BS. RELATED WORK EXPERIENCE 1998-Present MITK M CORPORATION Warwick,Rhode Island - Preparation laboratory Supervisor 1998 PFIZER PHARMACEUTICALS Croton,Connecticut Contract Hazardous waste Specialist/Chemist 1996-1998 M1TKM CORPORATION Warwick,Rhode Island Preparation Laboratory Chemist LEONARD A.RANALLI Chief Finaneial Officer Mr.Ranalli has an extensive financial and business background. He brings to the MitkcVA CoMomtioa 18 years of banking cgmxieace- M enPerfm is in operations and financial EDUCATION: BROWN UNIVERSITY Providence,Rhode Island Sociology,BA RELATED EXPERIENCE: 1994Present MITKEM CORPORATION Warwick,Rhode Island -Chief Financial Officer 1992-1994 OLD STONE BANK providence,Rhode Island -Assistant Vice President/ Commercial Real Estate Officer [990-1992 EASTLAND BANK Woonsocket,Rhode Island -Assistant Vice Presidend Commercial Loan Officer i 1981-1990 RHODE ISLAND HOSPITAL TRUST NATIONAL BANK Providence, Rhode Island -Loan Officer -Credit Analyst -Operations Manager,Wuc Transfer Department -Operations Manager,Purchasing Department i I i PAUL A.SENECAL a Marketing Director Mr.Senecal has several years of experieaaoe in marketing mW client services in the eatvironmental laboratory industry as well as a strong scientific background. His duties include business development,projed management and budding and maintaining client relationships- Mr.Senecal works.with-engineers,-Consultants and-government clients to develop'and define the scope of analytical chemistry programs. He has experience in the set-up and management of a wide variety of site assessment and monitoring projects. "Ibis experience includes programs performed under the auspices of the New York State DEC, the US EPA,Army and Air Fora covironmental agencies. He also has managed a number of large-scale analysis programs for commercial and industrial clients. He is familiar with the method and QC requirements of these analytical programs,the evaluatioa of samples received at the laboratory for compliance with program requirements,the communication of any technical or schedule issues developed during t the sample analysis process. Prior to his employment at M.rtkem Mr.Senecal worked for a large multi-location ' environmental testing laboratory participating in a wide variety of govemmeat and private chemistry program& EDUCATION: ST.LAV RENCE UNIVERSITY i Canton,New York Biology,BS RELATED EXPERIENCE: 1995-Present MITE EM CORPORATION { Warwick,Rhode Island -Account Executive 093-1995 PACE,INCORPORATED Winneapolis,Minnesota -Account Executive -Ciicatt Services Technician -Chemist 1992 MINNESOTA PUBLIC LOBBY Wmeapolis,Minnesota -Field Manager 1 BENJ'AMIN F DODGE Account Executive W.Dodge oversees day-to-dayprogtam management of in-house projects and serves as technical liaison to clients. In this vole Mr.Dodge is responsible for defining project scope&vugh discussion with the diem,detaminatioa of proper analytical methodology, development of price quotations,discussion of technical and schedule issues with laboratory personnel,reviewing client inquests on chain of custody and sample transmittal documentation,resolution of any problems in sample delivery or . documentation,review•of project log-In Inf)rmadoa,monitoring project status and communication of status information to the cheat,discussion of results and communication of questions or technical interpretation with the client,and follow-up on completed projects. Mr.Dodge has manMod a wide variety of analytical services projects'at&frtke m, including site investigation,remedial support,long-term landO monitoring,industrial wastewater and hazardous waste programs, A number of these programs have involved -the production of EPA Contract Laboratory Program(CLP)data deliverables,or New York State Analytical Services Protocol(ASP)deliverables and methodology. A significant portion of the programs Managed by Mr.bodge have involved rapid turnaround analytical services,requiring a high level of program mianagmuent. EDUCATION EASTERN CONNECTICUT COLLEGE Willimantkc Connecticut Eavironmental Science,BS RELATED WORK EXPERIENCE i996-Pi+aseat 1M' RM CORPORATION Warwick,Rhode Island Project Coordinator + Sample Custodian, QA:Plan section Na b rev.4 Date Initiated 1/15/94 Date Revise&1/08103 Panel of 2 6.o QUALITY ASSURANCE OBJECTIVES FOR MEASUREMENT DATA IN TERMS OF PRECISION,ACCURACY,REPRESENTATIVENESS,COMPLETENESS AND COMPARABILITY As part of the evaluation component of the overall QA Program,laboratory results are compared with the data quality indicators defined as follows: • Precision:the agreement of reproducibility among individual measurements of the same property,usually made under identical conditions. • Accuracy:the degree of agreement of a measurement with the true or accepted value. • Representativeness:the degree to which data accurately and precisely represent a characteristic of a population,parameter variations of a sample of a finite process condition,or of a finite environmental condition. • Completeness:a measure of the amount of valid data obtained from a measurement system compared with the amount that was expected to be obtained under normal conditions. • Comparability: an expression of the confidence with which one laboratory data set can be compared with another laboratory data set in regard to the same property and laboratory sample population. Quality Assurance objectives may vary by project and requested parameters. The accuracy,precision, and representativeness of data will be functions of the origins of the sample material,the procedures used to analyze samples and generate data,and the specific sample matrices involved in each project.. Quality control practices utilized in the evaluation of these data quality indicators include blanks,replicates, spikes, standards,check samples,calibrations and surrogates. The process for quantifying or assessing the above indicators for data quality is addressed in Section 15. 6.1 Precision and Accuracy: For each parameter analyzed,the QA objectives for precision and accuracy will be determined from: i • Published historical data; • Method validation studies; • MITKEM experience with similar samples and/or, • Project-specific requirements,such as those stipulated by the USEPA in the CLP protocols and control documents. i QA Plan Section No.6 iev.4 Date kd iaW:1/15/94 Date Revise&1/08M3 Page 2 of 2 6.2 Representativeness: Analytical data should represent the sample analyzed regardless of the heterogeneity of the original sample matrix. In most cases,representativeness is achieved by mixing the laboratory sample well before removing a portion for analysis. On occasion,multi-phase laboratory samples may require that each phase be analyzed individually and reported in relation to its proportion in the whole sample. 6.3 Completeness: The completeness goal is 100%in all cases and includes: • Analysis of all samples; • Generation and analysis of all required QC samples; • Sufficient documentation of associated calibration,tuning and standardization; • Records of data reduction processes,including manual calculations. While the laboratory staff is responsible for achieving the completeness objective stated above,completeness is ensured by assigning each project a specific project manager whose functions include sample management and tracking. 6A Comparability: To assure comparability,Mr=M employs established and approved analytical methods(e.g.USEPA protocols),consistent analytical bases(dry weight,volume, etc.)and consistent reporting units(mglKg,µg/L,etc.). Where data from different samples must be comparable,the same sample preparation and analysis protocols are used for all of the samples of interest. i i QA Plan Section?rev.4 Datehddated Y15M Date Revised:1/0"3 Page 1 of 9 7.0 SAMPLING PROCEDURES For most proj ects,outside sampling teams deliver or send samples to the MITKEM laboratory. When sampling by MTTKEM personnel is required,the sampling team follows the sampling procedures outlined in the EPA/SOW Test Methods for Evaluating Solid Wastes,SW-846, P Edition,or procedures found in the EPA"Handbook for Sampling and Sample Preservation of Water and Wastewater". Appropriately prepared sample containers are supplied by MI TKEM at clients'request. When required,preservatives are added to the sample containers. Tables 7-1 through 7-3 provide the MI TKEM Recommended Methods for Sampling,Sample Volume and Preservation of Samples for Analysis. Additional sample volumes may be required if additional QC functions are to be performed. Holding times for SW846,CLP Methods,Standard Methods and certain USEPA methods are different and are presented in Tables 7-1 to 7-3. i i �I i i i. QA Plan Section 7 rev.4 Date inidatak 1115/94 DateRevised:1/0"3 Page 2 of 9 Table 7-1 Recommended Container,Preservation Techniques and Holding Times for SW-846 Analyses Required* Holding motes Method Containers Volume Preservation Times Volatile Organics Solid 8260B,5030E Amber glass jar Minimal bead 4'C 14 days with Teflon lining space in jar Solid a 8260B,5035 40mL vial or Encore 5.0gram t 0.5 4'C,unpreserved 48 hours with Teflon lining DI Water 14 days -10 to—200C Sodium bisulfate 14 days -10 to—20°C,4°C Methanol 14days 4°C Aqueous 8260B,5030B 40mL VOA Vials 40mL 4°C 14 days with Teflon septum HCI,pH<2 Semivolatile Organics Solid 3540C,3550B Amber glass jar 30gram 40C Extraction within 14 days 8270C with Teflon lining Analysis within 40 days Aqueous 3510C,3520C Amber glass bottles IL 4'C Extraction within 7 days 8270C with Teflon lining Analysis within 40 days Polychlorinated Biphenyls Solid 3540C,3550B Amber glass jar 30gram 40C Extraction within 14 days 8082 with Teflon lining Analysis within 40 days Aqueous 3510C,3520C Amber glass bottle 1L 4°C Extraction within 7 days 8082 with Teflon lining Analysis within 40 days Organochlorine Pesticides Solid 3540C,3550B Amber glass jar 30gram 40C Extraction within 14 days 8081A with Teflon lining Analysis within 40 days Aqueous 3510C,3520C Amber glass bottle IL 40C Extraction within 7 days 8081A with Teflon lining Analysis within 40 days Chlorinated Herbicides Solid 8151A Amber glass jar 30gram 40C Extraction within 14 days 8151A with Teflon lining Analysis within 40 days Aqueous 8151A Amber glass bottle 1L 40C Extraction within 7 days 8151A with Teflon lining Analysis within 40 days QAP1an Section 7 rev.4 Date Igi iated:1/15M Date Revised 1106103 Page 3 of Table 7-1 (cont'd) Recommended Containers,Preservation Techniques and Holding Times for SW846 Analyses Required+ Holding Ana�es M Containers Volume Preservation Times Total Petroleum Hydrocarbons Gasoline Range Organics Solid 8015M,5030B Amber glass jar Minimal head- 40C 14 days With Teflon lining space in jar Solid' 8015K 5035 40mL vial or Encore S.Ogram t 0-5 4°C,unpreserved 48 hours with Teflon lining DI Water 14 days -10 to 200C Sodium bisulfate 14 days -10 to—20°C,40C Methanol 14days 40C Aqueous 8015K 5030B 40mL VOA vials 40mL 40C 14 days With Teflon septum HCi,pH<2 Diesel Range Organics Solid 3540C,3550E Amber glass jar 30gram 40C Extraction within 14 days 8015M with Teflon lining Analysis within 40 days Aqueous 3510C,3520C Amber glass bottle 1L 4°C Extraction within 7 days 8015M with Teflon lining H28O4i pH<2 Analysis within 40 days Total Metals except Mercury and Chromium(VI) Solid 3050B Amber glass jar log 4°C 180 days 6010B with Teflon lining Aqueous 3005A,3010A Polyethylene bottle 10081L HNO3,pH<2 180 days Chromium(VI) Solid 7196A Amber glass jar log 4°C Digestion within 30 days with Teflon lining Analysis within 96 hours Aqueous 7196A Polyethylene bottle 25mL 4°C 24 hours Mercury Solid 7471A Amber glass jar log 40C 28 days Aqueous 7470A Polyethylene bottle loomL 40C 28 days HNO3,pH<2 1 QA Plan Section T rev.4 Dete la"tcd 015194 D*Rcvised tMM Page 4 of Cyanide Solid 9012 Amber glass jar lg 4°C 14 days with Teflon lining Aqueous 9012 Polyethylene bottle SOmL 4"C 12 days NaOH,pH>12 Flashpoint Aqueous 1010 Amber glass bottle 30mL 40C 28 days i QA Plan Section 7 rev.4 Date Initiated:1/t 5/94 Data Revisal:t/06M Page 5 of 9 Table 7-2 Recommended Container,Preservation Techniques and Holding Times For CLP/ASP Analyses Required* Holding �l method Containers Volume Preservation Times Volatile Organics Solid CLP/ASP Amber glass jar Minimal head- 40C 10 days from VTSR with Teflon lining space in jar Aqueous CLP/ASP 40mL VOA vials 40mL 40C 10 days from VTSR with Teflon septum HCI,pH<2 CLP Low 40mL VOA vials 40mL 40C 10 days from VTSR with Teflon septum HCl,pH<2 Semivolatile Organics Solid CLP/ASP Amber glass jar 30gram 4`C 10 days from VTSR with Teflon lining Analysis within 40 days Aqueous CLP/ASP Amber glass bottle 1L 40C 5 days from VTSR with Teflon lining Analysis within 40 days CLP Low Amber glass bottle IL 4-C 5 days from VTSR with Teflon lining Analysis within 40 days Organochlorine Pesticide/PCB Solid CLP/ASP Amber glass jar 30gram 40C 10 days from VTSR with Teflon lining Analysis with 40 days Aqueous CLP/ASP Amber glass bottle 1L 40C 5 days from VTSR with Teflon lining Analysis within 40 days CLP Low Amber glass bottle 1L 4°C 5 days from VTSR with Teflon lining Analysis within 40 days Cyanide - Solid CLP/ASP Amber glass jar 2gram 40C 12 days from VTSR Aqueous CLPIASP Polyethylene bottle 50mL 40C 12 days from VTSR NaOH,pH>12 Total Metals except Mercury Solid CLPIASP Amber glass jar 2gram 4°C 180 days from VTSR Aqueous CLP/ASP Polyethylene bottle 100mL HNO3,pH<2 180 days from VTSR QA Plan Section 7 m.4 Date fidtiated:1IM4 Date Revised:IIM3 Page 6 of 4 Table 7-2(con't) Recommended Container,Preservation Techniques and Holding Times For CLP/ASP Analyses Required* Holding Anabdo Method SQ _ ipm Volume Preservation Times Mercury Solid CLP/ASP Amber glass jar logram 40C 26 days from VTSR Aqueous CIP/ASP Polyethylene bottle 100mL 40C 26 days from VTSR HNp3i pH<2 QAPIan Section 7 rev.4 Date laitiated:In5N4 Date Reviscd:I10"3 Page 7 of Table 7-3 Recommended Containers,Preservation Techniques and Holding Times for Other Analyses Required* Holding Anal vtces Method Containers Volume Preservation Times Volatile Organics Aqueous 624 40mL VOA vials 40mL 4°C 14 days with Teflon septum HCI,pH<2 524.2 40mL VOA vials 40mL 40C 14 days with Teflon lining HCI,pH<2 Semivolatile Organics Aqueous 3510C,3520C Amber glass bottle 1L 4°C Extraction within 7 days 625 with Teflon lining Analysis within 40 days Organochlorine Pesticide/PCB Aqueous 3510C,3520C Amber glass bottle 1L 4°C Extraction within 7 days 608 with Teflon lining Analysis within 40 days EDB/DBCP Aqueous 504.1 40mL VOA vials 35mL 40C 28 days with Teflon septum HCI,pH<2 MA Extractable Petroleum Hydrocarbons(EPH) Solid 3540C,3550E Amber glass jar 30gram 40C Extraction within 7 days MADEP with Teflon lining Analysis within 40 days Aqueous 3510C,3520C Amber glass bottle 1L 40C Extraction within 14 days MADEP with Teflon lining HCI,pH<2 Analysis withing 40 days MA Volatile Petroleum Hydrocarbons(VPH) Solid MADEP Amber glass jar 30gram 40C 14 days with Teflon lining 15mL Methanol Aqueous MADEP 40wL VOA vial 40mL 40C 14 days with Teflon lining HCI,pH<2 Oil&Grease Aqueous 1664 Amber glass bottle 1L 40C 28 days with Teflon lining HCI,pH<2 Alkalinity Aqueous SW320 Polyethylene bottle 100mL 40C 24 hours Ammonia Aqueous SM4500NH3B Polyethylene bottle 100ML 40C 28 days H2SO4,pH<2 Chloride Aqueous SM4500CI B Polyethylene bottle 100mL 40C 28 days QA Plan Sermon 7 rev.4 Date Initiated:1/15/94 Date Revised:1/MM Page 8 of 9 Table 7-3(cont'd) Recommended Containers,Preservation Techniques and Holding Times for Other Analyses Required Holding Anal Method Containers Volume Preservation Times COD Aqueous SM5220C,D Amber glass bottle 50mL 4°C 28 days H2SO4,pHQ Color Aqueous SM2120B Polyethylene bottle 50mL 4°C Immediate Nitrates Aqueous SM450ONO3 E Polyethylene bottle 50mL 40C 48 hours H2SO4,pHQ 7 days Nitrite Aqueous SM450ONO2 b Polyethylene bottle 50ML 4C 48 hours Orthophosphate Aqueous SM4500-P,E Polyethylene bottle 50mL 4°C 48 hours Total phosphate Aqueous SM4500-P B,E PoIyethylene bottle 50mL 40C 24 hours 50ML HCl'pHQ 28 days Phenols Aqueous SM5530B Polyethylene bottle 250mL 40C 28 days SM5530C H2SO4,pHQ Sulfates Aqueous SM4500SO4 E Polyethylene bottle 50mL 49C 28 days Sulfide Total Aqueous SM4500-S D Polyethylene bottle 50mL 40C 28 days Reactivity Solid Chapter 7 Amber glass jar logram 40C 28 days SW846 Aqueous Polyethylene bottle 250mL 4°C 28 days Total Organic Carbon(TOC) Solid 9060 Amber glass jar 20g 49C 14 days Aqueous 415.1 40mL VOA vials 40mL 4'C 28 days HCl,pH<2 QA Plan Section 7 rev.4 D*Initiated:1/15/94 Date Revised.1/0003 Page 9 of Table 7-3 (cont'd) Recommended Containers,Preservation Techniques and Holding Times For Other Analyses Required* Holding nnal da Method Containers Vol Preservation Times TKN Aqueous SM4500Norg C Polyethylene bottle or 50mL 4°C 28 days Amber glass bottle H2SO4,pH<2 Total Solids(TS) Aqueous SM2540B Polyethylene bottle 200mL 40C 7 days Total Dissolved Solids(TDS) Aqueous SM2540C Polyethylene bottle 200mL 40C 7 days Total Suspended Solids(TSS) Aqueous SM2540D Polyethylene bottle 200mL 40C 7 days Settleable Solids Aqueous SM2540F Polyethylene bottle 2o0mL 40C 48 hours *These represent minimum required volume. Additional sample volumes should be collected to minimise headspace loss for volatile analysis. Additional sample aliquot are also required to perform QA/QC functions(e.g.spikes,duplicates),%moisture for solid samples and sample re-analysis(if needed). a For Massachusetts analyses,the volatile soil samples are to be preserved in methanol in the field. QA Plan Section No.8 rev.4 Date Initiated:1/t51% Date Revised:I/OM3 Page I of IS 8.0 SAMPLE CUSTODY 8.1 Chain of Custody: Samples are physical evidence collected from a facility or the environment. In hazardous waste investigations, sample data may be used as evidence in(EPA) enforcement proceedings. In support of potential litigation,laboratory chain-of- custody procedures have been established to ensure sample traceability from time of receipt through the disposal of the sample. A sample is considered to be in the custody under the following conditions: • It is in an authorized person's actual possession,or • It is in an authorized person's view,after being in that person's physical possession,or • It was in an authorized person's possession and then was locked or sealed to prevent tampering, or • It is in a secure area. Chain-of-custody originates as samples are collected. Chain-of-custody documentation accompanies the samples as they are moved from the field to the laboratory with shipping information and appropriate signatures indicating custody changes along the way. Laboratory chain-of-custody is initiated as samples are received and signed for by the Sample Custodian or his/her designate at MITKEM. Documentation of sample location continues as samples are signed in and out of the central storage facility for analysis in the several MITKEM departments using the Sample Tracking Forms(Fig 8.4-1). After analysis,any remaining sample is held in the central storage area to await disposal. 8.2 Laboratory Security: Samples at NUTKEM are kept within the secure areas during all stages of residence,including the periods of time spent in preparation for analysis,while undergoing analysis and while in storage. The entire laboratory is designated as a secure area. The doors to these areas are under continuous surveillance or are kept locked after regular business hours and may only be accessed by key. Only authorized personnel are allowed to enter the secure areas. Visitors to the laboratory must be accompanied by a MTI'KEM staff member. QA PIm Section No.8 cev.4 DatcWtimed 1A5194 Date Revised:1A)W3 Page 2 of 18 8.3 Duties and Responsibilities of Sample Custodian: Duties and responsibilities of the Sample Custodian include but are not limited to: 8.3.1 Receiving samples. 8.3.2 Inspecting and documenting sample shipping containers for presence/absence and condition of 8.3.2.1 Custody seals,locks,"evidence tape",etc.; 83.2.2 Container breakage and/or container integrity. 8.3.3 Recording condition of both shipping containers and sample containers (cooler temperature,bottles,jars,cans,etc.). 8.3.4 Signing Documents shipped with samples(i.e. air bills,chain-of-custody record(s),Sample Management Office(SMO)Traffic Reports,etc.) 8.3.5 Verifying and recording agreement or non-agreement of information on sample documents(i.e.sample tags,chain-of-custody records,traffic reports,air bills,etc.). If there is non-agreement,recording the problems, contacting the client for direction,and notifying appropriate laboratory personnel. (CIient's corrective action directions shall be documented in the case file.) 8.3.6 Initiating the paper work for sample analyses on laboratory documents (including establishing sample project files)as required for analysis or according to laboratory standard operating procedures. 8.3.7 Label samples with laboratory sample identification numbers,and cross- referencing laboratory numbers to client numbers and-sample tag numbers. 8.3.8 Placing samples and spent samples into appropriate storage and/or secure areas. 8.3.9 Where applicable,making sure that sample tags are removed from the sample containers and included in the project file. 8.3.10 Where applicable,accounting for missing tags in a memo to the file or documenting that the sample tags are actually labels attached to sample containers or were disposed of,due to suspected contamination. 8.3.11 Monitoring storage conditions for proper sample preservation such as refrigeration temperature and prevention of cross-contamination. QAPIan Section No.8 rw.4 Date hdtiated:I/IS194 Date Revised:11OW3. Page 3 of Is 8.3.12 Sending shipping containers,prepared sample bottles and sample instructions to clients who request them. 8.3.13 Recording temperatures of freezers and refrigerators in the laboratories. 8.4 Sample Receipt: Sample shipments are received at MITKEM by the Sample Custodian or his/her designated representative. Unless the shipment is a continuation of a previous project,a new project file is started for the sample. The information is logged into the Sample Receipt Logbook(Figure 8.4-1). The cooler is inspected for the following(if applicable)and documented on the Sample Login Form(Figure 8.4-2)for USEPA CLP samples and on the Sample Condition Form(Figure 8.4-3)for the other samples: • Custody seal(conditions and custody number) • Air bill(courier and air bill#) The cooler is then opened and the following checked(in order). Make sure the hood is turned of when the cooler is opened. • Chain of custody record(or traffic report). These are usually taped to the inside of the cover. • Cooler temperature using the temperature gun. Record the temperature of a temperature blank if available • Radioactivity using the Geiger counter.(This should go before cooler temperature) The Sample Custodian will perform the following: • Remove the sample containers and arrange them in the same order as documented in the chain of custody report. • Inspect condition of the sample containers. • Assign laboratory sample ID and cross-reference the laboratory ID to the client ID. • Remove tags and place in the project file. • Check preservative and document in the Sample Condition Form(Figure 8.4- 3)if needed. • Peer review to ensure proper cross-referencing and labeling of sample containers. Any discrepancies or problems are noted in the Sample Condition Notification Form(Figure 8.4-4). QA Plan Section No.8 rev.4 Date hddated.V1-"4 Date Revised:1109103 Page 4 of 18 Depending on the project,the sample custodian may directly inform the client of the discrepancies or convey the information to the project manager who will in turn inform the client. The Sample Custodian signs the Sample Receipt Form and originates a file for the set of samples. The following forms are included in the file:the Sample Receipt Form,chain of custody records,shipping information, and an orange Sample Condition Notification Form if any problems or discrepancies need to be addressed. When the Sample Custodian is not-available to receive samples,the sample container is signed for by another MITKEM staff member. The time,date and name of the person receiving the container are recorded on the custody records. In addition,the cooler temperature and radiation count are measured and recorded on the Sample Condition Form. The samples are then stored in the centralized walk-in refrigerator in the sample receipt area. The sample receipt area is located in the secure area of the laboratory. The samples are officially received and documented by the Sample Custodian or designee before the next business day. At times,samples will be sent to another lab for analysis not performed at MITKEM. These subcontracted analyses are performed by laboratories certified to perform the analyses. These samples are placed in bubble bags to prevent breakage and stored in a cooler in the walk-in or stored in the small refrigerator in Sample Receiving. The samples are either hand delivered to a local sub-contract lab or air courier with MITKEM chain-of-custody(Figure.8.4-5). 8.5 Sample Log-in Identification: 8.5.1 Sample Identification; To maintain sample identity,each sample received at MITKEM is assigned a unique sample identification(Sample ID)number. Samples are logged into MITKEM via the ChemWare Horizon Laboratory Information Management System(LIMS). After inspecting the samples,the Sample Custodian assigns each sample a MITKEM Sample ID Number. These Numbers are assigned sequentially in chronological order. MITKEM Sample Identification Numbers appear in the following format:Wxxxxyyy where:W—represents the current year with 6 for 1999 xxxx—represents a four digit project number which is assigned sequentially yyy—represents the sample number within the group or case. QA Plan Section No.8 rov.4 Date hdtiate&1/15/94 Date Revim 1/08/03 Pages of is For example,the fifth sample of the 20 case of 1999 would have the number:60020005 The M=M Sample ID Numbers are recorded on the Sample Login Form(Figure 8.4-2)for USEPA CLP samples and on the Sample Condition Form(Figure 8.4-3)for the other samples. Information on these forms cross-reference the Sample ID Numbers with SDG numbers, sample tag numbers and/or other client identifiers. Each sample is clearly labeled with its MITKEM Sample ID Number by the Sample Custodian. The same sample ID Number appears on the LIMS status report,on each sample preparation container and extract vial associated with the sample. 8.5.1.1 Sample Extract Identification: As desmbed in Section 8.5.1,a sample extract is identified with the same unique sample identification number as the sample from which it derives. In addition,it bears one of the following prefixes: For Organic Analyses: S for Sernivolatile Organics F for TPH EPH for Extractable Petroleum Hydrocarbons O&G for Oil and Grease H for Herbicides P for Pesticides B for PCBs P is also used for CLP analysis when Pesticide and PCB are analyzed as a single analysis. 8.5.2 Sample Login: Sample login system at MITKEM consists of computerized entry using ChemWare Horizon LIMS(Figure 8.5-1). The information recorded onto the Project Information Form includes: • Project number • Client name • QC requirements • Date of receipt • Date sample collected • Due date • Initials of the Sample Custodian and Project Manager • Comments • MITKEM Sample Identification numbers QA Plan Section No_8 M.4 Data]unwed:1/15/94 Date Revised:IM/03 Page 6 of IS • Client Sample Identification numbers • Sample matrix • Analyses required • Cost of analyses • Reporting requirements 8.5.3 Sample Information: After sample information is properly recorded(Sample Receipt Logbook, Sample Receipt Forms and Project Information Forms)and samples have properly been assigned Sample ID numbers and labeled,the Sample Custodian notifies the Project Manager or peer or supervisor. This person reviews all the information associated with the samples. He/she verifies (by dating and initialing)the correctness of the information on the Project Information Form. A project file is initiated by the Sample Custodian This file contains the original Sample Project Form,air bills, SMO traffic reports and all correspondence with the Client or SMO of others. Copies of the Project Information Forms are distributed to the various departments. 8.6 Sample Storage and Disposal: Samples at MITKEM are stored in a central storage facility. After sample receipt and login procedures are completed,the Sample Custodian places the samples in the centralized walk-in refrigerator. Volatile Organic sample aliquots are released to the volatile organic lab with documentation(Figure 8.6-1). The sample storage area is for samples only,no standards or reagents are to be stored there. Access to the centralized sample storage area is locked at all times. All sampletextract refrigerators are maintained at 40C f 2°C. Standards are kept in freezers maintained at -10 to-20°C. Temperatures are recorded every working day in the Temperature Log(Figure 8.6-2). . When analysis is complete, any remaining sample is retained in the central storage area until it may be removed for disposal(see SOP'G24 for Sample Disposal). Broken and damaged samples are promptly disposed of in a safe manner. Unless notified by the client,excess,unused sample aliquots are stored for at least 30 days after the submission of compliant data. The samples are then disposed after such period USEPA and NYS ASP extracts are stored for at least one year.After such time,the extracts are disposed of. All disposals are documented in a manner compliant with federal and state regulations. QA Plan Section No.8 ncv.4 Date Initiated I115/94 Date Revised:IM"3 8.6.1 Extract Transfer:. Pagel of 18 The extracts generated during the preparation for the organic analyses are transferred from the Organic Prep Lab to the Analysis Labs. The extracts, for Semivolatiles,TPH,Pesticides and PCBs,are checked in the Analysis Lab by entries in the appropriate Extract Transfer Logbook(Figures 8.6-3 and 8.6-4) 8.6.2 Extract Storage: Semivolatile,Pesticide/PCB,and TPH extracts,which are contained in crimp top vials or screw cap vials with Teflon lined septa,are stored at 4°C t 2°C. Semivolatile extracts are stored in R7. Pesticide/PCB and TPH extracts are stored in R5. They are catalogued numerically by project number that approximates chronological order,according to date of receipt. USEPA CLP extracts are stored separately from sample extracts of other clients. Excess Pesticide extracts,not analyzed,are stored in screw cap vials with Teflon lined septa in the Organic Prep Lab. In most instances;they consist of the remaining 8.5mL portions of aqueous and soil sample extracts and are chronologically ordered. 8.7 Sample Tracking: When a sample is removed from storage,the analyst who has custody signs the Sample Receipt Log. This information indicates the location of the sample at any point in time. Chain-of-custody of a sample ensures that the sample is traceable from when it was taken in the field through laboratory receipt,preparation,analysis and finally disposal. The primary chain-of-custody documents are used to locate a sample at any point in time. 1. The chain-of-custody form from the field describes the origin and transportation of a sample; 2. The laboratory Sample Receipt Log and supporting login records, documents acceptance of a sample by the Mitkem laboratory; and 3. The MITKEM Sample Receipt Logbook,documents which analyst has custody of the sample after removal from storage. QAPUn Section No.8 rw.4 Daze Initiated:1l15/94 Date Rovimd:IMM3 Page 8 of 18 Figure 8.4-1 Sample Receipt Tracking Logbook Form ce a o V I i u 6 �Yy t V N U �g 5�N�5 a i QA Plan SxtionNo.8 rev.4 Date laitiated:l/15/94 Date Revue&-1/08103 Page 10 of 18 Figure 8.4-2 USEPA CLP Sample Login Form t 1 i i SAMFLS LOG-IN SMET Lab Name 1 CdL rA i 1 Page _ of _ Received By (Print Name) Log-in Date Received By (Signature) Case Number Sample Delivery Group No. SM Number Remarks.(1)pJMW Sa ASS6Ci&4t.- Corresponding 5"'L 1 wraq -tom 1#X4- "s uubw*a with.Aia data �af(cGg Condiditicu of #EPA Sample Sample Tag Assigned Lab # SSaaople t, etc. Pae 1. Custody Seal(s) Present/Absent• Yntact/Broken 2. Custody Seal Nos. 3. Chaff Custody Present/Absent* rds 4. Traffic Reports Present/Absent* .or Packing Lists S. Ai.rbill Airbill/Sticker Present/Absent* b. Airbl.11 No. 7. Sample Tag$ Present/Absent* Sample Tag Listed/Not Listed on Chain- of-Custody S. Sample Condition Intadt/aroken*/ Leaking 9. Cooler Temperature 1O.Does information Yes/No* o . custody records, traffic reports, and Sample tags agree? li.Date Received at Lab 12.Time Received Sample Transfer Fraction 814A Peso �1 Fraction 1f0AL Area # Area # $y By 0a On * Contact SMO sad attach record of resolution Reviewed By Logbook No. Date Lagbook Page No_ FOR14 DC-1 OLM04.2 SAMPLB LdG-3I SNOT Lab Hams - Page_ of _ Received By (Print Name) .Log-in Date Received By (Signature) Case der sample Delivery group No. Client Number iUm W.lqoo*- PP E�SSOCigiEd Slt �'CLt(A�� f((4fLS ! P �g ks siub:nlifid �y:Fh-$ysL �Cc�C SPA saddle Assigned Remarks: Condition Sample # Tag # , Lab # Of Sample, . - Shipment, etc. 1. Custody Seals) Present/Absent• Intact/Hrolron - 2. Custody seal Nos. 3. Chain of Custody Present/Absent* Records 4-. Traffic Repdxts Present/Absent* or Packing Lists S. Airbill Airbill/Stkaker Present/Absent* 6. Airbill Na. 7. Sample Tags Present/Absent* Sample Tag Nos. Listed/Not Listed an Chain- Of-Custody S. Sample Condition Intact/Erokea*/ —" Leaking 9. Cooler Prevent/Absent* Temperature Eadicator Rottle 3.0. C001or Temperature 11. Does Yes/No* Information on custody records, traffic reports, and sample tags agree? 12. Date ,Received at Lab- 13. Time Received Sample Mnmsfar Practian + P•if VDA Area # Urea #VVk lob Sy BY On On * Contact SMD and attach record of resolution Reviewed By Logbook No, r Date Logbook Page No. FORM VC-1 OLC03.2 QA Plan Soation No.8 rev.4 Pate Initiat ed.1/15/94 Date RcdsW:WS/03 Page 11 of l8 Figure 8.4-3 Sample Condition Form MITKEM CORPORATION Sample Condition Form Page_of_ Received By: Reviewed By: date: MITKEM Pro ect Client Project Client Preservation(pH) VOA Condition: Lab Sample ID HNO3 H2SO4 HC1 Nao Matra 9)Custody Seal(s) Present 1 Absent Coolers / Bottles Intact I Broken Custody Seal Numbers 3)Chain-of-Custody Present / Absent 4)Airbill(s) Present I Absent Airbill Number($) 5)Cooler Temperature Coolant Condition 6)Sample Bottles Intact/Broker"king 7)Date Received B)Tlme Received �^ VOA Matrix Key: US=Unpresewed Soil A=Air UA=Unpresetved Aqueous H=HCI MIN=McOH&NaHSO4 E=Enure N=NaHSO4 M=McOH See Sample Condition Notification I Corrective Adon Form yes I no Comments I Remarks Red Ok yes I no I 1 i QA plan i Section No.8 rev-4 Date ba&ted:1/95/94 Date Revised:1/o8/03 Page l2 of 18 Figure 8.4-4 Sample Condition Notification Form 1 i i i i i i 1 z s i I 1 i i Sampie Condition Notification Mitkem Project#: Date of Receipt: Client: Received By: Client project#/name: Unusual Occurance Description: i Client Contacted: Contacted via: Phone/Fax/E-mall Date: Time: Contacted By: Name of person contacted: i Client Response: Responded via: Phone/Fax/E-mall Date: Name of person responding: Responding to: Mitkem Action Taken: I I 1 QA Plan Scotian Na 8 rev.4 Date Mat&1/15/94 Date Revised 1/09M a Pw 13 of 18 Figure 8.4-5 MITKEM Chain-of-custody Form 1 i 1 I 3 ( iI I i 1 I i l 1 i 1 o. 1 . a ' Q N Q I y t- a 1 Z r z m SHHNJVIXW do m O U a � )OHIO luos ft O N. VI.VMauswwoo \ � E e5 E 3 � Q v y f O I QA Plan Section Na 8 mv_4 Date lnitkW:1/15/94 Date Revised:W/03 Page 14 of l8 Figure 85-1 Project Information Form r F 1 I r 1 1 rig=8-5-1 Project Information Form 04 b �, - s a N � . N M - o QA Plan Section No_8 rev.4 Date Initiated:IA594 Date Revised:1M16f03 Page Isdis Figure 8.6-1 Volatile Organic Tracking Logbook Form i mo � a = a o _ m � � g z 0 O E IL 3 U l c in O oho i f 1 QA Plan Section No.8 ncv_4 Date Initiated 1/15m Mete Revisal IAD8103 Page 16 of 18 Figure 8.6-2 Temperature Logbook Form i i r 1 1 3 1 i I om o000 � e eeeo0�e o � a QA Plan SeedmWo.8 mv.4 Date Initiated:115/94 Date Revised:108103 Page 17 of t8 Figure 8.6-3 Extracts Transfer Logbook Form—Semivolatile Analysis mnlmM CORPORATION EXTRACT TRANSFER Ldcwo :SENWOLATILE ANALYSIS Date Traosf=cd RoinPrep Lab Lab ID TranaftrodBy Ra eivod By S Location comments i QAT40141 Page: Log ID:SV 12 Reviewed By: QA Plan Section No.8 rev.4 Date hdtiatai-1115/94 Date RRevise&1108103 Page 18 of 18 Figure 8.6-4 Extracts Transfer Logbook Form—Pesticide/PCB Analysis WKEM CORPORATION EXTRACTS TRANSFER LOGBOOK: PESTICIDES/PCB ANALYSIS Date Transferred Transferred Received Storage fr6m Prep Lab Lab ID by by Locafion Comments Log ID:8PS-21 i QAT00132 Revlswsd BY• Page: i I QA Plan Section No.9 rev.4 Date Initiated:V15/94 Date Revised 1109/03 Page 1 of 9 9.0 CALIBRATION PROCEDURES AND FREQUENCIES 9.1 Instruments: Specific calibration and check procedures are given in the analytical methods referenced in Section 10. The frequencies of calibration and the concentrations of calibration standards are determined by the cited methods and special contractual requirements. Standard calibration curves of signal response versus concentration are generated on each analytical instrument used for a project,prior to analysis of samples. A calibration curve of the appropriate linear range is established for each parameter that is included in the analytical procedure employed and is verified on a regular basis with check standards as specified in the appropriate CLP Protocols. For non CLP work,MIT"M adheres to the calibration criteria specified by SW-846 and/or Standard Methods for both organic and inorganic analyses. Where requested,other method specific calibration criteria are used. The following are examples of calibration procedures for various instrumental systems. Please refer to the Standard Operating Procedures for the specific calibration requirements. GC/ECD and GQJFID—An initial calibration is performed using five different concentration levels for each parameter of interest for SW-846 analyses. The initial calibration is done on each column and each instrument,and is repeated each time a new column is installed or whenever a major change is made to the chromatographic system. An initial calibration verification(ICV),near mid level concentration for all analytes,is performed immediately after the calibration. If the ICV does not meet method specific criteria,a new calibration curve is generated and an ICV is analyzed. If repeated ICV failures are encountered,the system is checked out to find the cause of these failures and the problem is corrected. A continuing calibration verification(CCV),near a mid-level concentration for all analytes,is run at ten(10)sample intervals. If CCV values are determined outside the upper limit of the method specified range and if no analytes were detected in the samples,the run will be accepted as valid and`No Detects' reported for the sample. If an analyte is detected and the CCV is out at the high end,the problem will be identified and corrected and the affected samples will be re-analyzed with a compliant CCV. If a CCV value is out of the method specified limits at the lower limit,the cause of the problem will be identified and corrected,and all samples affected by the out of control CCV will be rerun with a compliant CCV. QA Plan Section No.9 mv.4 Date Initiated-1/15/94 nwte Revise&MMI Page 2 of For CLP-type analyses,the continuing calibration takes place at the beginning of the analytical sequence and once every twelve(I2)hours throughout the analytical sequence. The percent difference in calibration factors for each standard must not exceed the criteria specified by the method. If a CCV fails to meet criteria limits,a new calibration curve will be generated and all samples affected will be re-analyzed. GUMS—For CLP methods,a minimum of five-level calibration(four-level for selected semivolatile compounds)is carried out for each analyte per system before analysis of samples take place. Continuing calibrations,near midpoint levels,are analyzed every twelve hours of instrument analysis time for CLP analyses. Re-calibration takes place whenever a major change occurs in the system,such as a column change in the GC or a source cleaning of the mass spectrometer or when the continuing calibration fails to meet method specific requirements. Tunes are performed once every twelve(12)hours. The GUMS system is tuned to USEPA specifications for bromofluorobenzene(BFB)or decafluorotripheaylphosphine(DFTPP)for volatile and semivolatile analyses, respectively. Verification of tuning criteria occurs every twelve hours of instrument run time for all CLP-type and SW846 analyses. More detailed instrument and method-specific calibration procedures and criteria are described in the individual analysis SOPs. ICAP—Instrument calibration,for each wavelength used,occurs at the start of each analysis. The calibration curve is constructed per method specification. An initial calibration verification and initial calibration blank(ICB)are analyzed before analysis of samples. If the ICV and ICB do not meet method specific criteria for an analyte,the analyte is re-analyzed with a new calibration. During the analysis, a continuing calibration verification(CCV)and continuing calibration blank(CCB)is analyzed at least every ten(10)samples. If either the CCV or CCB fails to meet method specific criteria for an analyte,the CCV and/or CCB are re-analyzed one time. If a failure still occurs,the analyte is re-analyzed with a new calibration. The CCV is obtained from a source independent from that of the standards. The CCV concentration for the different analytes are at method specified levels. 1 a i QA Pion Section&9 rev.4 Dato initiated:l/15/94 Date Revised:i/OM Page 3 of 9 The Flow Injection Mercury System(FIMS)-Instrument calibration occurs at the start of each analysis. The calibration curve is constructed per method specification. An initial calibration verification(ICV)and initial calibration blank(ICB) are analyzed before analysis of samples. If the ICV and ICB do not meet method specific criteria for Mercury,re-calibration and reanalysis are required. During the analysis,a continuing calibration verification(CCV)and continuing calibration blank(CCB)is analyzed at least every ten(10)samples. If either the CCV or CCB fails to meet method specific criteria for Mercury,the CCV and/or CCB are re-analyzed once. If a failure still occurs,re-calibration and reanalysis are required. The CCV is obtained from a source independent from that of the standards. The CCV concentration for Mercury is at method specified levels. Other instttimentation: pH-the meter is calibrated at three pH levels(4.0,7.0, and 10.0)before analyses of samples. Lachat 8000-automated flow-through spectrophotometer is calibrated per method specification before the analyses of samples. An initial calibration verification and initial calibration blank are analyzed before analysis of samples. If the ICV and ICB do not meet method specific criteria for an analyte,re-calibration must occur. During the analyses,a continuing calibration verification and continuing calibration blank is analyzed at least every ten(10)samples. If either the CCV or CCB fails to meet specified criteria for an analyte,the CCV and/or CCB are re- analyzed once. If failure still occurs,re-calibration and reanalysis must occur. The CCV is obtained from a source independent from that of the standards. The CV concentration for the different analytes are at method specified levels. Spectronic 20-manual spectrophotometer is calibrated per method specification. A calibration curve calibration verification is analyzed at the beginning,end,and at least every 10 samples. If the calibration verification does not meet method specific criteria for an analyte,it is re-analyzed once. If failure still occurs,a new calibration curve is established and any affected samples are reanalyzed. Balances-are calibrated once a year by an outside service. A calibration check is performed with NIST verified weights quarterly_.- QA Plan Section No.9 rev.4 Date Initiated.1/15194 Date Revised:1/08103 Page 4 of Class"S"weights are NIST certified by an outside certified service every 2 years. A verification check is performed with Class 3 weights each day. Class 3 weights are checked against the Class S weights on a quarterly basis. Thermometers are calibrated once a year against a NIST verified thermometer or as they are replaced The NIST thermometers are certified by an outside certified service annually. Gel Permeation Chromatography is used to clean samples according to CLP and client requirements. There are two GPC's in use. These are calibrated using a calibration standard provided by Ultra Scientific,Cat.#CLP-340. Once a successful calibration is achieved it is valid for a period of seven days. The organic preparation lab uses three maintenance logbooks with distinctive DYS. I Refrigerated Recirculator.QAT00211 GPC I : QAT00059 GPC 2 : QAT00185 9.2 Standards and Reagents. Standard reference materials used for routine calibration,calibration checks,and accuracy are obtained from commercial manufacturers. These reference materials are traceable to the source and readily compared to EPA references. Certain projects,especially those involving pesticide registration,may necessitate the use of reference standards supplied by the client. New standards are routinely validated against known standards that are traceable to EPA or NBS reference materials. Standards are dated upon arrival. Any material exceeding its shelf life as described by the methods in Section 10.0 is discarded and replaced. Standards are periodically analyzed for concentration changes and inspected for signs of deterioration such as color change and precipitate formation. Standards Receiving and Preparation Logbooks,which contain all pertinent information regarding the source and preparation of each analytical standard,are maintained by each of the MITKEM laboratory departments(Figures 9.2-1 to 9.2-4). Solvents are examined for purity prior to use to ensure there is no external source of contamination. See Mitkem analytical SOPS,sections 7 and 8 for standards preparation procedures. QA Plan j Sxtion No.9 rev_4 Date Initiated 1/15/94 Date Roby 11OM3 Pages of9 9.3 All purchased equipment,materials,and services must meet either specific method requirements,standard requirements,or project specific requirements. These requirements are documented in the individual analytical or project SOPS_ Reagents requirements are specified in the Mitkem SOP,Reagent Control,.SOP #G14.The equipment requirements are specified in the individual methods and sops. QA Plan Seddon No.9rev.4 Fate Initiated-1/15/94 Date Revised:IM/03 Page6 of 9 Figure 9.2-1 Metals Primary Standard Receipt Logbook—Instrument Laboratory 0 f m Z uj U U 2 ! O $m O J F- WWW @ m DC m N � a J � A_ Z 0 O y O IL w O 0 Wm QA Elan Secdon No.9 rev.4 Date Initiated 1/15/94 Date Revised 1/0"3 Page 7 of 9 Figure 91-2 Semivolatile Primary Standard Logbook—Preparation Laboratory i I i o cd � a a I � a I Ao 1 �a I J 0 i o � � z • � U E � f 04 I OZ R r i a 1 QA Plan Sec&m Na 9 rev.4 Date laifiuwE 1/1&94 Date RoviA-1/0"3 Figure 9.2-3 Pagc 8 of 9 Pesticide/PCB Working Standard Logbook—Preparation Laboratory i I i I I A A O CC d v a S d U . 0 V a .r p� 0 H UU a w a QA Plan Section Na 9 nev.4 Date Initiate.&V 15N4 Date Revisd 1/08/03 Page 9 of 9 ' Figure 9.24 1 Reagent Preparation Logbook—Preparation Laboratory , i i I i c a Y O c � � L m CL U Ic LL O 9 E O co c �E 'S O E ti 10 Q T c' • c�m i QA Plan Sectim%.10 mv.4 Date Wfiged:1/15/94 Date Rvdocd 1/06/03 Page 1 of i t 10.0 ANALYTICAL PROCEDURES MTTKEM uses the methods specified in Tables 10-1 through 10-6 unless otherwise specified by the client. I i 1 . , i I i f QA Plan Saxioa No. 10 my.4 Date Initiated:1115M Date Revised:1106/03 Paget of 11 !, Table 1Q-1 Potable Water Analytical Methods Parameter Method Des��i Method Reference Metals ICAP Analysis* 200.7 Aluminum Barium, Chromium,Cobalt,Copper,Iron, Manganese,Molybdenum, Nickel,Silver,Silver, Vanadium,Zinc Mercury Cold Vapor Analysis 245.1 Residual Chlorine Spectrophotomehic SM4500-Cl G Tnhalomethanes Purge&Trap 524.2 GUMS Analysis Volatile Organic Compounds Purge&Trap 524.2 GUMS Analysis 1,2-Dibromo-3-chloropropane Micro extraction 504.1 1,2-Dibromemethane GCIECD Analysis , i , *Please note;Antimony,Arsenic,Beryllium,Cadmium,Lead,Selenium,and Thallium I analyses in potable water are subcontracted to a Drinking Water certified laboratory.Mitkem is not certified for Graphite Furnace Atomic Absorption(GFAA)analysis for these auslytes. 1 QAP1an Section No.10 rev.4 Date hitiakd: 1/15/44 Date Revised: 1106M Page 3 of 11 Table 10-2 Non-potable Water Priority Pollutant Analytical Methods Parameter Method Description Method Reference Metals ICP 6010B Al mmum Antimony,Arsenic, Barium,Beryllium,Cadmium, Chromium,Cobalt,Copper,Iron, Lead,Manganese,Molybdenum, Nickel,Selenium,Silver, Silver,Thallium, Vanadium,Zinc Mercury Cold Vapor 7470A,7471A Alkalinity Titration SM2320 Chloride Titration SM4500-Cl B PH Electrode SM4500 H+B Sulfate Spectrophotometric SM4500-SO4 E Ammonia Distiilation/Nesslerization SM4500 NH3 B Nitrate Autoanalyzer EPA 353.2 Nitrite Colorimetric SM4500-NO2 B Orthophosphate Ascorbic,Manual SM4500-P E Total phosphate Persuifate,Manual SM4500-P B3 &E Chemical Oxygen Demand Spectrophotometric SM5220-C,D Total Organic Carbon Combustion 415.1 Phenolics Distillation,Color, SM5530 B Automated Total Dissolved Solids Gravimetric SM2540 C Total Solids Gravimetric SM2540 B Total Suspended Solids Gravimetric SM2540 D QA Pbn Section No.10 tov.4 Date Initiated_1/1-"4 Date Revised:L%M Table 10-2 Page 4 of 11 Non-potable Water Priority Pollutant Analytical Methods(can't) Parameter Method description Method Reference Total Settleable Solids Imhoff cones SM2540 F Volatile Organics Halocarbons Purge&Trap,GC/MS 624 Aromatics Purge&Trap,GC/MS 624 Semivolatile Organics Extraction GUMS 625 Organochlorine Pesticides/ Extraction,GC/ECD 608 PCBs Oil&Grease Extraction, Gravimetric 1664 QA P1w SectimNo.10 rm 4 Date bft4tcxk 1115194 Data Revised:1106N.3 Page 5 of 1 i i Table 10-3 SW-846 Inorganic Analytical Methods { Parameter Method Description Method Reference Metals Aqueous Acid digestion Method 3005A/3010A ICAP analysis Method 6010B Solid Acid digestion Method 3050A ICAP analysis Method 6010B Mercury Aqueous Permanganate digestion Method 7470A j Cold Vapor analysis Solid Permanganate digestion Method 7471A Cold Vapor analysis Hexavalent Chromium Aqueous Diphenyl Carbazide SM 3500Cr B Colorimetric Solid Acid Digestion Method,3060A,7196A Colormetric Cyanide Aqueous Midi-distillation Method 9012B Automated Solid Midi-distillation Method 9012B Automated PH Solid Electrode Method 9045C Ignitability(Flashpoint) Aqueous Pensky-Martens closed cup Method 1010 Solid Pensky-Martens closed cup Method 1010 Mod. Reactive Cyanide Solid Distillation 7.3.3.2 Automated Reactive Sulfide Solid Colorimetric 7.3.3.4 QA P1aa Section No.10 m.4 [batetnitiatod:JtjY% Date Revised:1"W Table 10-3 Page 6 of 11 SW 846 Inorganic Analytical Methods(con't) Paramcter Method Description Method Reference Toxicity Characteristic Leaching Procedure(TCLP) Aqueous Leachate Generation Method 1311 Solid Leachate Generation Method 1311 Synthetic Precipitation Leaching Procedure(SPLP) Aqueous Leachate Generation Method 1312 Solid Leachate Generation Method 1312 t • QA Plan Section No_Wrev.4 Date Iabled:III 5N4 Date Raised, 1/06/03 Pagc 7 of 1 I Table 10-4 SW-846 Organic Analytical Methods Parameter Sample Preparation Sample Analysis Volatile Organic Compounds 1 Aqueous Method 5030 Method 8260B Solid Method 5030 Method 8260B Method 5035 f Volatile Organic Compounds(Aromatic+Methyl t-butyl ether(MTBE)) Aqueous Method 5030 Method 8021B Solid Method 5030 Method 8021B Semivolatile Organic Compounds Aqueous Method 3510C Method 8270C Method 3520C Solid Method 3540C Method 8270C !, Method 3550B Method 3545 Organochlorine Pesticides Aqueous Method 3510C Method 8081A Method 3520C Solid Method 3540C Method 8081A Method 3550B Method 3545 Polychlorinated Biphenyls (Aroclors and Congeners) Aqueous Method 3510C Method 8082 Method 3520C Solid Method 3540C Method 8082 Method 3550B Method 3545 Total Petroleum Hydrocarbons Aqueous Method 3510C Method 8015M Method 3520C Solid Method 3540C Method 8015M Method 3550B,Method 3545 QA Plan Section Na 10 rev.4 Date Initiated.1115/44 Date Revisal_1/06M Paps of I 1 Table 10-4 SW-846 Organic Analytical Methods(con't) Parameter Sample PlOgMtion Sample Analysis Herbicides Aqueous Method 8151 A Method 8151 A Solid Method 8151A Method 8151A Toxicity Characteristic Leaching Procedure(TCLP) Aqueous Method 1311 Solid Method 1311 Synthetic Precipitation Leaching Procedure(SPLP) Aqueous Method 1312 Solid Method 1312 Gel Permeation Chromatography(GPC) Aqueous Method 3640A Solid . Method 3640A Florisil Cleanup Aqueous Method 3620B Solid Method 3620B Silica Gel Cleanup Aqueous Method 3630C Solid Method 3630C Sulfur Cleanup Aqueous Method 3660B Solid Method 3660B Sulfuric Acid Cleanup Aqueous Method 3665A Solid Method 3665A QA Plan Section No.10 m.4 Date Initiated:1/15M Date Revised:1/0"3 Table 10-5 Page9ofII CLP Type Analytical.Methods Parameter Method Reference USEPA CLP Organics OLM04.2 USEPA CLP Inorganics ILM04.1 USEPA Low Level Organics OLCO2.1/03.2 NYS-ASP CLP Organics ASP 1995/2000 SOw NYS-ASP CLP Organics ASP 1995/2000 SOW 11 QA Plan Section No.10 rev.4 Date]Diluted 1115r94 We Revised 1/06M Table 10-6 Page 10 of 1 I Other Analytical Methods I Parameter Methcxd Reference Volatile Petroleum Hydrocarbons Aqueous MADEP VPH 98-1 Solid MADEP VPH 98-1 Extractable Petroleum Hydrocarbons Aqueous MADEP EPH 98-1 Solid MADEP EPH 98-1 i New York State Total Petroleum Hydrocarbon Solid 310.13 Extractable Total Petroleum Hydrocarbons l Aqueous CT ETPH 99-3 i Solid Cr ETPH 99-3 r QA Plan 1 Section No.10 mv.4 Date Inidatad_I&W4 Date Revised:L06/03 Page 11 of 11 10.1 Analytical References 1. Analysis of Extractable Total Petroleum Hydrocarbons(ETPH)Using Methylene Chloride Gas Chromatograph/Flame Ionization Detection, Environmental Research Institute,University of Connecticut,March,1999 2. Analytical Services Protocol,Volume 1-8,New York State Department of Environmental Conservation,September, 1989. " 3. Annual Book ofASTM Standards. Part 31-Water. American Society for i Testing and Materials,Philadelphia,PA, 1981. - i 4. Chemical Characteristics of Marine Samples,API Publications No.4307, API,Washington,D.C. 5. Federal Register.Vol. 55,No. 61,March 29, 1990 6. Methods for Chemical Analysis of Water and Wastes,EPA-600/4-79-020, 3/83 Revision. 7. The EPA 600 Series. Methods for Organic Chemical Analysis of Municipal and Industrial Wastewater-,Appendix A,40 CFR Part 136,Federal Register, Vol.49,No.209, 1984. 8. Methods of Soil Analysis. Part 2,Chemical and Microbiological Properties, Second Edition,American Society of Agronomy,Inc.,Soil Science Society of America,Inc.,Madison, WI, 1982. 9. Standard Methods for the Examination of Water and Wastewater, 181h Edition,APHA,Washington,D.C., 1992. 10. Test Methods for Evaluating Solid Waste-Physical/Chemical Methods,SW- 846,P Edition Update III. Office of Solid Waste and Emergency Response, USEPA,Washington,D.C., 1996. It. USEPA Contract Laboratory Program. Statement of Work for Organic Analysis,USEPA,OLM04.2 and OLC03.2. 12. USEPA Contract Laboratory Program. Statement of Work for Inorganic Anaaysis,USEPA, ILM04.1. 1 i QA Plan Section No.11 rev.4 Date Initiated:1/15/94 Date Revised:1/08103 Page l of 13 11.0 DATA REDUCTION,VALIDATION AND REPORTING 11.1 Data Reduction: Instrument print-outs,computer terminal displays,chromatograms,strip chart recordings and physical measurements provide raw data that are reduced to concentrations of analytes through the application of the appropriate calculations. j Equations are generally given within the analytical methods referenced in Section 10. Data reduction maybe performed automatically by cotnputerized data systems on the instrument,manually by the analyst,or by PCs using spreadsheet and/or data base software. This software includes Thru-Put's `TARGET' for the analyses of organic analytes and Ward Scientific `EDR'for metals,cyanide and mercury analysis. 11.2 Data Validation: Data validation is an essential element of the QA evaluation system. Validation is the process of data review and subsequent acceptance or rejection based on established criteria. The following analytical criteria are employed by MITKEM in the technical evaluation of data: • Accuracy requirements. • Precision requirements. • Detection limit requirements. • Documentation requirements. As in the case of EPA/CLP procedures,data acceptance limits may be defined within the method. As one means of tracking data acceptability,quality control charts will be plotted for specific parameters determined in similar,homogeneous matrices. Control limits for non-CLP methods are statistically determined as analytical results are accumulated. Upon completion of the evaluation,the evaluator dates and initials the data review checklist as described in Section 11.5 below. 11.3 Data Verification: The verification process requires the following checks to be made on data packages before they are submitted to the client: QA Plan Section No.I I rev.4 Date MitWe&1/15194 Date Revin&1/09M Page 2 of 13 • A completeness inspection is required which ensures that all required data are included in the data packages submitted to the client and that the appropriate signatures are present on the data packages. • A contract compliance screening to ensure that contractual requirements have been satisfied. • A consistency check to ensure that nominally identical or similar data appearing in different places within a data package are consistent with respect to value and units. • A correctness check to ensure that reported data have been calculated correctly or transcribed correctly. 11.4 Data Interpretation and Reporting: Interpretation of raw data and calculation of results are performed by a scientist experienced in the analytical methodology. Upon completion of data reduction, the scientist signs for the reported results on the data review checklist. The laboratory supervisor or other senior staff,is responsible for the data generated in that department,performs an independent review of data and completed report forms. Members of the QA staff also check the results on selected sets of data(usually 10%). 11.4.1 Report Formats: Two types of data reports are generated at Mitkem:"commercial-format' data reports and CLP-format data reports. Commercial data reports are generated using MS EXCEL. All the pertinent client information and the analysis results are entered manually. The draft report is subjected to a 100°/a technical and completeness review before it is printed out in its final form. CLP data reports are generated using specialized software(Ttuu Put TARGET for organic analyses and Ward Scientific EDR for inorganic analysis). These reports also undergo a 100%review before they are generated in their final form. Records are maintained for all data,even those results that are rejected as invalid. i I _ 1 - QA elan Section No.I1 vev.4 Date Initiated:I/15/94 Date Revised:1/osro3 11.4.2 Data Reporting for Massachusetts Drinking Water Samples: Page 3 of 13 Drinking water data reports generated for clients in the State of Massachusetts need to be reported on state forms. These reports are sent to the client. The client is responsible for forwarding copies of the report to the regional DEP Offices and local officials. 11.5 Levels of Data Review: MiTKEM employs five(5)levels of data review. These are based on requirements outlined in several government and other environmental analysis programs including the U.S.Army Corps of Engineers,Air Force Center for Environmental Excellence(AFCEE),Naval Facilities Engineering Service Center (NFESC),HAZWRAP,EPA Contract Laboratory Program(CLP),as well as commercial engineering firm programs. The data review and evaluation process is structured to insure that all data reported to customers has been thoroughly reviewed and approved using a mWti- step process designed to identify and correct any error. At any step in the data evaluation and review process,the reviewer has the responsibility and authority to return any data not meeting requirements back to'the previous step for re-analysis or correction. No reports are released to the client as final data without successfully passing through each step in the data evaluation and review process. Any data released prior to the completion of the fill.review process are released with the statement that the data is preliminary pending final review. The five levels of data review are as-follows: 11.5.1 Level 1: A Level 1 review is performed by the analyst or a qualified peer analyst within the analytical laboratory section that produced the results. Level 1 review is comprehensive,evaluating 100%of the data for compliance with SOP and method requirements,as well as project-specific requirements. The analyst/peer reviews the data set to insure that sample preparation and analysis data are correct and complete. A checklist(Figures 11.5-1, 11.5- 2 and 11.5-3)is used to document that Level 1 review has been completed for each data set produced. The specific items reviewed may vary by method,but generally include the items listed below: All manual calculations or data entry steps 0 Use of proper significant figures and rounding QAPiaa Section No.I tev.4 Date laiatc&1/1-"4 Date Revised•i/OW3 Page 4 of 13 • That results are compliant with precision and accuracy requirements through evaluation of calibration,blank,LCS,spike,duplicate and/or duplicate spike QC results • An evaluation of analysis dates in comparison to holding times • That all analytes are within the calibration range of the test,and any necessary dilutions have been performed • That data are complete;that every sample for a work order or Sample Delivery Group(SDG)that requires this test has been analyzed. • That spectral identification for target analytes or tentatively identified compounds is correct. • Spot-check computer calculations to insure they are being performed correctly. • That any deviations from the SOP,method,or project-specific requirements,or any unusual occurrences during analysis are described for inclusion in the report narrative. 11.5.2 Level 2: Level 2 review is a technical review performed by the supervisor of the analytical laboratory section producing the data,another senior chemist experienced in the particular analysis,or other senior laboratory management,such as the Technical Director,Operations Manager,or QA Director. The samf,individual may not perform Level and Level 2 review on the same data set. Level 2 review is performed on 1001/0 of the data generated. This review maybe less comprehensive that Level 1 review in that it is designed to insure that the Level 1 review was completed for each data set produced. All items listed under Level 1 review above may be checked,with particular focus on the following. • That all project-specific criteria have been met • That result flags have been properly applied for any dilutions, calibration failures,blank contamination,etc • That the results are reasonable when compared to historic or on-going data for this program or for this analysis in general • Spot checks of manual calculations or data entry steps I QAPIan section Na 11 mv.4 Date lnitiab 11IS/94 Date Revised 1/09/03 Page 5 of 13 • Review the use of significant figures and rounding • That results are compliant with precision and accuracy requirements j through evaluation of performance indicators such as blanks, LCS, surrogate and matrix spikes or duplicate QC results I • Spot check of spectral identifications for target analytes or tentatively identified compounds • That any notations regarding deviations from SOP,method or project specific requirements,or any unusual occurrences are properly described for inclusion in the report narrative,and to add review comments as necessary. 11.5.3 Level 3: Level 3 review is an administrative or non-technical review.A level 3 review is evaluated by the report group coordinator,document control specialist,project manager,or other personnel in the data report group. The same person may not both enter the data and review the data entry. 100%of the data manually entered into the commercial data reporting system are reviewed to insure there are no data entry errors. All manual data entry steps used to produce electronic deliverables are also checked. Data reported using MITKEM's commercial data reporting system are evaluated somewhat differently from those produced using the CLP-type data reporting system,based on the different potential sources of error in these systems. The data review checklist is used to document Level 3 review has been completed on each data set. Additional forms are also used for CLP and CLP-type data assembly and review. The following items are checked during Level 3 review: • All typographical data entry into commercial data reporting templates • The client sample identifications are listed correctly for every sample • The completeness of the data report;that every analysis on the login sheet has been accounted for in the final report • That results and units are consistent throughout the data set • That any special requests or other notes on the login sheet have been addressed 0 QA Plan Section No.11 tay.4 Date laidstW:111"4 Date Revift&VM3 Page 6 of 13 • That a description of any flags and data qualifiers is included in the data report. The review of all sample login and chain of custody information is also included in Level 3 review. The review is evaluated by the project manager immediately following receipt of the samples and production of login paperwork. This review is documented by initialing on the appropriate line on the M nXEM sample login sheet. 11.5.4 Level 4: Level 4 review consists of the final management approval for the entire data report. Level 4 review is evaluated by senior laboratory management personnel,such as the Technical Director,Operations Manager,QA Director,Organics or Inorganics Laboratory Manager or Project Manager. This review and sign-off constitutes MITKEM's approval to release the final data report to the client. The signature on the report narrative documents that Level 4 data review has been completed on the entire data report Level 4 data review consists of • That any deviations from method or SOP requirements have been documented and explained such that they will be clear and understandable to the client • That all unusual occurrences have been clearly described in the report narrative • That any special analytical requests made by the client have been addressed and adequately recorded in the report • That the analytical report meets the goals of the testing program • That the data are reasonable from an overall perspective,for example, that hexavalent chromium does not exceed total chromium,or that dissolved metals do not exceed total metal concentrations. • That the final report format and appearance are professional and consistent with MITKEM's practice. 11.5.5 Level 5: The fifth level of data review is performed by the QA/QC Director or his designee on a subset of all data produced by the laboratory. QA review is performed on approximately 10%of all data reports generated by the laboratory,with results from each analytical section being represented. QA Plan section No.I I rev.4 Date hii"ed.1/15M Data RovW&Y08103 Page 7 of 13 Level 5/QA Review usually takes place following release of the data report to the client. During Level 5 review,reports are evaluated to check the proper functioning of the entire data acquisition,reduction,evaluation and reporting process. This is accomplished through spot checks and detailed calculation reviews of various steps in the analysis and data reporting process. The specific items checked are at the discretion of the QA/QC Director. Level 5 review functions as an additional check that the laboratory's QA systems are operating properly. Any deficiencies encountered during Level 5 reviews are promptly reported to MITKEM senior management. Flow charts of the data review process follow in Figure 11.5-4. 11.6 Document Control: All login sheets,Chains-of-Custody(COC)and Sample Condition Forms(SCF) I and other sample transmittal documentation are generated in Sample Receiving. A red Project File is initiated to contain all project-specific hard copy documents. Samples are signed in/out of the sample receiving area by analysts. In the Prep lab,samples and all pertinent information is recorded into logbooks. Once samples are moved to the instrument lab,the transfer of extracts is documented in the transfer logbook. I In the instrument lab,the analysis of extracts is recorded in the instrument run log. All analysis data,including ICAL,CAL and raw data are acquired using computer-controlled instruments, and stored on the hard drive of the computer performing data acquisition. Data are automatically copied to the company file server after acquisition. Organics analysis data are processed using Thru-Put Systems' Target software. This system creates a folder on the file server for each analysis fraction'for each work order or SDG. This folder contains raw data, processed analysis results,instrument tune,initial calibration and continuing calibration results as well as a copy of the data processing method used. This allows for long-term archiving and complete reconstruction,of the data at any time in the future. Data reporting forms and raw data are printed and arranged with all appropriate sample-preparation logbook page copies for technical review. Inorganic data files are copied to the hard drive of a local computer for processing using Ward Scientific EDR software. The data are assembled into a Sample Delivery Group and reporting forms are printed. The original instrument data files and the processed SDG are then copied to the file server for archiving. Hard copy printouts for reporting forms,instrument data hardcopy output and all associated preparation logbook page copies are assembled for technical data review. The company file server consists of two separate computers,each with an array of multiple hard disk drives,that are continuously mirrored,such that the failure of J QA Plan Section No.11 rev.4 Date Initiate&1/15M Date Revised:i/0N3 any single component or computer will not impact the operation of the systeem,or3 the ability to recover data. All new files or data are copied to magnetic tape on a daily basis. On a monthly basis full system back-up to tape is performed. Following technical review,and generation of the report narrative results go into the project file in data reporting. The original copy of the report is sent to the client. The report is also scanned into an optical file database for long-term archiving. As documents are scanned into the database they are recorded for Permanent storage on CD-ROM disks. Mitkem's system includes a`Jukebox"to provide access to numerous CD-ROMS on an as-needed basis.All other information associated with the report,including data review check-lists are kept in the red project file. The project files are kept onsite in a storage area for j approximately 6 months. The files are then shipped to an offsite storage area where they will remain for a total of 7 years. After this time,the files will be destroyed. 11.6.1 Logbooks: All logbooks are issued and controlled by the QA Department. When logbooks are complete, the QA Department archives them in order of control number for a minimum of ten(10)years.All controlled documents including SOPS,QA Manuals, Logbooks,etc.are dated.This is the date the document is controlled and will stay in force until the next official/controlled update. The logbooks are stored in an on-site storage facility for a minimum of 6 months and then boxed and stored in a locked off-site storage facility. 11.6.2 Project/Data Files: MITKEM is a secured, limited access building. The doors are secured with a keypad entry system. All hard copy information pertaining to the analysis of samples is maintained and stored in a project file folder. This information includes all login sheets,COC, SCF,bench sheets and analytical data. Electronic data are also stored by laboratory project number on the company file server,and in the optical file database of completed reports. File folders containing all hard copy data and other project information are stored in an off-site storage facility for a total of 7 years. The off-site storage facility is a locked storage area. Access is limited to the CFO or his designee and request to retrieve a file will be made to this person. In the event Mitkem Corporation changes ownership,the maintenance, control,storage and eventual disposal at the end of the appropriate time period,of all records,including client data and QAIQC files,will transfer to the new owners. QA Plan SwAian No.11 mv.4 Date lnidut41/15/94 Daft Revised L10"3 Pop 9 of 13 In the event Mitkem Corporation decides to cease operations,clients will be notified prior to the cessation of operations and their files/records will be made available to them.Within a designated time period after notification,the client will be responsible for taking custody and the future maintenance of their records.If the client determines they do not want to maintain the records,these will be disposed of properly. i 11.6.3 Standard Operating Procedures(SOPS): SOPs are prepared by the Lab Supervisor in conjunction with the QA/QC Director,reviewed and approved by the Lab Supervisor/Manager, Operations Manager and QA/QC Director and distributed as controlled documents by the QA/QC Director. All SOPs are reviewed and updated as necessary on an annual basis. The procedure for preparing,reviewing, approving,revising and distributing SOPS are described in SOP No.Q0L 11.6.4 Method Updates: It is the laboratory's policy to implement new revisions of frequently used methods within six months of the date the method revision is promulgated. The QA/QC Director and Technical Director make the final decision on when a method revision will be adopted by the laboratory. When the laboratory is in the middle of a client's sampling project,the lab will continue using the same revision for the entire sampling event unless advised otherwise by the client. Consequently,once the laboratory has formally adopted a new method revision,both the old and new revision may be in use at the same time,depending on the project. 1 I QA Plan Section No.It riw.4 Date lnitiatiA-VI5194 Date Rcvisai-1/0&'03 Page 10 of 13 Figure 11.5-1 Commercial Data Review Checklist I i u i 1 I I i QA Plan Section No.[I rev.4 Date Udatad:l/15/94 Bate Revisal:VOW Page t1 of 13 Figure 11.5-2 CLP and CLP-type Data Review Checklist—Organics i i 0 0 i 0 0 1 o ip DoftBavisod:3nIW Mitkem Corporation CLP/CLP-like Deliverable Review Check List for Organics Annlysls Project Number: — Analysis: Fraction: Target Category:_ (ASP only) Analyst: Data Pack.Assembly. Data Pack.Review: Correction by Analyst: Client:— An st Date: Reviewer Date: Items Pages OK/UnusualObswvation Check Commets SDG Summer Sheet &&me SummNy Sheet -- Extraction Bench % Solid Bench Sheet Extract Transfer Instrument Run Log _ gPC Run Log Internal Sample Tr ddag Loa Client IDs OK/UnusualObservation Check Comments Holding Time umo ate Initial Analysis at DilutiQ� _ -- SMples "DL"Samples _ - MS/MSD Samples . 0 ample et # OK/[JnasualObservation Cheek Comments Blank LCS _ Tune Initial Calibration Con' ' g Calibration - Intemal Standard Area Note: Yes No Client lD_Check ID Truncation Special Remit QAT00201 Page 1 of I QA P1an Section No.I rcv.4 Date Mitim d:1/1SM Date Revised:I W3 Page 12 of 13 Figure 11.5-3 CLP and CLP-type Data Review Checklist—Inorganics I f 1 i I I i P O i l MITKEM CORPORATION. CLP/CLP-like Deliverable Check List for Inorganic Analysis Project Number:—. Analysis:__ Client _ Category. (ASP onivl Input by/date Reviewer Forms generated on/date: (1) Data Reviewed: (2) Date Reviewed Corrections by:_ Elenwts Required: AI ISb lAs 18a 113e I lGa ICr 1co leu We IPb IM9 IMn IN IK ISe IAg INa 171 IV IZn ISn CN H f M I E. Checic OK/Unusuat Observation ! Sample Log-In Sheet Prep Log Sheet(AQ/SL) %Solid Bench Sheet Tumbling Log(TCLP/SPLP) Check Lab ID OK/Unusual ObservatlortlDevtatioNFlaas ICV/CCV Spiked Samples(N) - Duplicate Samples Serial Dilutions(E) Blanks LCS ICP Interference _ CRA/CRI Yes NQ Prep/Analysis Notes: Client ID Check: ID Truncation: Special Request: QAT00203 REVISED 3/7/00 e QA Plan Section No.It iev.4 EWo Initiated:1/15194 Date Revis d:1/0&/03 PW 13 of 13 Figure 11.5-4 Data Review Flow Diagram 1 I MITKEM CORPORATION Review Process Flow Diagram Sam le is Level 1 Review 10096 data and 'C Acceptable Analyst Recalculates Precision,Accuracy, 10 No l- or Reanalyzes &Com leteness Sam les Ye Level 2 Review Acceptable Precision,Accuracy, No &Completeness yes Data Reporting enters data into final re forms Level 3 Review t Data Acce table 0 No Entry Corrected YO_ Level 4 Review 62MLable --!•No ► 10 Yes Issue final report to Client r i QA Plan Section No.12 mv_4 Date Initiated.1/15/'94 Date Revisa&YOV03 Page 1 of 6 12.0 LABORATORY QUALITY CONTROL CHECKS MTTKEM analytical procedures are based on sound quality control methodology,which derives from three primary sources: 1. Specific EPA and other approved analytical methods,and 2. "Handbook for Analytical Quality Control in Water and Wastewater Laboratories"(EPA 600/4-79-019). 3. Standards for Good Laboratory Practice. In the application of established analytical procedures MITKEM employs,at a minimum, I the QC protocols described in the references found in the Analytical Methods section of this document. Specific projects may require additional quality control measures,due to such factors as difficult sample matrices or use of innovative techniques. For those projects MITKEM will recommend and implement,subject to client approval,QC measures to produce data of known quality. Each of the MITKEM laboratory departments have an individual QC program,which includes,but is not limited to,the practices described below. 12.1 Detection Limit Determination/Verification: Detection Limits are developed annually for all inorganic and organic target compounds. 12.2 Personnel Training: Chemists who begin their employment at MITKEM are first instructed under the MITKEM Safety Training Program. Before performing and analyses,a chemist is required to read the appropriate protocols and SOPS. Helshe must become familiar with the laboratory equipment and the analytical methods. The chemists begin a training period during which they work under strict supervision. Independent work is only permitted after the chemist successfully completes a proficiency review. Copies of results,if any,of training sessions and training course documentation will be placed in the employee's training file archived by the QA Director. 12.3 Control Charts: I i QA Plan Swtion No.12 m.4 We Initiated:1/15194 Date RavhW:1ANM Page 2 of b For organic and inorganic analyses,the recoveries of analyses in the lab control samples are plotted on control charts. These charts are used to establish control and warning limits. 12.3.1 Control limits are calculated and updated at least annually from the GCS, MS/MSD,and Surrogate data points for each analyte and matrix using the following equations: n Xt Average(x}= F=1 n n 2 I(xr—x) SD n-1 where: SD=Standard Deviation N=number of data points 0 Warning Limits=Average t 2 * SD Control Limits=Average t 3 *SD 12.3.2 Control limits must be approved by the QA/QC Director and by the Technical Director prior to adoption by the laboratory. In the event that limits are wider than method recommended limits,the method recommended limits may be adopted and the analytical procedure will be re-evaluated to determine possible causes. Additionally,in the event that control limits are tighter than 10%from the average,the lab may adopt a control limit of t10%from the average. QA Plan Section Na 12 rev.4 Date lnitiata-1/15/94 Date Revised 110W3 hge3of6 12.3.3 Control charts are plotted in EXCEL using the template in the QA Department directory:/Control Charts/Control Chart Template.xls. Data from each laboratory is downloaded into an EXCEL spreadsheet. The compounds,recoveries,and date analyzed for each file is copied into page one of the Control Chart Template. The data for each analyte is then automatically read into another page of the spreadsheet(one page for each analyte)and plotted onto a control chart. Control charts are generated for each analyte in the inorganic metals(to include cyanide)section,and for a representative sampling of analytes in the organic sections. Each control chart is then printed for review by the QA/QC Director and by the Lab Supervisor/Manager. Out of control situations noted on the control chart are brought to the attention of the Technical Director by the QA/QC Director. An example control chart is presented as Figure 12.3-1. LCS data must be reviewed and evaluated daily against the Control Limits to establish that the system is in control. 12.3.4 The following situations constitute an out of control situation on a control chart: • One data point above or below the Control Limit line. • Two consecutive data points above or below the Warning Limit line_ • Six or more consecutive data points above the Average Line or six or more consecutive data points below the Average Line. This situation suggests a trend and suggests the procedure has been changed in some way(for better or worse). The cause for this trend must be investigated. 12.4 .General QC Protocols: Organics Laboratory: • Trip blanks and holding blanks,when applicable,are analyzed to detect contamination during sample shipping,handling and storage. • Method blanks,at a minimum of one in every 20 samples,are analyzed to detect contamination during analysis. • Volatile organic method blanks are analyzed once during each analytical sequence. QA Plan Section No.12 m.4 Date Initiated:1/1S1% Date Revise&W8/03 Page 4 of6 • One blank spike(Laboratory Control Sample or LCS)consisting of an analytical sample of laboratory water or Ottawa sand with every batch of 20 or fewer samples,is analyzed to determine accuracy. • Sample spikes and spike duplicates,as requisitioned,are analyzed to determine accuracy and the presence of matrix effects.The Relative Percent Difference(RPD)is also determined for matrix spike/matrix spike duplicates to measure precision.The criteria followed are stated in the individual methods. For batches without a sample duplicate(for example,if insufficient sample volume is provided),a duplicate blank spike(LCS)is performed to provide for precision measurement. • Performance evaluation samples from EPA and state agencies are analyzed to verify continuing compliance with EPA QA/QC standards. • Surrogate standards are added to samples and calculations of surrogate recoveries are performed to determine matrix effect. • Internal standards for GC/MS analysis are added to sample extracts to account for sample-to-sample variation. • GC analysis of EPA traceable standards to verify worming standard accuracy and instrument performance. • Initial multi-level calibrations are performed to establish calibration curves. • Instrument calibration is established or verified with every analytical sequence. • Tuning of GUMS systems once every 12 hours for CLP and SW-846 methods or 24 hours for methods 624/625 to method specifications is implemented for consistency in data generation. When QC limits are not met during an analytical run,the source of the problem must be investigated. Following an evaluation of the data,those samples affected must be re-analyzed after the problem has been solved. If QC limits continue to be out of control,the instrument must be checked and/or a service call made and/or further corrective action implemented Inorganic Laboratory: • Trip blanks are analyzed when applicable,to detect contamination during sample shipping,handling and storage. i QA Plan section No.12 rev.4 Date bdfiated 1/15/94 Date Revised:1/O9/03 Page 5 of 6 I • Method blanks are analyzed at a minimum of one every 20 samples,to detect contamination during analysis. One matrix spike and matrix duplicate of an analytical sample or laboratory water or soil is made and spike recoveries are computed at least every 20 samples to determine accuracy.Duplicate samples are analyzed at least every 20 samples. If insufficient volume of sample is received,the duplicate and spike samples are analyzed at a frequency of one per batch or 20 samples,whichever occurs first. • Performance evaluation samples from EPA and state agencies are analyzed to verify continuing compliance with EPA QA/QC standards. • Metals analysis instruments are calibrated daily. • QC/LCS checks samples are analyzed during every analytical batch of up to I 20 samples in order to document accuracy. When QC limits are not met during an analytical rum,the source of the problem must be investigated. Following an evaluation of the data,those samples affected must be re-analyzed after the problem has been solved. If QC limits continue to be out of control,the instrument must be checked and/or a service call made and/or further corrective action implemented. QA Pfan Swdw Na 12 rev.4 Date Initiate&ASS Date Revised U08/03 Page 6 of 6 Figure 12.3-1 Example Control Chart I i I - co w l i, $mil l�l N l IL qy�l l� l� l� qy l l� • c� l l i I ' QA Plan Section No.13 rev.4 Datelnitiatcd l/15M Date Revised U07103 f Page 1 of 2 13.0 QUALITY ASSURANCE SYSTEMS AUDITS,PERFORMANCE AUDITS AND FREQUENCIES The MITKEM Quality Assurance staff performs routine internal audits of the laboratory. The frequency of such audits depends on the workload in house but is done annually,at a minimum. These audits entail reviewing laboratory logbooks and all appropriate operations to ensure that all laboratory systems including sample control,analytical procedures,data generation and documentation meet contractual requirements and comply with good laboratory practices.. I. 13.1 System Audits: The laboratory is audited annually by the QA/QC Director in order to detect any sample flow,analytical or documentation problems and to ensure adherence to good laboratory practices as described in MITKEM standard operating procedures and quality assurance plan. The checklist used in an internal systems audit at MITKEM is presented in Figure 13.1-1. Problem areas detected during the annual Systems Audit are monitored weekly in follow-up audits conducted by the QA staff. r 13.2 Performance Audits: MITKEM participates in external Performance Test(PT)studies under the National Environmental Accreditation Program(NELAP)through the State of New York(Mitkem Laboratory's Primary Accreditation Authority).The PTs [Drinking Water(DW)and Wastewater/Solid Waste(WW/SW)] are administered by the QA department of the laboratory. Internally,performance is monitored on a daily basis at MITKEM through the use Of surrogate standards,LCSW/LCSS,and MS/MSD samples. Check samples from independent commercial sources are employed routinely in each of the MITKEM laboratory departments and ensure continuing high level performance_ Internal blind PE samples are distributed to each laboratory department by the QA Director at a minimal frequency of annually. I i I i I 1 1 � QAPIan 1 Section No.13 rev.4 Date Initiated'1/15/94 Data Revised:1/07/03 Page 2 of 2 Figure 13.1-1 QA Systems Audit Checklist I i I i l I� 'r I j I i 1 I I - I MITKEM CORPORATION j QA Internal Audit Oct-0i- 1 L Quality Assurance: QAIQC Director with assigned duties? Yes /No QA Report to Management submitted Quarterly? Yes /No Organizational Chart Up to Date?(Attachment A) Yes /No Quality Assurance Plan Updated Annually? Yes /No Date Revised: is the Quality Assurance Plan a controlled.document? Yes I No Laboratory Equipment Is equipment adequate and up to date? Yes I No Attach current Equipment List(Attachment B) Audit Program Internal Systems Audits performed annually? Yes/No Attach list of External Systems Audits from last year. (Attachment C) Internal Performance Audits performed annually? Yes/No Attach list of External Performance Audits from last year (Attachment D) Interval Data Audits performed on I(r/o of data generated? Yes/No Employee Training Employee Training Files up to date? Yes/No Safety Training Record for all employees? Yes/No Standard Oaeradng_Procedures Are the general SOPS updated annually? Yes/No Are SOPs updated annually for each analytical method? Yes/No Are SOPS updated annually for Sample Receiving? Yes/No Are SOPs updated annually for QAIQC Procedures? Yes I No Are SOPs updated annually for Data Reporting/Data Review? Yes 1 No Are SOPS updated annually for Standard Traceability? Ye's/No Are SOPs controlled documents? Yes/No Are SOPS signed by appropriate individuals? Yes 1 No Method Validation Initial Demonstration of Proficiency before method is implemented? Yes/No Page 1 of 10 O Are MDL studies up to date for each method? Yes/No Is the Amount Spiked equal to 3-5x the calculated MDL or per SOP? Yes/No Does the lab maintain a copy of each method it performs? Yes/No Corrective Actions Is a formal system for Corrective Actions in place? Yes f No Does the QA/QC Director review CARS? Yes!No Are CARS controlled documents? Yes/No Loebooks Are laboratory logbooks controlled and archived by QA? Yes I No Are logbook templates controlled and archived by QA? Yes/No Are logbooks peer reviewed weekly? Yes/No Proper correction techniques used? Yes/No Empty spaces properly"z"'d out? Yes/No Are logbooks paginated? Yes/No IL Quality Control: General Laboratory Eguinment Is an NIST traceable thermometer available? Yes/No Are lab thermometers calibrated annually against the NIST thermometer? Yes/No Are correction factors in use on lab thermometers? Yes/No Are Class"S"weights calibrated NIST every 2 years? Yes/No Are balances serviced annually? Yes/No Are balances calibrated as needed and the calibration recorded? Yes/No Is balance calibration acceptance criteria clearly defined and posted? Yes/No Control Charts Are control charts in place for each method and matrix? Yes!No Does each chart have a minimum of 30 points? Yes/No Are control charts checked quarterly? Yes!No Are control limits updated annually or when major method changes are made? Yes/No Page 2 of 10 Standard Traceabilit:/Ecgivalencv Are standards labelled with standard name,concentration,solvent, i working standard ID,expiration date,and preparers initials? Yes/No ' Are expiration dates of standards clearly defined in an SOP? Yes/No Are standards QOs against a second source standard after each initial i calibration? Yes/No 1 Are standards traceable from working standard analysis back to the standard received date,manufacturer,and lot#? Yes/No Are solvents traceable from preparation logbook to date received, '• manufacturer,and lot#? Yes/No DI Sample Receiving: i. Is an up to date SOP present in the area? Yes/No Is a sample receiving checklist used to receive samples? Yes/No Condition of samples on receipt? Yes/No Sample temperature on receipt? Yes/No Radiation screen? Yes/No C-O-C signed and properly filled out? Yes/No r Sample Storage Are samples,except aqueous metals,refrigerated at 40 f 20C? Yes/No Are refrigerator temperatures checked daily? Yes/No Are aqueous metals stored at room temperature? Yes/No Is sample pH checked and recorded for samples requiring acid/base preservation? Yes/No Are high conc6atration VOAs stored separately from other samples? Yes/No Are VOA samples stored separately from other samples? Yes/No Is a system of corrective actions in place? Yes/No A holding blank stored with each batch of VOA sample? Yes/No 0 Sample Containers Are sampling instructions provided with sample containers? Yes/No Ara proper preservations,sample containers,etc.posted? Yes/No Are preservatives traceable to original manufacturer&lot? Yes!No Are containers precleaned by the manuf tc-turer and a certificate of cleanliness supplied? Yes/No Page 3 of 10 ci SSnlp161�gg-�I Is a unique ID assigned to each smznple? Yes/No Is each sample container uniquely identified? Yes/No Is there a peer review of sample labelling procedures? Yes/No Waste Disposal Do internal COC procedures exist from Tempt to disposal? Yes/No Are samples disposed by a company certified to dispose of hazardous waste? Yes/No Is a certificate of disposal received and filed? Yes/No Safety Are safety glasses,lab coat,and gloves worn by the sample custodian? Yes/No Are sample coolers opened under a ventilated food? Yes/No IV. Data Reporting/Data Review: Has the Data Review SOP been reviewed/updated annually? Yes/No Are Data Reviews clearly documented with the use of checklists? Yes/No Is 100%of data peer reviewed? Yes/No Is data reviewed technically by a Lab Supervisor/L ab Manager? Yes/No Is 10%of data reviewed by the QA/QC Department? Yes/No Are estimated concentrations reported for values found between the Reporting Limit and Method Detection Limit(USACOE)? Yes 1 No Is a system in place for archiving data reports? Yes/No How long are data reports kept? V. Inorganics: oks Does a run logbook exist for each analytical instrument? Yes/No Does an instrument maintenance log exist for each instrument? Yes/No Does a prep log exist for each procedure? Yes/No Are logbooks peer reviewed weekly? Yes/No Proper correction techniques?. Yes/No Empty spaces"z"'d out? . Yes/No o Page 4 of 10 Paginated? Yes/No Controlled? Yes/No Do logbooks contain all pertinent information to the procedure? Yes/No (I.e.,,method,matrix,reagent lot#,digestion temp.,eta)' Standards Are standards QC'd against a second source after each ICAL? Yes/No Are standards traceable throughout-the lab? Yes/No Are expired standards present in the lab? Yes/No Es there a defined system for assigning expiration dates? Yes/No Anadyt}Eal Methods Are SOPS method compliant? Yes/No Do analysts follow the SOP? Yes/No Do analysts do an initial demonstration of proficiency study? Yes/No. Are analysts adequately trained and knowledgeable? Yes/No Does the EEC contain all analytes that interfere with target aaalytes? Yes/No (not just Ca,Fe,Al,Mg) Is ICAL documentation maintained on file in the lab? Yes/No Corrective Actions Is there a system for corrective actions in place? Yes/No Safety Do analysts wear safety glasses,lab coats,and gloves? Yes/No Are all reagents which need to be handled under a hood,handled in this manner? Yes/No VE. Volatiles: x. Does a run logbook exist for each analytical instrument? Yes/No Does an instrument maintenance log exist for each instrument? Yes/No Are logbooks peer reviewed weekly? Yes/No Proper correction techniques? Yes/No Empty spaces"z"'d out? Yes/No Paginated? Yes/No Controlled? Yes/No Do logbooks contain all pertinent information to the procedure? Yes/No (Le.,method,matrix,,reagent lot#,soil weight,etc.) Standards Are standards QC'd against a second source after each ICAL? Yes!No I Page 5 of 10 Are standards traceable throughout the lab? Yes/No Are expired standards present in the lab? Yes/No Is theme a defined system for assigning expiration dates? Yes!No Is standard fl=er temperature monitored? Yes!No Anal tical Methods ° Are SOPS method compliant? Yes f No Do analysts follow the SOP? Yes/No Do analysts do an initial demonstration of proficiency study? Yes!No Are analysts adequately trained and knowledgeable? Yes!No Is ICAL documentation maintained on file in the lab? Yes/No When%RSD> 15%,is the average adopted? Yes!No Is a CCV run at the end of the analytical sequence?(USACE) Yes/No Corrective coons Is there a system for corrective actions in place? Yes/No We!y. Are all reagents handled under a hood? Yes/No Are all safety equipment used? Yes/No VIL Semivolatiles: Lo ooks Does a run logbook exist for each analytical instrument? Yes/No Does an instrument maintenance log exist for each instrument? Yes/No Are logbooks peer reviewed weekly? Yes/No Proper correction techniques? Yes f No Empty spaces"z"'d out? Yes/No Paginated? Yes!No Controlled? Yes/No Do logbooks contain all pertinent information to the procedure? Yes!No (La.,method,matrix,reagent lot#,etc.) Standards Are standards QC'd against a second source after each ICAL? Yes f No Are standards traceable throughout the lab? Yes/No Are expired standards present in the lab? Yes!No Is there a defined system for assigning expiration dates? Yes!No Is standard freezer temperature monitored? Yes/No AnalAcal Methods Page 6 of 10 0 Are SOPS method compliant? Yes/No Do analysts follow the SOP? Yes/No Do analysts do an initial demonstration of proficiency study? Yes/No Are analysts adequately trained and knowledgeable? Yes/No Is ICAL documentation maintained on file in the lab? Yes/No When%RSD>15%,is the average adopted? Yes/No Is a CCV run at the end of the analytical sequence?(USACE) Yes/No Is a Method Blank analyzed after each CCV? Yes/No Is DDT breakdown and tailing factors for benzidine and pentachlorophenol evaluated for acceptat ality? Yes!No Does analyst review data for false negatives? Yes/No Corrective Actions Is there a system for corrective actions in place? Yes/No Safety Are all reagents handled under a hood? Yes/No Are all safety equipment used? Yes/No V1II. Pesticides/PCBs: Logbooks Does a run Logbook exist for each analytical instrument? Yes/No Does an instrument maintenance log exist for each instrument? Yes/No Are logbooks peer reviewed weekly? Yes/No Proper correction teclpiques? Yes/No Empty spaces"z"'d out? Yes/No Paginated? Yes/No Controlled? Yes/No Do logbooks contain all pertinent information to the procedure? Yes/No (Le.,method,matrix,reagent lot#,etc.) Standards Are standards QC'd against a second source after each ICAL? Yes/No Are standards traceable throughout the lab? Yes!No Are expired standards present in the lab? Yes/No Is there a defined system for assigning expiration dates? Yes/No Is standard freezer temperature monitored? Yes/No Anal-yi3cat Methods Are SOPS method compliant? Yes/No Do analysts follow the SOP? Yes!No Page 7 of 10 .o Do analysts do an initial demonstration of proficiency study? Yes/No Are analysts adequately trained and knowledgeable? Yes/No Is ICAL documentation maintained on file in the lab? Yes/No When'YcR.SD> 15%,is the average adopted? - Yes/No Is a CCV run after every 10 samples? (USACE) Yes/No Is.a Method Blank analyzed after each CCV? Yes/No Is DDT&Endrin breakdown monitored for PCB only analyses? Yes/No Are QC samples run on same instn ment as field samples? Yes/No j Are retention time studies performed after each column change? Yes/No Is target analyte%D between primary and confirmation<406/*Y Yes/No Corrective Actions Is there a system for corrective actions in place? Yes/No Safety Are all reagents handled under a hood? Yes I No Are all safety equipment used? Yes/No DL Organic Preparation: O LA)gL3OOk.S Does a preparation logbook exist? Yes/No Does a run logbook exist for each instrument? Yes/No Does an instrument maintenance log exist for each instrument? Yes/No Are logbooks peer reviewed weekly? Yes/No Proper correction techniques? Yes/No Empty spaces"z"'d.out? Yes/No Paginated? Yes/No Controlled? Yes/No Do logbooks contain all pertinent information to the procedure? Yes/No (Le.,method,matrix,reagent lot#,pH,%solids,etc.) 0 Page 8 of 10 o 1 i Standards Are standards QCd against a second source after each ICAL? Yes/No Are standards traceable throughout the lab? yes/No Are expired standards present in the lab? Yes i No Is there a defined system for assigning expiration dates? Yes/No Is standard freezer temperature monitored? Yes/Na Are solvents traceable through preparation? Yes/No Are personnel aware of syringe tolerances? Yes/No Analytical Methods Are SOPS method compliant? Yes/No Do analysts follow the SOP? yes/No Do analysts do an initial demonstration of proficiency study? Yes/No Are analysts adequately trained and knowledgeable? Yes./No Is ICAL documentation maintained on file in the lab? Yes/No Are temperatures of water baths and hot plates monitored? Yes/No Is deionized,charcoal-filtered water used for Pest/PCB blanks? Yes/No Corrective Actions Is there a system for corrective actions in place? Yes/No Ssfety Are all safety equipment used? Yes/No Are all'rcagents handled under a hood? Yes/No Comments Page 9 of 10 O 4 !1 i Not.supaNi r Date: I QA/QC Officer.------ Date: o i l u I i i 1 i Page10of10 0 x Department SOP Review and Analysis Checklist: DEPARTMENT: DATE: i • Have the SOPS been read and documented in else per sonnak turning files? YESINO/NA • Do die department personnel know where the SOPS are located?- YES/NOINA • Is the information documented In the SOPS accurate and follow the method pwoodures? YES/NU/NA • Is flee"Summary of Procedure'accurate? YES/NCNNA • Is"Sample Preservati2n,Container,Handling,and Storage"correct? YES/NO/NA • Are the reagents and EquipmenVApparatus caxrect? YES/NO/NA • Does the"Procedure"section accurately state exact procedures being followed by the analysis? YES/NOJNA • Are second source standards being used for all analyts? YES/NO/NA • Arc the criteria for the but ud CaltbradM Continuing Calibration,and Initial Coibration Verification QC criteria stated in the SOW YEWONA • Are the SOP calibration criteria being followed on a daily basis? YES/NO/NA • Are the QC criteria for the Blanks,LaboratotyControl Standards,Fortified Blanks,Duplicates,Matrix Spikes and Matrix Spike Duplicates slated in the SOPS? YES/NO/NA • Are the SOP QC frequency and criteria being followed on a daily basis? YES/NO/NA • Are hold times stared in the SOP? YES4401NA • Are other QC criteria such as Tunes,Retention Times,Peak Separation,and Ion Abundance stated in the SOPS? YES/NO/NA Are the SOP"other QC"criteria being followed on a daily basis? YES/NO/NA • Are calculations accurate and are being checked by the supervisor or analyst? YES/NO/NA • Is the"Quality Assurance!Quality Control'section accurate and all QC criteria Stated? YES/NO/NA • is the"Data Validation and Reporting"section accurate and being followed? YESNO/NA • Is the"Corrective Actioe section accurate and do the analyst/analysts Understand the procedures for initiation and completion of corrective action procedures? YES/NO/NA • Are common roufine and non-routine eorrective action examples specific to this analysis included in the SOP? YE&W0/NA • Is all safety equipment accessible and being worn where appropriate? YESJNO/NA ■ Are balances being calibrated daily before use? YES/NO/NA = • Does the balance calrtiration meet the SOP specified criteria? YESINO/NA • Is corrective action being taken and doarmented if the balance caltbration does not meet the criteria? YES/NO/NA i • Are the balances being calibrated at least once a month and documental in the balance calibration logbook? YES/NO/NA • Is the oven temperature being checked and recorded each day of use? YES/NO/NA • Is corrective action being taken if the oven temperature does not meet elm Criteria stated in the SOP? YES/NO/NA SOPs Reviewed: 0 Comments(on reverse side) QA Plan Section No.14 mv.4 Date loWded.1n5194 Date ReviW :I/MS103 Page t of 5 14.0 PREVENTIVE MAINTENANCE i Preventive maintenance is a routine practice at MITKEM for all instrumentation. Scheduled preventive maintenance minimizes instrument downtime and subsequent interruption of analysis. All major instrumentation is under service contracts so that downtime(due to catastrophic events)are minimized. Only those equipment items meeting or exceeding applicable performance requirements are used for data collection. This includes items such as laboratory balances as well as major analytical instruments such as ICPs,GCs and GC/MSs. MITKEM's laboratory personnel are familiar with the routine and non-routine maintenance requirements of the instruments they operate. This familiarity is based an education,hands-on experience and manufacturer's training courses. GC Maintenance: 0 1. The injection septum will be replaced once approximately fifty(50)injections or earlier if a leak develops. 2. The injection liner will be replaced once approximately fifty(50)injections or when initial and/or continuing calibrations fails repeatedly to meet method requirements. 3. The gold seal will be replaced except for septum and liner,and the column will be trimmed whenever an initial calibration is run. 4. The column will be replaced if chromatograms show excessive peak tailing and/or initial and cpntinuous calibration verifications fail repeatedly to meet method requirements. 5. Once a year,under service contract,all GC equipment under-go extensive maintenance by a manufacturer's service engineer. GC/MS Maintenance: 1. GC injector and liner are cleaned daily for semivolatiles and monthly for volatiles. 2. The column will be replaced if chromatograms show excessive peak tailing and/or initial and continuous calibration verifications fail repeatedly to meet method requirements. 3. The ion source will be cleaned when initial and/or continuing calibration repeatedly fail method specified criteria. QA Plan Section No.14 tev.4 Data initiated ]/1"4 Date Revised:LJOW3 Page 2 of 5 4. The pump oil will be replaced once a year. 5. Once a year,under service contract,all OC equipment under-go extensive maintenance by a manufacturer's service engineer. IC"Maintenance: 1. Peristaltic pump tubing will be replaced every sixteen(16)hours of instrument time or sooner when memory effects are manifested. 2. The plasma torch is cleaned with(aqua regia)every 1-2 weeks.If memory effects are manifested the torch will be cleaned immediately. 0 3. The sample introduction(spray chamber and nebulizer)is cleaned every 2-3 weeks. 4. Air filters are cleaned each time the torch is cleaned or as needed upon visual inspection. 5. Once every six(6)months,under service contract,the instrument undergoes extensive maintenance by a manufacturer's service engineer. Mercury FIMS 100 Maintenance: I. Pump tubing is replaced every 48 hours of instrument run time. 2. Sample loops,gas tubing extensions,and sample capillaries are replaced as needed. Lachat 8000 Maintenance: 1. All pump tubing is replaced every 48 hours of instrument run time. 2. Auto sampler arm is lubricated every 48 hours of instrument run time. 3. The manifolds,tubing connections,valves,etc.are cleaned or replaced as needed TCLP/SPLP Tumbler Maintenance: 1. The tumbler is checked at every use for number of rotations per minute(30rpms) and the ambient temperature checked and documented in the RPS Logbook. 2. If the tumbler is not spinning at 30rpms,motor is cleaned and oiled. 3. If tumbler is not spinning at 30rpms after maintenance,the motor will be replaced. I QA Plan Section No.14 m.4 Date Initiated.M5/94 Date Revised_1/08/03 Page 3 of 5 Instrument maintenance logs are kept for each instrument(Figure 14-1). The person performing the maintenance is required to provide the following information in the log: • Equipment identifier • The inspection,maintenance,calibration or corrective action(s)performed • The trigger(s)for the maintenance action(s) • The identity of the person(s)performing the maintenance • The date on which the work was performed, and • The condition of the equipment upon completion of the work. MITKEM maintains an inventory of replacement parts required for preventive maintenance and spare parts that often need replacement,such as filaments for GC/MS systems and the more mundane electrical fuses and GC column ferrules. To control cost, the appropriate supervisor shall decide the types and numbers of spare parts kept on hand for each equipment item. O I I . QA Pow Section No.14 rev.4 Date h&iatod:1/1-"4 Date Revised:1/08/03 Page 4 of 5 Figure 144-1 Example Instrument Maintenance Logbook Form I i 4 hGTKEM CORPORATION GPC 3 N AINTENANCE LOGBOOK Data Maintenance Description i i i i i QAT00185 6P-23 Reviewed By PAGE: 1 QA Plan Section No.14 rev.4 Date hidated:1115194 Date Revised 1109/03 Pars of 5 Figure 142 Instrument Maintenance Schedule @ § $ d v t 7 � a, u G IL § » 2 $ $ k 2 . . CL 9 b � ( o (aL \ ® = E § ° 7 D § ° % A _ E e & � § k \ E § 8E 2 2 � r $ xo xa g � S O � 8 . k k cc23 @ E E 2 A 2 a ■ % �� _. CO- LL $k k §° a e � § Ti 7 k f © | § 7 f\ 7 $ a I P E 2 \ f CL 2 zi k 5 & Ek 8 _ � > i ¢ ƒ k 0 k k R c 7 $ � \ � CL Ls _ / 4 Cl) E o k � � E k q 7 to o 2 2 % ■ $ � . E S � � k � k � % 2 $ $ to 01 2 m 277 O a & Irm- § ■ � � � i 7 _ LL § _ D CD % � \ C 2 \° t 21 § . L 7 2 k c f \ / 0 k @ § { § k \ D e @ a. A k A £ © 82 ■# E �© § t f 7 § 2 . . 2CL �$ � � 0 0 . Ffa & %§ / 2 0 e a§ § c . f � 2 $ , m 77 . g § . E § e 2 cu § § � t a k £ ® � 7 / � f R � S 2 � 2 k / k / a CL 2 E Z \ § E E E E 2 # ¢ J 2 / o � 8 � - k C . E 2 f cl CL £ @ R 2 B . 0 t QA Plan Section No.15 rev.4 Date faidated:W5/94 We Revised:1IM3 Page 1 of 3 15.0 SPECIFIC ROUTINE PROCEDURES USED TO ASSESS DATA PRECISION, ACCURACY,COMPLETENESS,METHODS DETECTION LIMIT AND LINEAR DYNAMIC RANGE These mathematical equations represent.the means of calculating analytical figures of merit on a routine basis at MITKEM. However,they may be supplanted with other calculations if requestedi by the client. Precision,accuracy and completeness are also discussed in Section 6. 15.1 Precision: Precision is frequently determined by the comparison of replicates,where replicates result from an original sample that has been split for identical analyses. Standard deviations,s,of a sample are commonly used in estimating precision. Sample standard deviation,s: n 11 1 r=t where a quantity,xi(e.g. a concentration),is measured n times with a mean, Y. The relative standard deviation,RSD(or sample coefficient of variation, CV), which expresses standard deviation as a percentage of the mean,is generally useful in the comparison of three or more replicates(although it may be applied in the case of n=2). a/oRSD= 100(s/ x) or CV= 100(s/ x) where:RSD=relative standard deviation,or CY=coefficient of variation s=standard deviation x=mean For duplicates(samples that result when an original sample have been split into two for identical analyses),the relative percent difference(RPD)between the two samples may be used to estimate precision. QA Plan Section No.15 iev.4 Date Initiated:1113/94 Date Revised:I1"3 fl Page 2 of 3 RPD= 2(D.-Di)x 1000/0 (D.+D.,) where:D1=first sample value D2=second sample value(duplicate) 15.2 Accuracy: The determination of accuracy of a measurement requires a knowledge of the true or accepted value for the signal being measured. Accuracy may be calculated in terms of bias as follows: Bias=X—T %Bias=100(X—Y) T L where:X=average observed value of measurement T="true"value Accuracy also may be calculated in terns of the recoveries of analytes in spiked samples: %Re cov e %R 100 x CSS SA SR) 1y( }_ where: SSR=spikes sample result SR=sample result SA=spike added 15.3 Completeness: Determine whether a database is complete or incomplete may be quite difficult. To be considered complete,the data set must contain all QC check analyses verifying precision and accuracy for the analytical protocol. Less obvious is whether the data are sufficient to achieve the goals of the project. All data are reviewed in terms of goals in order to determine if the data set is sufficient. Where possible,the percent completeness for each set of samples is calculated as follows: valid data obtained %Completeness=---------------------------x 100 total data planned 1 I - QA Plan Section No.15 rev.4 Date Initiated:1115194 Date Revised.t/o6PQ3 15.4 Method Detection Limit: Page 3 of 3 The method detection limit(MDL)is the minimum concentration of a substance that can be measured and repotted with 99%confidence that the analyte concentration is not zero. It is computed as follows from data obtained by repeatedly determining an analyte in a given sample matrix: 1. Analyze at least seven samples of a homogeneous matrix spike that contains the analyte(s).of interest at concentrations of three to five times the expected MDL. The entire sample preparation and analysis protocol must be.applied in each analysis;simply preparing one sample and repeating a measurement three or more times on the sample in not acceptable. 2. Compute the standard deviation of the results for each analyte. 3. Compute the MDL using the following equation: MDL=t(�t.a-0_99)(s) Where t is the one-sided student's t value appropriate for the number of samples analyzed,n;a is the statistical confidence level;and s is the standard deviation. O The one-sided t-values are presented below: Number of samples t-value 7 3.14 8 3.00 9 2.90 10 2.82 15.5 Linear Dynamic Range: The linear dynamic range is the concentration range over which the instrument response is linear. It is determined by analyzing a series of standard solutions that extends beyond the non-linear calibration region at both the low and high extremes,and selecting that range of standards which demonstrates a linear relationship between instrument response and concentration. QA Plan Section No.16 rev.3 I Date initiated:1/1S194 Date Revised:I1OV103 Page 1 of ' 16.0 CORRECTIVE ACTION !I An essential element of the QA Program,Corrective Action provides systematic, active measures taken in the resolution of problems and the restoration of analytical systems to their proper functioning. Corrective actions for laboratory problems are described in MITKEM Corporation laboratory standard operating procedures. Personal experience often is most valuable in alerting the bench scientist to questionable results or the malfunctioning of equipment. Specific QC procedures are designed to help the analyst determine the need for corrective actions(see Section 11,Data Reduction,Validation and Reporting). Corrective actions taken by scientists in the laboratory help avoid the collection of poor quality data. Mitkem's corrective action program divides these Issues into routine and non-routine corrective actions as described below. 1 Routine Corrective Action—A routine corrective action is taken when the out-of-control I event encountered is one that is detected at the appropriate level in the QA process. Routine corrective actions are defined in the analytical SOP with specific steps to be taken as corrective action. (i.e.,low surrogate recovery,continuing calibration verifications,project specific protocols that do not meet acceptance criteria,etc.) Routine corrective actions must be documented as described in the analytical SOP,but do not require further documentation in the corrective action logbook. Example ofroutine corrective action situations: surrogate/surrogates out,LCS out,CCV out,ICV out,IS area/areas out, typographical errors,random blank contamination,or false positive hittspectral ID match corrected during data review. No - outing Con•eetive Action—A non-routine corrective action is taken when the out- of-control event encountered is not typical for the method. For example,QC failures that pass through the final review to the client,procedural errors—not following the SOP,or a situation nct being detected by normal QA procedures that could adversely impact the accuracy,precision, etc.of a result. Non-routine corrective actions must be documented in the Corrective Action Request(CAR)logbook. The analyst,using his/her own judgement,may deem any corrective action situation non-routine and formally document it on a CAR. When.in doubt about a corrective action, the analysts are instructed to err on the side of formal CAR documentation.Examples of non-routine corrective action situations are: bad standard,expired standard mix being used, incorrect equation,"client- detected"problems,not following SOP protocols,using bad or contaminated lot of chemical/reagent/solvent,deciding to release data not conforming to SOP requirements, compound retention time outside of range, or improper library spectrum that leads to re- occurring mis-ideritifirttion of compounds. The essential steps in MITKEM Corporation corrective action system are: 1. Identify and define the problem. QA Plan Section No.16 rev.3 Date Initiated 1115/94 Date Revised IM/103 Page 2 of 4 2. Assign responsibility for investigating the problem. 3. Investigate and determine the cause of the problem. 4. Determine a corrective action to eliminate the problem. 5. Assign and accept responsibility for implementing the corrective action. 6. Establish effectiveness of the corrective action and implement it. 7. Verify that the corrective action has eliminated the problem. 8. Document the actions taken and those planned. 1 This scheme is generally accomplished through the use of Corrective Action Request Forms(Figure 16-1)available to all MITKEM staff members. Using this form,any laboratory scientist or project member may notify the QA Director of a problem as described in SOP No. Q07. The QA Director initiates the corrective action by relating the problem to the appropriate laboratory managers and/or project managers who then investigate or assign responsibility for investigating the problem and determine its cause. Once determined, appropriate corrective action will be approved by the QA Director. Its implementation is later verified through and internal laboratory audit. Information contained on corrective action forms is kept confidential within MPFKEM and is generally limited to the individuals involved. Severe problems and difficulties may warrant special repi:rts to the President of MITKEM who will ensure that the appropriate corrective actions are taken. Nonconformance: Any breech of standard protocols is a nonconformance item that is documented on the Corrective Action Request Form and management informed immediately.The following are nonconformance items: 1. Sample holding time exceeded. 2. Hoods,Class"S"weights,MIST Thermometers,balances,automatic pipetters,being used but not certified. 3. Expired standards being used. 4. Manual integration being misrepresented. QA Plan Section No_16n:v.3 Date Initiate&1/15/94 Date Revised:LW/03 Page 3 of 4 16.1 Client Complaints: Mitker n Corporation ensures client complaints are dealt with quickly and completely.The -policies are stated in the laboratory Client Complaint Standard Operating procedure (SOP)#Q02. 0 QA Plan Section No.16 rev.3 Date Initiated.1/1-"4 Date Revisal•VW103 Page of Figure 16-1 Quality Assurance Corrective Action Request Form NHTKEM CORPORATION Quality Assurance Corrective Action Request Originator. _ Date: i Laboratory:- Project: i Problem: Action Planned: Date Implemented; Resolution: i QAIQC Director: _ _ Date: _ QAT00001 CAR# Page: -. 1 QA Flan SectionNo.17 nv.4 Date Initiated:t/15/44 Date Revised M103 Page 1 of 2 17.0 QUALITY ASSURANCE REPORTS TO MANAGEMENT The MITKEM Quality Assurance Director submits a QA report each quarter to the Technical Director and Operations Manager of the Laboratory. The report is to be completed and submitted no later than the end of the second week of the month following the end of the quarter.The quarter months are March,June,September,and December. The report contains detailed information and QA activities during the previous three months including. i 1. Status and results of internal and external audits. 2. Status and results of internal and external proficiency tests. i 3. Identification of quality control problems in the laboratory. 4. Discussion of corrective action program issues. 1 5. Status of external certifications and approvals. 1 6. Status of staff training and qualifications. 7. Discussion of new QA program initiatives. f A copy of the report is kept on file in the QA department. In case of a severe problem or difficulty, a special report is prepared by the QA Director and submitted immediately to management. 7 1 l QA Plaa SeWon No.17 rev.4 Date hd iatei 1/15/94 Date Revised V07l03 -Page 2 of 2 i Figure 174 i Quality Assurance Report to Management Format i l I i i i i i. AME EM CORPORATION Quality Assurance Report to Management 1. Status and results of internal and external Audits I Status and results of internal and external proficiency testing 3.. Identification of quality control problems in the laboratory 4. Discussion of corrective action program issues S. Status of external certifications and approvals ' 6. Status of staff training and qualification 7. Discussion of new QA program initiatives QA/QC Director Date i I 3 QA Pima Section No.18 nev.4 Date Initiated:VI 5194 Date Revised L07/03 Page I of I 18.0- SAFETY MITKEM maintains safety program managed by the Health and Safety Officer,the Safety Committee Chairperson, and the Safety Committee. Responsibilities include many aspects that comply with the Right-to-Know Laws. Training includes: • Training seminars with information on basic safety instruction,SARA Title III/Right- to-Know, location of safety equipment,etc., • Chemical Hygiene Plan/Health and Safety manual, • Monthly Safety Committee meetings, • Centralized MSDS information, • Maps with safety equipment and all exits noted,and • Posted safety rules. i I i i i i i NIITKEM CORPORATION INSTRUMENTATION and EQUIPMENT LIST APPENDIX A t l } r - i QA Plan Appcn&A rev.2 EWe Initiated:6n309 Date Ravised:09IM1 Page 1 of 5 MITIWM CORPORATION INSTRUMENTATION and EQUIPMENT LIST Updated 9/20101 Instrumentation Vendor and Model Number Age(years) 2-GC System for Hewlett Packard Model 5890 GC with 2 and 5 Volatile Organics Tandem OI PIDMECD or PID/FID Detectors;with Tekmar Purge and Trap sample concentrators and Auto-sampler Or OI Analytical concentrator and auto- Sampler. 3-GC/ECD Systems for Pesticides/ Hewlett Packard Model 5890 GC with 2 to 5 PCB's and Herbicides dual Electron Capture Detectors and Auto-sampler. 1-Micro-GCIECD System for Hewlett-Packard.Model 6890 GC with 1 Pesticide,&TCB's dual Micro-Electron Capture Detectors and Auto-sampler. 1-Micm-GC/ECD System for Agilent Model 6890 GC with New Pesticides/PCB's dual Micro-Electron Capture Detectors and Auto-sampler. 1-GC system for Petroleum Hewlett Packard Model 6890 GC 3 Hydrocarbon Analysis and with dual towers,dual FID detectors Fingerprinting and Auto-sampler. 2-GC/MS Systems for Volatile Hewlett Packard Model 5890/5972 5 Organics GC/MS with OI Analytical Concentrators and 4551-DPM16/4552 Auto-samplers. 1-GC/MS System for Volatile Hewlett-Packard Model 6890/5972 2 Organic Analyses. GC/MS System with OI 4560/DPM 16 Purge and trap concentrator and Auto-sampler. 1-GC1MS System for Volatile Hewlett-Packard Model 6890/5973 new Organic Analyses. GC/MS System with 01456/4552 Concentrator and Auto-sampler. QA Plan Appendix A rev 2 Date bgfiated:&M/99 Date Revisstd 09l2MI Page 2 of 5 2-GC/MS System for Hewlett-Packard Model 5890/5872 2 and 5 Semivolatile Organics Analysis GUMS with auto-sampler. 1-GCIMS System for Hewlett-Packard Model 6890/5973 new Semivolatile Organics Analysis GC/MS with auto-sampler. High Performance Liquid Perkin Elmer System with Variable UV 3 Chromatography(HPLC)System Detector. Inductively Coupled Argon Plasma Perkin Elmer Optima 3000XI.Transaxial 3 (ICAP)Specrophotometer for ICAP with auto-sampler. Metals Analysis Inductively Coupled Argon Plasma Perkin Elmer Optima 3100XL Transaxial 1 (ICAP)Spectrophotometer for ICAP with auto-sampler. Metals Analysis Graphite Furnace Atomic Perkin Elmer 4100ZL ZEEMAN with - 5 Absorption Spectrophotometer for (GFAA)auto-smvler. Low Level Metals Analysis Flow Injection Atomic Absorption Perldn Elmer FIRS with auto-sampler. 5 Spectrophotometer(FIRS)for Mercury Analysis Ion Autoanalyzer for automated LACHAT Quick Chem 8000 dual 2 wet chemistry analyses channel ion analyzer. 2-Gel Permeation Chromatograph ABC/O.L Analytical. New for Sample Cleanup for Organic Analyses Total organic carbon,total carbon, 01 Corporation Model 1020 2 total inorganic carbon analyzer combustion TOC system with water and soil analysis modules. Diskette and Forms Deliverable Target Software by T1uuPut 3 for CLP Organics Corporation for Windows NT. Diskette and Forms Deliverable EDR System Software by Ward 3 QA Plea Appendix A rev.2 Date Initiated:6/23/99 Date Revised:09nMi Page 3 of 5 for CLP Inorganics Scientific 50 Gigabyte Onstream tape drives 2ea. 1 Veritas Backup Exec for Windows Nf Multi-system. 1 Analytical Balance Denver Instrument Company 3 Model.100A. Top-Loading Balance Denver Instrument Company 1 -4 Model XE-510. Model XP-3000(X010176). Model XP-3000(X010122). Ohaus,Model TS2KS. Ohaus,Model CT200. Ohaus,Model 5C6010. Ohaus,Model C1200. RefrigeratomTreezers RI,Walk-in. 1 -5 R2,Kenmore. R/F3,Kenmore. R/F4,GE. R/F5,Hotpoint. R/li 7,Hotpoint. R/F8,GE. R/F9,GE. R/F 10,Amana. RI 1,GE. I I QA Plan Appendix A rev.2 Date Wdated:6123/99 Date Revised:09/20/01 Page 4 of 5 R 12,Diplomat. RIF13,Whirlpool. R14,Excellence: Recirculator,refrigerated Neslab,CFT 150. 2 Neslab,CFT-150,3e& 1-6 Ovens Fisher Scientific,Model 516G. 1-6 Precision,25EG,2ea. Fisher Scientific,Model 750F. DI Water System Barnstet4 E-Pure. 4 Millipore. 4 US Filter. 1 Hotplates and Stirrers Fisher,Stirrer,lea. 1-5 Fisher,Hotplate/Stirrer,3m Thermolyne,Hotplate,lea Conductivity Meter Hanna,Model HI 8733. 1 PH Meters Orion,Model 520A,2ea 2 With 4 Combination Electrodes. Water Baths Precision. 1 Hot water baths,2ea 2-5 Thermometers NIST,Certified,50 to I Oft. 1 NIST,Certified,0 to 20ft,tea. 2-4 Oven,0 to 2500C,4ea. 1-6 QAPIm Appendix A rev.2 ! Data Initiated:6/2M Date Itcvised:0MV01 Page 5 of 5 Refrigerator,-5 to 150C,Bea. 1 . 5 Freezer,0 to�300C,Sea. 1-5 Mtxffie Furnace Paragon,Model DTC 800C. 2 Spectrophotometers Genesys,Spectronic 20. 1 Spectronic,Spectronic 20. 6 Pepettors Wheaton and Fisher,Adjustable 1-3 10—100uL, 1 lea Centrifuge IEC Centra,Model CL2. 2 Computer laboratory information ChemWare,Inc.Horizon Laboratory 2 Management system to manage Wormatioa Management(LIMS) information from;project quote system for Windows. through sample receipt,login, analysis,data collection,reporting and invoicing. Providesmanagement information,status tracking,QC charting and documentation. Instrument Maintenance Contractors: 1. Organics: A. Agilent Technologies. B. Professional Technical Service(PTS). C. 01 Analytical. 2. Inorganics: A. Perlan-Elmer. B. Lachat. C. FIMS 100. 1 I I � - MITEEM CORPORATION CONFIDENTIALITY,ETHICS,and DATA INTEGRITY AGREEMENT i APPENDIX B 1 1 i t 1 i i I t I MITKEM CORPORATION SUBCONTRACTORS CONFIDENTIALITY,ETHICS AND DATA INTEGRITYAGREEMENT I. I, _ CAamei,authorized representative of _ (Subcontractor)state that I understand the standards of integrity required of me and the Subcontractor with regard to the duties performed and the data reported in connection with the analysislanalyses contracted by Mitkem Corporation. II. Subcontractor agrees that in the performance of analysis for Mitkem Corporation: 0 A. Subcontractor shall not intentionally report data values or results that are not the actual values measured or observed; B. Subcontractor shall not modify data values unless the modification can be technically justified through a measurable analytical process; C. Subcontractor shall not intentionally report the dates and times of data analyses i that are not the true and actual dates and times of analyses; and D. Subcontractor shall not intentionally represent another's work as its own. III. Subcontractor agrees to report immediately any accidental or intentional reporting of non-authentic data to Mitkem. IV. Subcontractor agrees not to divulge any pertinent information including but not limited to data and information about any Mitkem projects to outside sources without the prior consent from Mitkem or its clients. i I understand that failure to comply with the above ethics and data integrity agreement can result in immediate termination of the subcontract relationship with Mtkem Corporation. (s=gnan«'e) - (Date) i (Name) OWN i I