LABORATORY QUALITY ASSURANCE (QA) PLAN … · erm-northwit 0300927 laboratory quality assurance plan work plan document ii, attachment i remedial investigation facet enterprises,

LABORATORY QUALITY ASSURANCE PLANWORK PLAN DOCUMENT II, ATTACHMENT I

REMEDIAL INVESTIGATIONFACET ENTERPRISES, INC.

ERM-Northeast

0*38

ERM-Northwit 0300927

LABORATORY QUALITY ASSURANCE PLANWORK PLAN DOCUMENT II, ATTACHMENT I

REMEDIAL INVESTIGATIONFACET ENTERPRISES, INC.

OCTOBER 27, 1989

PREPARED FOR:

FACET ENTERPRISES, INC.MOTOR COMPONENTS DIVISION

3 MIRACLE MILEELMIRA, NY 14092

PREPARED BY:

COMPUCHEM LABORATORIES, INC.3308 CHAPEL HILL/NELSON HIGHWAYRESEARCH TRIANGLE PARK, NC 27709

100

Quality Assurance Plan

CompuChem* LaboratoriesP. 0. Box 12652

3308 Chapel Hill/Nelson HighwayResearch Triangle ParkNorth Carolina 27709

This document conforms to "Guidelines and Specificationsfor Preparing Quality Assurance Program Plans"(QAMS-004/80) as published by the EPA's QualityAssurance Management Staff, Office of Monitoring Systemsand Quality Assurance, Office of Research and Development.

Director of Quality Assurance:

Issued To: ELRM - NORTHEAST"

Date: CTDE gL IQ/ (989

Copy Number .. 433

PROPRIETARY MATERIAL - Confidential Property ofCompuChem*1 Laboratories, Inc. Reproduction, disclosureor use without specific written authorization ofCompuChem* 1s strictly prohibited.

0541

Section: Table of ContentsRevision No. 6Date: October 17, 1988Page 1 of 2

QUALITY ASSURANCE PLAN

TABLE OF CONTENTS

1.0 Quality Assurance Program Plan Identification Form

2.0 Introduction

3.0 Quality Assurance Policy Statement

4.0 Quality Assurance Management4.1 Introduction4.2 Assignment of Responsibilities4.3 Communications4.4 Document Control4.5 QA Program Assessment

5.0 Personnel Qualifications5.1 Introduction5.2 Training

6.0 Facilities, Equipment, and Services6.1 Introduction6.2 Laboratory Areas6.3 Equipment6.4 Instrument Maintenance6.5 Material Procurement and Control

7.0 Data Generation7.1 Quality Assurance Project Plans7.2 Standard Operating Procedures

8.0 Data Processing8.1 Collection8.2 Validation8.3 Storage8.4 Transfer8.5 Reduction

FAC 001 0642

Section; Table of ContentsRevision No. 6Date: October 17, 1988Page 2 of 2

QUALITY ASSURANCE PLAN

TABLE OF CONTENTS (continued)

9.0 Data Quality Assessment9.1 General Quality Assurance Program Objectives9.2 Methods for Attaining Routine Quality Control Requirements9.3 Specific Routine Quality Control Requirements9.4 Organic Precision and Accuracy QC Acceptance Criteria9.5 Inorganic Precision and Accuracy QC Acceptance Criteria

10.0 Corrective Action10.1 Introduction10.2 Routine QC Check Reports10.3 Monthly QA Activity Reports10.4 Laboratory Performance Reports10.5 Laboratory Audit Reports

11.0 Implementation Requirements and Schedule

12.0 References

Appendix A: Method Validation StudiesAppendix B: Resumes and Experience of Key PersonnelAppendix C: Tables of Contents; Standard Operating Procedures (SOPs), Sample

Preparation Procedures (SPPs), andInstrument Procedures (IPs)

Appendix D: Condition CodesAppendix E: Chain-of-CustodyAppendix F: Drinking Water RequirementsAppendix G: Subcontracted Services

FAC 001 0643

Section No. 1.0Revision No. 5Date: October 17, 1988Page 1 of 2

1.0 QUALITY ASSURANCE PROGRAM PLAN IDENTIFICATION FORM

Document Title Quality Assurance Plan: CompuChem* LaboratoriesDocument Control Number:________Organization Title: CompuChem^ Laboratories. Inc.

Address: P.O. Box 126523308 Chapel Hill/Nelson Highway________Research Triangle Park. NC 27709_______

Responsible Official: Mr. Kees Verkerk_________Telephone; (919) 549-8263Title: Chief Executive Officer and President of CompuChem*_______

CorporationQuality Assurance Officer; Mr. Robert E. Melerer Telephone; (919) 549-8263

Address: CompuChem* Laboratories. Inc.______________3308 Chapel Hill/Nelson Hlohway_____________Research Triangle Park. NC ?7709______

Plan Coverage Environmental Laboratories Including:Production Planning and Control____STassware PreparationSample Preparation LaboratoryHigh-Hazard LaboratoryInorganics LaboratoryGC/MS LaboratoryGC LaboratoryData Entry ana Report Preparation)1ox1n Coordination and ReportingEPA Technical ReviewiPA Customer InqulnCommercial Technical ReviewCommercial Customer InquiryIns trumentHa TntenanceQuality Assurance

PAC 001 0644

Section No. 1.0Revision No. 5Date: October 17. 1988Page 2 of 2

Concurrences

(1) Name: Hr. Robert E. Helerer

Title: Director pfc Quality Assurance

Signature:

(2) Name: Mr. Kees Verkerk

Date:

Title: Chief Executive Offlcgf and Resident of CompuChem* Corporation

Signature: Date:

PAC 001 0545


2.0 INTRODUCTION

CompuChem* 1s dedicated to providing the highest quality data available. TheIntent of this manual 1s to describe the manner 1n which the laboratory producesdata of known quality, assures that the data meet or exceed all QC/QA

objectives, and permanently documents that analytical systems at the time of

data acquisition were under control. The Quality Assurance Plan defines thelaboratory's purpose, Its organization and Its operating principles.

This document 1s not Intended to Identify specific details of the laboratory'squality control systems, analytical methods or laboratory Information management

systems, although a general discussion of these areas 1s covered. For thisreason, the manual Is often referred to as the "Generic QA Plan." Manual users

are referred to the laboratory's Standard Operating Procedures (SOPs), the

Quality Assurance SOPs or specific Quality Assurance Project Plans (QAPPs) forgreater detail.

The Quality Assurance Plan was developed with the aid of a variety of resources,the format and content generally following the recommendations made 1n

"Guidelines and Specifications for Preparalng Quality Assurance Program Plans"(QAMS-004/80) and "Interim Guidelines and Specifications for Preparing QualityAssurance Project Plans" (QAMS-005/80). Other references are sited 1n Section12.0.

The following section describes the responsibility for the contents of the QAPlan. The QA Department at CompuChem*, consisting of the Director, Manager,various QA Specialists and support staff, 1s organizationally and functionally

FAC 001 0646


Independent from the analytical laboratories. It 1s the responsibility of the

QA Department to assure that all laboratory personnel comply with the

requirements of the QA Plan and "Good Laboratory Practices" (GLPs).

PAC 001 0647


3.0 Quality Assurance Policy Statement

The Management of CompuChem* Laboratories 1s fully and firmly committed to the

quality assurance program described 1n this QA Plan. Each director, manager and

supervisor as well as their staff members, as assigned 1n accordance with this

plan, 1s obligated to comply with Its stated requirements, responsibilities andobjectives.

The primary QA objective 1s to develop and Implement procedures for sample

receiving, cha1n-of-custody, sample preparation, laboratory analysis, data

validation, and reporting that will provide data that are legally defensible 1n

a court of law. Key aspects of these procedures are described In this QA Plan,while specific details are Included 1n the laboratory's SOPs and QA SOPs — all

three references serving to document the elements of CompuChem's QA Program.

The QA Program will be maintained and expanded or modified as necessary, to

ensure all reported data are of uncompromising quality. In order to determine

whether QA objectives are met, sufficient quality control will be generated to

evaluate precision, accuracy and completeness, and when possible, a statement

regarding representativeness and comparability will be provided.

FAC 001 0648


4.1 Quality Assurance Management4.1 Introduction

With over 400 employees, CompuChem* offers the scientific and technical

expertise needed to service the analytical and Informational needs of our

customers. In addition to our experienced analytical laboratory personnel (with

specialized skills 1n organic and Inorganic analyses) CompuChem* utilizes a

computer systems staff that plans, develops, and Implements software systems for

data management and sample scheduling and control. To ensure that the

analytical needs of our clients are met, customer service representatives are

assigned to each account, providing a liaison between the customer and the

laboratory.

For our Involvement with the EPA, dialogue has been established and 1smaintained with the Program Office 1n Washington, DC through our Project Officer

and with our Deputy Project Officer located In our region (Region IV).

The following section describes the operational and functional responsibilities

of key lab personnel, Including the duties and services performed as they relateto product quality. Additionally, the roles and responsibilities of the QualityAssurance Department and Its organizational relationship to lab management are

Identified. Please refer to the organizational charts at the end of thissection for an overview of these relationships.

The Quality Assurance staff monitors and reviews all laboratory units and

operates Independently of production areas. All quality control criteria aredocumented and compliance 1s verified at each level of laboratory data review.

FAC 001 0649


In-lab data validation and Independent QA auditing SOPs describe the details of

these quality control functions. Section 8.2 presents a general overview of

the data rev lew/data validation processes. The QA Department 1s responsible

for, among other things, verifying the Integrity of these functions and

documenting performance for lab management review.

001 0650

Section Mo. 4.1Revision No. 4Data: October 17.Page 3 of 6

10voo

1988

CompuCham* Corporation

Oo

u3

Chief Executive OfficerKMS Verkerk

V.P. 4 CFOPaul Brunsulck

Olr actor.Human ResourcesGeorge Hedrlck

General Manager ForensicDrug Testing Operations

Janes McCarthy

Director.Quality AssuranceRobert E. Malerer

Administrative AssistantDabble Petlllo

Director, EnvironmentalTesting Operations

Kees Verkerk

______C Acting)_____

V.P.,Envlron«antalMarket Development

Thomas A. Peacock

Director. MISDan Kessler

Director, EnvironmentalMarketing/Sales

Rick Glgllo

V.P.. FDT Marketing/SalesMike Terrettl

President. CheapestAnalytical Labs

Joel Bird

Section No. 4.1Revision No. 4Date: October 17. 1988Page 4 of 6

ID\f>O

October 17, 1988ConpuCheM* Laboratories, Inc.

oo

DirectorCnvlromMAtal TestingOperations (Acting)

Kees \torkarh

Director, Production,Planning and Control

Richard Bloom

Manager. LabInstr MentationJlo Ch

Industrial Engl(Vacant)

Manager.Prep/Final Technical

ReviewAnn Flaherty

Manager, Inorganics LabsBruce Rolrbech

Manager. Organic LabsStew* Ma I burn

Sactlon 4.1Revision No. 4Oat*: OctoberPag* 5 of 6

17, 1988romtoo

October 17. 1988CoepuCnee* Laboratories. Inc.

Quality Assuranc*

Oo

Director. QualityAssuranc*

Bob Milarar

OoMMunlcatlon Spec.Wi l l I a* Marton

Manager QABob Mhltehaad

Hard IVocassorDenis* Ge*

QA Clerks/CoordinatorsMalonle JacksonSlwlla Maddox

QK SpecialistsPeter Hill

Roshlnl JoshlDabble Rlss*

ST. QA SpecialistWanda Boon*

Sr. StandManh

Laboratory Operations/Quality Assurance Relationships

Section: 4.1Revision No. 4Date: October 17. 1988Page 6 of 6 in

V£>O

umiA

rtolU«r»

>r •»••«!» •«*•!••

Mr CMt«MT KKrwl tetrcl•*«M*t -»*•€••••• Owl*--**«••*• Utaml «l-CiMt«*/

"~l

8C/XI t«xr»t«r«-11 «/• ll

•f>r<MrWMI*«U I Allf.fr«c»r«MTM All

M (T

L OUWITV MIM*HCfyWM.IfT ODMTDOl

•4»«ti«« ri«n«i««

rkl•ck lftU

mt »l»IICatM

-«l«rt« 9* St»tl ••-Will** Ml MIU

> CrllvU |_

-4«*lt> ••!• lr« AllSt*tl«M

: ttt»r«l«nr l»«rM«lc» t«»r»t«ni 0Sfeir -»^—«—•-I rMltCl* ' -CM* «MJW MT««T

M* HnklcM* fMlftlt1

I

f>

OO

Iflwl T«ck*l<M It »•«• «•»!•• j

. I

/


4.2 Assignment of Responsibilities

The main objectives of CompuChem's Quality Assurance Program are to assure that

our laboratories generate data of known quality, that data quality meets orexceeds all QC/QA criteria, and that the records necessary to document

laboratory performance are maintained. Additionally, the QA Department has theresponsibility of providing feedback to management and to Identify and Implement

policies to Improve quality. The success or failure of the program 1s, to a

great extent, dependent on the capabilities of those assigned the responsibility

of carrying 1t out.

The following 1s a brief summary of the responsibilities and authoritiesassigned to each of the QA Department staff members:

Director of Quality Assurance

To be certain that the laboratory achieves all QA Program objectives, the

Director of Quality Assurance monitors and directs the quality activities of

QA Department and Lab personnel. The Director acts 1n strict adherence to the

procedures and requirements stated 1n the Quality Assurance Plan.

The Director of QA reports directly to the corporation's CEO, 1s a member of the

Executive Staff* and 1s organizationally and functionally Independent of allpersonnel directly Involved 1n the operation of the technical program. The

Director has the authority to terminate non-conforming work at any time.

Additional responsibilities and duties Include:Preparing and overseeing the preparation of the QA Plan;Monitoring the QA Program as documented 1n the QA Plan and ensuring that allelements are carried out as written;

FAC 001 0655


Developing and Implementing new QA programs, Including statistical procedures,additional quality control measures, validation of new methods, etc.;Conducting scheduled or unannounced audits and Inspections, reporting findingsto management, and when needed, ensuring that corrective action 1s taken;

Maintaining current documentation of all measurement procedures routinely used1n the laboratories, Including those used by subcontractors;Periodically Informing management of the status of the QA Program;

Seeking out and evaluating new Ideas and current developments 1n the field of QAand recommending means for their application where advisable;Implementing or modifying analytical methods to conform with recognizedstandards and/or fundamentals of Good Laboratory Practices, Includingalteration of analysis/procedure codes used by the Computerized LaboratoryManagement System (CLMS);Final authority to terminate or alter any Incorrect or Improper analytical ormeasurement procedure 1n order to conform to requirements of the QA Plan;Training, directing and qualifying personnel 1n specified laboratory QC andanalytical procedures, or designating qualified Individuals to do so;Review and advise lab management on requirements and applicability of specificQuality Assurance Project Plans (QAPPi), new statements-of-work (SOWs), RFQs,RFPS, IFBs, and other contract-related Issues.Reviewing corrective action reports for out-of-control events and verifying thatremedial action has been taken to restore control;Assuring that subcontractor laboratories are complying with the QA Program;

Serving as polnt-of-contact for exchange of QA/QC Information and approving,along with the Laboratory Director, release of QA/QC Information;

Direct the activities of the QA Department technical staff and CommunicationsSpecialist.

FAC 001 0656


Manager of Quality Assurance

The Manager of Quality Assurance reports to the Director of Quality Assurance

and functions Independently from the laboratory technical program. The Manager

1s primarily responsible for overseeing and directing the activities of the

Quality Assurance staff, consisting of Sr. QA Specialists, QA Specialists, Sr.Standards, Chemists, and clerical staff. The Manager of QA, the QA Specialists

and the Sr. QA Specialists have authority to approve data. Other than these1nd1v1d1uals, only the Final Tehcnlcal Relvewer has the authority for final data

approval.

Additional responsibilities and duties Include:

Provide QA reports to management, as described 1n Section 10.0;Oversee the laboratory's participation 1n external QA/QC programs;Coordinate external (on-s1te) or Internal QA/QC audits or Inspections;

Review and approve all laboratory-generated data qualifying notices;

Write Quality Assurance Notices, used to document exceptions to QCacceptance criteria or other matters affecting data useablHty orInterpretation, for Inclusion 1n data packages;

Provide training to QA and laboratory staff;Provide assistance on special projects as required by the QA Director;Oversee all subcontractor QA Programs, Including administration ofsubcontractor proficiency studies and on-slte audits;Assume the responsibilities of the QA Director, 1f necessary.

Quality Assurance Staff

The Quality Assurance Staff 1s responsible for carrying out quality activities

as directed by the QA Manager and QA Director. All members of the QualityAssurance staff function Independently from the laboratory technical programs.

FAC 001 0657


Additional responsibilities and duties Include:

Create and revise SOPs, Including Integration Into proper document controlformat, maintaining a chronology and distributing SOPs to laboratorystations;

Ensure that the laboratories meet all requirements as documented 1n the QAPlan, as well as the specific QA and lab SOP manuals;

Audit and spot-check work 1n process for quality and completeness;Provide deviation/exception reports to laboratory managers and the QADirector regarding out-of-control analyses and provide recommendations forcorrective action;Oversee corrective action as required;

Generate, analyze and document QC/QA data (much of the QC data 1s generatedby the laboratory staff In the normal course of producing analytical data,or by using the CLMS during data acquisition or data entry);

Based upon laboratory performance statistics and/or statement-of-workrequirements, establish and update control limits using QC data from routinesample analyses;Provide Information and documentation for Internal/external audits orInspections;Function as a liaison between the QA Manager/Director and personnel withinthe laboratories;Communicate QA Program objectives'and requirements to clients and externalauditors;Reinforce GLP within the laboratory;Communicate any quality concerns to the QA Manager/Director;

Communicate any safety concerns to the Manager of Facilities and Safety;Review and approve Performance Evaluation (PE) and Proficiency Testing (PT)sample data;Review PE and PT scores, coordinating lab personnel review of unacceptablescores and associated data, and assembling findings Into unified documentfor response to certifying agency;Initiate and document corrective action (1f necessary) related tounacceptable scores and associated data, and assembling findings Intounified document for response to certifying agency;


Initiate and document corrective action (1f necessary) related tounacceptable PE/PT scores or audit deficiency reports;

Introduce Internal "blind" PE samples Into the CLMS (or mailing tosubcontractor labs) and report performance to management (this Includes bothInitial and continuing certification of performance, and 1s required of allsubcontractor laboratories);

Document approval and traceablHty of all standards to NBS, USEPA or othercertified source;Document calibration traceablHty of all thermometers, balances and Class-Sweights used 1n dally calibrations;

Audit the Environmental Site Profile (remote reporting) database,summarizing findings 1n reports to management;Conduct routine Performance Audits and System Audits, summarizing findings1n report to management;Audit computer output tabulating all keycard accesses to restricted areas,summarizing findings 1n report to management.

Laboratory Personnel and Management

A variety of Quality Control functions and duties directly or Indirectly

affecting data quality are performed by laboratory personnel and management.

Key responsibilities of this nature Include:

Perform scheduled, routine preventatlve maintenance or Instruments oroversee work done under service contracts;

Assure compliance with methods and SOPs and as written as directed by theQuality Assurance Director;Verify that all Instruments meet calibration and tuning requirements;

Respond to corrective action requirements;Follow GLPs and recommendations of the QA Department for Improving qualityand safety;Perform and document action steps based on established QC acceptancecriteria;Provide adequate and documented training of personnel.

pAC 001 0659


4.3 Commun1cat1onb

The Quality Assurance Department communicates to other areas of the laboratory

and to Management via several different types of reports, the key QA reports asdescribed 1n Section 10.0 . The Director of QA and the QA staff also distribute

Inter-off1ce memoranda to appropriate laboratory management detailing theresults of Internal and external audits, blind Inter laboratory proficiency

studies, blind Internal proficiency studies, and deficiency reports/corrective

action needs. Good Laboratory Practices and successful performance on various

studies and audits are also reinforced through these memoranda.

Section 10.0 provides additional details regarding the monthly and quarterly

reports distributed to all laboratory managers and appropriate senior and

executive staff.

PAC 001 0660


4.4 Document Control

Document control procedures, as described 1n section 1.4.1 of the Quality

Assurance Handbook for A1r Pollution Measurement Systems. Volume J.(EPA-600/9-76-005), are used 1n the production of the QA Plan and other

documents vital to the operation of the laboratory. This document controlsystem, described 1n the QA SOP Manual, Includes official distribution lists, a

historical file of all updated standard operating procedures, and appropriate

signature levels for the ensurance of correct methods, procedures and

techniques.

PAC ""1 0661


4.5 QA Program Assessment

The Director of QA and the department staff conduct periodic assessments of the

total QA program. Based on these assessments, a written status report of QA

activities and progress 1s forwarded to management. The following Items are

addressed 1n these reports, most being addressed 1n the Monthly QA ActivitiesReport to management as described 1n Section 10.0. All Items are addressed at

least semi-annual1y 1n the QA report to the CEO.

1. Status of or changes to QA Program Plan

2. Status of QA Project Plans, 1f any3. Measures of data quality

4. Significant QA problems, accomplishments, and recommendations5. Results of performance audits6. Results of system audits

7. Status of QA requirements for contracts8. Summary of QA training (Internal and external QA/QC seminars and

courses)

001 0662


5.0 Personnel Qualifications

5.1 Introduction

CompuChem*, located 1n Research Triangle Park, NC, and within minutes of three

major university campuses, 1s Ideally positioned for recruiting both degreedscientists and experienced professionals. Many applied science graduates jointhe organization as entry-level technicians, and progress through extensive

training Into senior chemist, data review/validation, and QA positions. In

most technician positions and Instrument operator positions, the training period

lasts from six months to one year, depending on the level of experiencerequired and complexities of the position/Instrumentation.

Job descriptions, Including required educational, training and experiencequalifications, are Incorporated Into Individual personnel records, and are

available for review 1n the Human Resources Department. These records alsoserve to document additional cross-training, and participation 1n continuingeducation programs.

QA Plan users are referred to Appendix B for resumes of key personnel. AlsoIncluded 1n this appendix are the USEPA's requirements for qualifications oftechnical personnel Involved 1n the analysis of EPA samples. CompuChem'stechnical personnel meet or exceed these requirements 1n all cases. Suitablestaff are nominated 1n the QA SOP to deputize for senior technical staff and QAmanagement 1n their absence.

001 0663


5.2 Training

There are two principle modes of training at CompuChem*. New employees, after

familiarizing themselves with pertinent lab SOPs and the QA Plan, are trained

one-on-one with the department manager, supervisor or an appropriate experiencedtechnologist. This training follows an established format with statedobjectives and evaluations at specific Intervals. Training manuals are required

at various laboratory stations to document acceptable performance on sample

preparation or analytical procedures, and to Indicate when a technician or

analyst 1s qualified to perform these duties Independently. Those qualified to

perform certain procedures are specified 1n the Initial Documentation Forms of

the area's SOP Manual, which also become a part of the Individual's personnelfile.

In the Sample Preparation Laboratories, for example, blind samples are submittedfor continuing evaluation of the technician's performance. The goals that can

be measured are to produce or demonstrate acceptable accuracy based on

recoveries of spike and surrogate standards 1n both routine QC samples and blind

samples, show no sample contamination during processing, provide properdocumentation with each sample preparation, demonstrate precise and reproducible

work, and show the exercise of sound technical judgment.

The second form of training 1s for new procedures or new Instrumentation as they

arrive 1n the laboratory. The manufacturer usually provides training coursesand certificates for those who successfully complete the program. Supervisorsand senior technologists who are trained by the manufacturer are thenresponsible for providing Instruction and training to staff members.

0664


Documentation of training, Including certificates, 1s maintained as part of the

employee's permanent personnel record. New methods, or procedures reflectingsignificant changes 1n existing methods, must be validated following theprocedures outlined 1n Appendix A.

In addition to the Initial training, employees are encouraged to participate 1ncontinuing education. This education often Involves Intradepartment seminars or

review sessions conducted by techn1cal/QA management. These seminars are

Intended to keep employees abreast of recent changes 1n procedures and newtechnologies. More experienced employees are given an opportunity to sharetheir knowledge and skills with newer employees.

A variety of local seminars, workshops and lectures are also made available to

employees. Again, because of CompuChem's Ideal location within minutes of anumber of college campuses and key federal agencies (U.S. Environmental

Protection Agency—Environmental Research Center/Office of A1r Quality Planningand Standards, National Institute of Environmental Health Sciences, ResearchTriangle Institute), employees have ready access to a variety of educationalresources. Workshop and seminar attendees usually transmit their experiences 1nthe form of trip reports or 1n-house presentations to appropriate staff members.

CompuChem* has also established an Educational Assistance Program, reimbursingemployees for the cost of formal coursework that enhances Job performance andopportunities for advancement.

The formal training program at CompuChem* also Involves safety training. TheManager of Facilities and Safety has the responsibility of coordinating andenforcing the laboratory safety program at CompuChem*, and 1s the designated

FAC 001


Laboratory Safety Officer. The safety program Involves the following key

elements:

- safety training programs for all personnel

- the Safety SOP Manual, approved by the Director of QA and the CEO- periodic (at least quarterly) Inspections of the facilities forcompliance with safety regulations and the Safety SOPs

- verification that all safety equipment 1s operable and 1n goodworking condition {Including Inspection and recharging of all fireextinguishers, and semi-annual Inspection of hood velocities)

- Initial testing of all new safety equipment- periodic (at least annual) fire/evacuation drills

- the Safety Committee, comprised of Safety Facilitators representingkey sections of the operation

- R1ght-to-Know Seminars held for all laboratory personnel, andconducted by chemical manufacturers, to discuss chemical hazards,safety precautions, medical treatment, and spill cleanupprocedures.

The Safety Officer has the responsibility of conducting Internal safety

Inspections, covering all aspects of laboratory safety Including fire, hazardousmaterials, personal dress, electrical safety, posted evacuation routes, andcondition of all safety equipment. Corrective actions Identified 1n the

Inspection or during safety drills are the responsibility of the SafetyFacilitator for each laboratory section.

Yearly safety briefings for all employees are the responsibility of thedepartment/laboratory managers. Managers receive their Instruction through the

section Safety Facilitators, the Safety Officer and the Safety SOP Manual.


Training shall Include safety for fire, electricity, compressed gases, chemical

i hazards, radiological hazards, and safety equipment, depending on the

responsibilities of the department or laboratory. New employees must be trained!

1n all aspects of safety concerned with their position responsibilities and

(when applicable) the laboratory(les) they work 1n.

Laboratory/department managers, Safety Facilitators and the Safety Officer must

maintain documentation of safety training. The documentation must Include a, 11st of the attendees, the training subjects(s) the time spent 1n training, and1 the date.

001 0667


6.0 Facilities. Equipment and Services

6.1 Introduction

This section describes the facilities at CompuChem*, the Instrumentation and

peripheral equipment, and the services provided 1n maintaining the facility.

CompuChem* 1s located 1n Research Triangle Park, NC, 15 miles west of Raleigh.

The total facility 1s comprised of both the Environmental and Forensic Drug

Testing Operations of CompuChem* Laboratories, Inc. The two operations have

separate laboratories that function Independently, Including separate computer

systems. Much of the office space 1s also separate, however, many

administrative functions overlap (I.e., Accounting, Quality Assurance, Human

Resources, Computer Operations) and share common office space. Facility space

allocation 1s described 1n section 6.2, and Includes the Environmental

Operations laboratory sp^ce, Environmental office space, and administrative

office space common to both operations, totaling approximately 64,000 square

feet. The two operations share two adjacent buildings which are connected by apermanent, enclosed walkway. Electrical power 1s supplied by Duke Power

Company, with a service capacity of 2000 amperes at 480 volts. The

envlornmental controls for the heating, ventilating, and air conditioning

systems are Honeywell Electric and provide automatic starting and stopping aswell as temperature control. All critical temperature areas such asrefrigerators, freezers and computer rooms are monitored 24 hours/day by an

off-site monitoring firm. The temperature of the refrigerators and freezers 1s

maintained by a standby generator 1n the event of a power failure. Theelectrical power to the computer room 1s regulated by a power conditioner.

001 0668


Building security 1s maintained at all times. The main entrance 1s monitored by

a full-time, contracted security staff (24 hours/day, seven days/week).

Visitors must s1gn-1n at the security guard's desk and be escorted through thefacility by members of the staff. The exterior doors as well as the doors of

various controlled access areas within the building are equipped with electronict

card readers, controlled by Rusco Electronic Card Entry Access System. A

burglar alarm system has been Integrated with the Rusco system to provide

protection when the facility 1s closed. Smoke detectors, as well as associated

pull stations and fire alarm horns, are provided throughout the building forfire protection. Adequate fire extinguishers and emergency equipment are also

provided. The fire burglar alarms are also monitored by the off-site security

firm. When an alarm sounds, the off-site personnel alert the appropriate

laboratory personnel, the Sheriff's office, or the F1re Department, as

necessary.

CompuChem* Laboratories contains sophisticated, state-of-the-art Instrumentation

and data processing equipment capable of performing most organic and Inorganic

analyses. Two Hewlett Packard-3000 Series 70 mainframe computers are dedicatedto scheduling and tracking sample analyses through the laboratories and are

directly networked to GC/MS Instrumentation. An HP-3000 Series 950 mainframeprovides system redundancy 1n the event of primary system failure, and handles

additional production coordination. One of two HP-3000 Series 39 microcomputers1s dedicated to systems research; the second handles all accounting functions.The Computerized Laboratory Management System (CLMS) 1s accessed by laboratory,marketing, systems, and accounting personnel via more than 90 CRT computer

terminals.

001 0669


The Manager of Facilities and Safety, Manager of Instrumentation, and Manager of

Computer Operations are primarily responsible for the evaluation, selection and

maintenance of all facilities, Instrumentation, and computer equipment,

respectively. The Manager of Facilities and Safety 1s also responsible for

overseeing general housekeeping services and functions as the Laboratory SafetyOfficer. In this capacity, the Safety Officer conducts periodic safety

Inspections and manages the activities of the Safety Committee.

All analytical Instruments are maintained by a staff of full-time servicetechnicians, operating during all three shifts, seven days/week (also available

on-call on weekends). Instrument log books are maintained for each Individual

Instrument In each of the laboratories (GC/MS GC, Inorganics), for recordingroutine maintenance performed by the operator or laboratory staff.

Additionally, service records for each Instrument are kept 1n the Maintenance

Department to record all routine and non-routine maintenance performed by

service technicians.

The Pure Water Room houses a state-of-the-art water purification system.Municipal water 1s fed through two mixed-bed 1on exchange cylinders and a highcapacity activated carbon tank. The effluent 1s pre-pol1shed by two mixed-bedIon exchange columns, distilled 1n a Corning 12-liter all-glass still, thenpasses through a Negapure Polishing System. This final purification processfeeds water through two more mixed-bed 1on exchange cartridges, and activatedcarbon column and a clarifying filter. Water quality 1s monitored dally by an

1n-l1ne specific conductivity meter, and by the various method blank andInstrument blank QC checks performed on the water. A similar system 1s used at

001 0670


an off-site warehouse facility to produce pure water used 1n the trip blanks

that accompany SampleSavers (sample coolers) Into the field during samplingoperations. The Sample Preparation Laboratory and QA SOPs Include additionalInformation regarding the operation of the stills.

Two other laboratories have systems 1n-place to perform additional processing ofthe water from the Pure Water Room. Teflon transfer lines feed the water Into

the Inorganics Sample Preparation Laboratory and Volatile GC/MS Laboratory

systems. Inorganics Lab pure water passes through an additional MHHpore Pure

Water System (with Ion-exchange cartridges and a carbon filter), and water for

the Volatile Lab 1s sparged with nitrogen 1n an all-glass reservoir for 24 hours

prior to use.

The laboratory also has a full complement of support equipment andInstrumentation, such as glove boxes and hoods, walk--n refrigerators, freezer

units, autoanalyzers, and sonlcators.

The following sections describe the laboratory area by function and equipment.

The floor plan was designed to allow for the efficient and secure movement ofsamples and data between work areas.

001 0571


6.2 Laboratory Areas

Shipping and Receiving: This area 1s located adjacent to the laboratory section

of the building. Samples arriving are Identified and Introduced Into the

scheduling and control system. The sample receiving area for environmental

samples has about 1,570 square feet of floor space. The receiving area has 102square feet of bench space for receiving and opening samples, three data entrystations, one laboratory sink and ample storage shelving.

Walk-In Refrigeration System: This area 1s accessed from the Sample

Custodian's area outside of Sample Receiving. This 2,500 cubic feet system has

two Independent refrigeration units, 1s temperature controlled to 4°C +, 2°C and1s equipped with an activated carbon air filtering system, which maintains anenvironment free of organic vapors. The temperature 1s recorded dally. Both

entrances are secured by locks and the temperature-activated alarm system 1stied Into a private security service. In the event of unauthorized access or

temperature fluctuations, appropriate parties are notlfed by the privatesecurity service. A generator maintains the temperature 1n the event of apower failure.

Organic Extractions and Inorganic Preparations Laboratory; This area 1s

equipped with hoods as well as extraction equipment sufficient to process manythousands of samples per month. The environmental sample preparation laboratoryhas 2,008 square feet of space, four 8' fume hoods, three IEC centrifuges, twovacuum ovens, two sinks, six water baths, and 220 square feet of bench space.The air handling system for the sample preparation laboratory was customdesigned for the extraction process. Conditioned 100X outdoor air 1s supplied

FAC 001 0672


Into the room through linear dlffusors and vented through exhaust ducts which

extend from wall-to-wall on the north and south ends of the laboratory. This

method maintains air flow at the work/stations at all times and virtually makesthe room a large walk-In fume hood. A complete air exchange occurs every two

minutes. Separate exhausts are provided for furnaces and hoods. Adequatecabinet space 1s provided. Specially-designed water baths controlled and

programmable to temperature and duration are also used. The glassware

preparation room has 750 square feet of floor space and 1s equipped with two

glassware washers, 26 feet of stainless steel counters with four built-insinks, and one 72 cubic foot annealing oven.

Solvent Storage Area: This area 1s accessible through a secured door adjacent

to the extraction and preparation area. The room 1s designed with reinforcedconcrete walls, an automatic halon fire-extinguishing system, alarm systems anda roof that relieves pressure 1n the event of an accident.

GC Laboratory: The laboratory's nineteen gas chromatographs are equipped

with autosamplers or purge-and-trap devices (Tekmar LSC-2) and are Interfacedwith a Hewlett-Packard 1000 laboratory computer for data processing (all of

which are Installed on a raised computer floor). A variety of detectors areattached to the GCs, Including Flame Ion1zat1on (FID), Flame Photometric,Electron Capture, Thermionic Specific (also called NPD or AFID), Photo1on1zat1on

(PID), and Electrocoulometrlc (Hall) detectors.

GC/MS Laboratory: The special features Included 1n this area are numerous.

All twenty-three GC/MS systems are raised on a computer floor. This allows


gas, water, cooling and exhaust systems required to support each Instrument to

be Introduced to the room Independently, beneath the floor. There are 12

distillation units for cyanide and 8 units for phenols distillation.

Equipment 1s arranged 1n efficient work stations. In this way, specific

Instruments can be utilized for specific types of analyses. Several Instrumentsare physically Isolated from the rest of the GC/MS Laboratory by a glass wall

(with an Independent air handling system) dedicated to volatile organicanalyses. These Instruments are never subjected to semi-volatile work;therefore, cross-contamination of the Instruments 1s eliminated. Furthermore,

each station of Instruments 1s staffed by experts familiar with the procedures

associated with each specific method. This staffing system allows Intimatedally Interaction between the operator, his/her Instruments and themethodologies required. All other Instruments are dedicated 1n a similar

fashion. The GC/MS Laboratory has a total of 3,380 square feet of space, and1s provided with an Individual power supply from a breaker panel locatedwithin the lab. The GC/MS Instruments are powered by three 1-phase, 75 KVA480/220 volt Isolation transformers. Helium, the carrier gas used, 1s suppliedfrom a manifold system 1n an adjacent room through a piping system under the

raised floor. There are three of these systems, each having a catalyticscrubber to remove traces of oxygen and water, prior to entering an Instrument.

The 23 GC/MS Instruments are configured with both packed and capillary GCcolumns, and have accessories for purge and trap, direct Injection, or solidprobe for Introduction of samples. Both electron Impact and chemical1on1zat1on sources are available. Each GC/MS Instrument 1s equipped with Itsown dedicated microprocessor for data processing.

FAC 001 0674


Standards Laboratory: This area 1s separated completely from all other

laboratories and 1s equipped with Its own GC Instrument. Refrigeration, glove

box and hood units are located 1n this area. The entrance to this area 1s

locked at all times and secured by a cypher lock.

Inorganics Laboratory: This area 1s separated completely from all other

laboratories and has Inductively Coupled Plasma (ICP), Technlcon autoanalyzer,

Atomic Absorption Spectrophotometers (AAS) and UV/v1s1ble spectrophotometersystems. Several other analytical Instruments required to perform classical

analyses are also located 1n this laboratory. Hood systems are also an Integralpart of this laboratory.

Mercury 1s detected by flameless-cold-vapor methods established by the USEPA(Cold Vapor Technique). For maximum data management, the Inorganics Laboratory

uses a mini-computer (Digital, PDP11/73) Interfaced to the ICP Instrument(Jarrel Ash, Model 1100).

Extract Storage; Sample extracts are stored 1n specially-designed refrigerationunits located adjacent to the Walk-In Refrigeration System. These refrigerationunits are kept locked and may be accessed only by a sample custodian. Theserefrigeration units are also connected to an alarm system. In the event oftemperature fluctuations outside acceptable levels (4°C + 2°C), appropriateparties are notified by a private security service and the problem 1s correctedby laboratory staff.

0675

Section No. 6.2Revision No. 4

i Date: October 17, 1988I Page 5 of 6

i High Hazard Laboratory; A limited access laboratory has been designed for

sample preparation aspects associated with high-hazard samples. For example,( all samples requiring analysis for 2,3,7,8-TUJD arc prepared 1n this lab.

Access to the laboratory 1s by means of a cypher lock. The hoods are equippedi

with an HEPA filtration unit. Laboratory personnel use more sophisticated

protective clothing than other extraction laboratory personnel (I.e. full sacksuits, booties, face masks, etc).

PAC 001 0676

Section 6.2Revision No. 4Date: October 17, 1988Page 6 of 6

FACILITY SPACE ALLOCATION

TOTAL LABORATORY BUILDING SQUARE FEET 24,005

,' 1. Sample Receiving 1,570 sq. ft.

2. Glassware Prep 750 sq. ft.

: 3. Organic Extractions and 2,008 sq. ft.Inorganics Sample

Preparation

4. High Hazard Lab 450 sq. ft.

5. GC/MS 2,840 sq. ft.

6. Computer Room 1,450 sq. ft.

7. Standards Laboratory 312 sq. ft.

8. Metals (Inorganics) Instrumentation Lab 650 sq. ft.

9. GC Lab 1,200 sq. ft.10. Solvent Storage 542 sq. ft.

< 11. Utility 960 sq. ft.

12. Walk-In Refrigeration System (2 units) 250 sq. ft.

13. Miscellaneous (Canteen, Corridors, 5,000 sq. ft.Rest Rooms, etc.)

14. Office* 6,023 sq. ft.

TOTAL PAMLICO BUILDING SQUARE FEET 55,487

1. Office* 40,142 sq. ft.

TOTAL COMPUCHEM LABORATORIES, INC. FACILITIESRESEARCH TRIANGLE PARK, NC* 79,492 sq. ft,

* Includes both Environmental and Forensic Drug Testing Operations.

001 0677


GAS CHROMATOGRAPH LABORATORY EQUIPMENT

Item

GCGCGCGC

GC

GCGCGCGCGCGCGCGCGC

GC

GC

GC

GC

GC

Model*VARIAN 3700VARIAN 3700VARIAN 3700VARIAN 3700

HP 5880

VARIAN 3400VARIAN 3400VARIAN 3400VARIAN 3400VARIAN 3400VARIAN 3400VARIAN 3400VARIAN 3400VARIAN 3400

VARIAN 3400TEKMAR LSC-2TEKMAR ALSO.I. 442

VARIAN 3400O.I. 4460HNU PI-52

VARIAN 3400TEKMAR LSC-2TEKMAR ALSHNU PI -52

VARIAN 3400TEKMAR LSC-2TEKMAR ALSO.I. 4420

VARIAN 3400O.I. 4460O.I.O.I.HNU PI -52

Serial*

58760308-1371280469-1332968966-1174550509-13

2236A04163200623102309231236233052230823072311

30531441016

3054171-6-9B620045

230618211041620100

200515569026644-5-102

305552 1-605 1C365-6-002005836

CCheml

000000

001177001175001178001173

001174001179

001357

001647

001356001499001362

001176001241001648

000953001316001649

001358001507001508001509

A-D*

2&3741

23

215046910121424

19

20

18

17

16

TypeDUAL ECD AUTOSAMPLERDUAL ECD AUTOSAMPLERFID NPDFID

FID

FPDECD NPD AUTOSAMPLERECD NPD AUTOSAMPLERECD FID AUTOSAMPLERECD FID AUTOSAMPLERECD AUTOSAMPLERECD AUTOSAMPLERECD AUTOSAMPLERECD AUTOSAMPLER

HALL DETPURGE AND TRAPAUTOSAMPLER

PID DETPURGE AND TRAP

PIDPURGE AND TRAPAUTOSAMPLER

HALLPURGE AND TRAPAUTOSAMPLER

PIDPURGE AND TRAPLOOP SAMPLING MODULE

Install

1980198019801982

1982

198619861986198619861986198619861986

1985

1985

1985

1985

1985

SW365OVEN BLUE M SW-11TA-1

COMPUTER HP 1000

CHARCOAL AIR FILTERING SYSTEM

001353 OVEN

ALS SYSTEMDATA PROCESSING

FAC 001 0678

Revision No. 5Date: OctoberPage 2 of 3

17, 1968

GC/MS LABORATORY EQUIPMENT (ENVIRONMENTAL)

OWA I

OWA - 1020OWA - 1020OWA - 1020OWA - 1020OWA - 1020OWA - 1020

102010201020102010201020

OWA - 1020OWA - 1020OWA - 1020OWA - 1020OWA - 1020OWA - 1020OWA - 1020OWA - 1020OWA - 1020OWA - 1020

I NCOS 50

Serial* Type Of Application Installed

OWAOWAOWAOWAOWAOWA

12137-098012391-3-028112141-098012138-098012140-098011957-2-018011957-3-018011957-4-0180

11957-127912391-2-028012391 028112139-098012391-1-038012391-4-038112391-5-038112645-1-118112645-4-118112645-6-128112645-3-118112645-2-1181S12645-5-1281

13954-0387 '

CAPILLARY COLUMN 9/81CAPILLARY COLUMN 9/81VOA-LSC/PURGE AND TRAP 9/81CAPILLARY COLUMN 9/81CAPILLARY COLUMN 9/81CAPILLARY COLUMN 9/81CAPILLARY COLUMN 9/81CAPILLARY COLUMN 9/81VOA-LSC/PURGE AND TRAP 9/81VOA-LSC/PURGE AND TRAP 9/81VOA-LSC/PURGE AND TRAP 9/81VOA-LSC/PURGE AND TRAP 9/81VOA-LSC/PURGE AND TRAP 9/81VOA-LSC/PURGE AND TRAP 6/82CAPILLARY COLUMN 9/81CAPILLARY COLUMN 6/83VOA-LSC/PURGE AND TRAP 6/83VOA-LSC/PURGE AND TRAP 6/83CAPILLARY COLUMN 6/83CAPILLARY COLUMN 6/83CAPILLARY COLUMN 6/83VOA-LSC/PURGE AND TRAP 6/83

HP-GC WITH CAPILLARY COLUMN 1987

001 0679


INORGANIC LABORATORY EQUIPMENT

Item

AUTO ANALYZER II

CIRCULATING BATH

ANALYTICAL BALANCE

ICP

MICROPROCESSORIONALYZER PH METER

UV VISIBLESPECTROPHOTOMETER

CYANIDE/PHENOLSAUTOANALYZER

ATOMIC ABSORPTIONSPECTROPHOTOMETER



VAPOR GENERATIONACCESSORY

MakeTECHNICON

PRECISION

METTLER

JARRELL ASH

ORION

Mode 11

TRAACS 800

MODEL HL 52

MODEL 1100

ORION 901

Serial!

A76373

22483

93353

Installed1987

1987

1980

1986

1979

VARIAN CARY 219

TECHNICON AAII

0438812 1981

GG0797940 1980

INSTRUMENTATION VIDEO 22(857)LABORATORY



AVA 440

2027

2127

2128

1625

1987

1986

1986

1986

°01 0580

.it v . i « i i ' • >- . O.iRevision No. 4Date: October 3, 1988Page 1 of 7

6.4 Instrument Maintenance

Analytical Instruments are maintained by experts employed by CompuChem* on a

full-time basis. Preventatlve maintenance as well as major Instrument repairs

can be accomplished on-s1te. An extensive 1n-house stock of spare parts allows

for rapid repair. CompuChem* maintains service agreements with Instrumentmanufacturers to further assure the operational viability of all 1n-house

equipment.

The operational condition of Instruments 1s one of the keys to successful

completion of analytical tasks. This requirement 1s further magnified by the

necessity to complete large programmatic requirements 1n a limited period oftime. CompuChem's commitment to Instrument maintenance assures clients thatequipment will be available to generate the required data.

In discussing Instrument maintenance services at CompuChem*, a distinction

between GC/MS Instruments and other hardware 1s required. In the case of theGC/MS Instrumentation, CompuChem* staff have full maintenance and repair

responsibility. These staff have been trained by the Instrument manufacturerand are fully qualified to perform the required work. For other Instruments, we

have service contracts for periodic maintenance visits by the vendor, although

maintenance personnel do assess whether repairs can be made 1n-house before

outside vendors are called.

All GC/MS Instrument repair logs and Instrument service records are maintained

1n Individual Instrument files 1n the Instrument repair shop.

FAC 001 0681


All services performed on the Instruments are recorded and filed on an

Instrument-specific basis to maintain an on-going historical record of the date

and type of work performed. Similar records are maintained for preventatlve

maintenance activities. Example 1, beginning on the next page of this section,

shows a typical maintenance record for the GC/MS Instruments.

A procedure manual outlining the proper use of each piece of equipment 1s

maintained. These manuals are located with the Instrumentation and Include

Instructions for use, calibration, and maintenance of the Instrument.

FAC 001 0682

INSTRUMENT NOI ll 2

CC OWM not h*«tl«fl

ENNMFU I

OOMPUCICM SERVICE REPORT R-1234 A

11 OPERATOR: SUMH BMS

oovoo

oo

START DATE

START TIME

0|7

ASSEMBLY NO.

*hi lo

8 ) 6

,1 ,

'loliH.M.hh1 1 1 1 1 1

2|o|

M i l l1 1 1 1 1 1 1 11 1 1 1 1 1 11 1 1 M M 11 1 1 1 1 1 1

| |

| |

| |

| 1

END DATE

END TIMEREV

LEVEL

O|A

|

|

|

j

|

0 | 7

REPAIRCODE

1 <>l«

| |

| |

j

J

|

|

,|oFAILURI

CODE

l°l<

| |

| |

| |

| |

| |

|

,|,

RESPONSE TINE

TOTAL DOWNTIMECOMPONENTDESIGNATOR

1 1'

| |

| |

| |

| |

1 |

4

1 1 •>\ .1*

PART NO.

M i l lI IMIM i l lM i l lII II 1M i l l

m«n<HIMMi l lM i l lMi l lM i l l

S/E L*» Gregory

JOB COMPLETE? YES | X

DESCRIPTION

F-.

OTY

| ,

|

|

|

|

|

NO

COST

1 3)

COMMENTS; 0»«n not h»«tli»9. 24 «olt r»l«y net •ngaglna fomd lu» F4 bloan In yovtr supply. R»pl«c«J fu»* F4,

_______ctMCh»d O4 «oMt. ct>«ch«4 op -«tlon of PC. g«y« b«Cfc to opwctor L.G. ___________________

OPERATOR ACCEPTANCE: I DATE I Ol ?l 2l I TIME! il il ol o IRE V072M216

INSTRUCTIONS

LIST AS 05 FOR OWA05, 12 for OWA12. ETC. THE 4021 GC/MS/DS ISINSTRUMENT 00. ALL STANDALONE DATA SYSTEMS ARE INSTRUMENT 99?

ENTER DATE AS MM/DD/YY; AUGUST 28. 1985 IS 08/28/85. ENTER T I M E BY24-HOUR CLOCK. 9:25AM IS 0925 AND 9s2SPM IS 2125. THE TIME AND DATESHOULD BE WHEN A PROBLEM IS D I S C O V E R E D AND REPORTED VIA THIS FORM.WHO YOU ARE.

COCEA DESCRIPTION • USE THE 3 D I G I T PROBLEM CODE THAT MOST APPROPRIATELY DESCRIBES YOUR

PROBLEM. PLEASE DETAIL THE PROBLEM AS FULLY AS YOU CAN.,

USE BLACK INK ONLY A W R I T E OR PRINT LEGIBLY.

INSTRUMENT NO.

DATE I TIME -

OPERATOR -

PROBLEM COOES(CAUSE 1 EFFECT)

».M.

ANNOT MEET TUNE

(DOS ERRORS -1ST AND FULLYESCRIBE WHATHE DATA SYSTEM

HAS DOING

OCR SENSITIVITY

wRIFTING RET.TIMES

0 SPECTRA OR0 MS RESPONSE

•OFT WAREANOMALIES

•AS CHROM.

ISC DRIVE

RINTER

URGE A TRAP

ACUUM FAULT

IR LEAKS

ERMINAL

"'ATA SYSTEM

tNNOT BOOT

UNKNOWN

000

001

002

003

004

005

006

007

008

009

010

Oil

012

013

014

019

016

REPAIR ACTIONCODES

PIRATE PARTS

ADJUSTMENT - ELEC

ADJUSTMENT - MECH.

REPLACED ASSY.

RETURNED TO VENDOR REPAIR

RETURNED TO VENDORWARRANTY

REQUESTED IN-HOUSEVENDOR SERVICE

WAITING FOR PARTS(NOTE P.O. *>

CLEANED SEPARATOR

CLEANED MASS FILTER

CLEANED SOURCE

REPLACE PART

REPAIR IN-HOUSE

UNABLE TO REPRODUCE

100

102

104

106

108

110

112

114

116

118

120

122

124

126

FAILURE ANALYSISCODES

UNKNOWN

MISCELLANEOUS

OPERATOR ERROR

SOFTWARE

HEADCRASH

MECH. DEFECT

OUT OF ADJUSTMENT

INTERMITTANT

EXCESSIVE NOISE

EXCESSIVE WEAR

SHORTED COMPONENT

OPEN COMPONENT

FAULTY CRIMP

POOR CONTACT

POOR SOLDER JOINT

DIRTY/DUSTY

LEAKING

REPLACE • WITH

1 • ELECTRICAL2 • MECHANICAL3 • VACUUM4 • SOFTWARE

200

202

204

206

208

210

29»

29«

29*

212

214

216

218

220

222

224

226

001 0684

PWEVEWTIVE MAINTENANCE • 3 MONTH INTEHVAL

• WCYENTIVE MAINTENANCE CHKKS AND SCMVICCS OUIOC*

•

ITEMS TO K INSPECTED

STgwa 3 «C

I* l!«« fuso* forttw OC

2. Injoetor for packa<9eel inns

3. Splttlass InJorMonfor capillary colons

4. Injector coptuM Inthe OC

3. C«rfr«r |M ee^MCtlonJoBi H i

e. Corrlcr fM ftltvfn tt» OC

7. riltw. flowcontrol l«r

•• OiptllVf cotton

t. P*ck*d eelimn(glais tyec)

10. ••etod eolwn(Wt«l typ«)

11* OvtKtor port toOC/MS lAtvrtac*

12. OC cool down fan

PROBABLE SltFTOM

Inaetrvo OC, blown fuM

obrh-uct?ofl, looks

lookooo

r •place vfcon nov gatevllndor !• Install oddirty ft (far

oveatsfvo waot, toaksat Injoetlon and lntar>faca pert of ttto iono-haatlng block

KKVICCIMTEMVAL

tf**

X

X

£

2 r«

X

X

«

»

I!1S

X

X

X

X

X

X

X»#

X

X

UK VICEIKTE*NAL

I

NOTE: Applleablara prtantad InOparafor Manual (ott«r*ltc spvelf

roplaea fusa

elaan,Inspact orraplaea asroqwlrod

ropfaea ftltarelaanInspact orroplaea asmadad

Inspect and/or raplaca

WXEOUHE

a proeadurntha Flnntgni), unlasstad.

*Thosa AaTntananca procodyros aioat or oxeood Flnntgan'* rocaa»a»idad orovanttv* •alntonaneachocks and aorvleaa*

FAC 001 0685

REPAIR • PR£*KTIVE MAINTCNA»C£ C*CCKS AW KWVICCS 9UIOC (Cent.)

ITEMS TO 1C INSPECTED

Mass SpaetroMatar

1. Mass Jat sapor *tor

2. Steii Jat aaparatorfarrulas

3* Mass an sly tar hasdanambly (In thavacuum Manifold)

••agnat aall flanga assy*CAi. gas «alva assy*««nt vslva assy••star flow sansor switch

*• -Xiadrueola siass onalysar

9. tloctron •ultlpllar

«. Atcatat vacuu* soaps 12)

7. »falf for turbo pu*p

1. tatiar turbo su*p

». Vacua* aysta*) flltar/drlor

10. Ion Sourca

•Ion sourea fllawont assy•eollaetor•Ions•opartura'Ion volaM

OC/MS Intarfaca Ovan

1. Capillary Intarfaea tubing

2. Saparator tlvart fitting

3. Vaew* dlvart valva

•oaar Modulo

1* MS aowar supply

2. Tarfeo sowar supply

Card Caga ttodula

1. Air flltar at bottom of cagi

2. Fan .

3. Signal cab la onDigital I/O KB

•ftCBWLE SYMPTOM

- .

obstruction or glass

braakaga

gross tasks, oraslstantprassura dua to dagastngof trappad gssas In thavacua* aystanlaakaga. faulty CAL gasprassura (aaa 'Iranigauea)faulty switch

.

dirty oil

aveasslva usa, dirty flltar

lack of aansltlvtty.faulty aaak shapa,no outotuna

• I»B0*4

dirty flltar, obstructionof air flowburnod out fan

9F«vieeIWTEKVAL

V I!

X

X

X

X

X

!11S

X

X

X

II*iiX

X

X•

Sarvlea eoncurrontlywith avary fllswantassambty raplacanant

X

X

X

X

X

X

X

X

X

X

X

X

X

KftVlCCIKTCRNAl.

claan orraplaea

raplaea

Inspaet

InspaetInspactInspaet

Inspact and/or raplaea

svrga waaklyand raplaeaoil

cloan 1Inspaet

roplaeaclam, Inspaetor raplaea asroa.ulrad

claan, Inspactand/or ro-ot oca

awasura »varlfy *CB

claan and/orraplaea

Inspaet forsacura fit

PROCEDURE

•a liar Msnualpg...23

i;

FAC 001 0686

nevctfnvc MAIMTEWCE c*c« AND st*VICES OUIK

ITEMS TO K IWtCTIO

ttova Computer

1. Fan

•erfclM-Claor Olek Drive

1. Output signal

2. Adjustable BC voltages<*5V, 413V, -!3V)

* ra'ls 0"*r

5. iplnd|e chuc* and eona

7. Flied disk

1. Air filter•prof liter•e*ln filler

•. Sloeer ground brush

). t»lndle round brush

1. flow drive belt

~«ti sr^r*

faulty fan rotation

KRVICCINTERVAL

K

5 f !X

X

X

X

X

Tli

\

X

X

».

\

X

X

X

!

s

ICMVICE

1

Inspect and/orreplace

check endverify

cleen and/or replaceclean andInspectclean andInspectInspectand repair

replacereplace

replace

replece

replace

*CCED*E

F/tOEM Msnusl

•/ton Manual

P/EQEM Manual

001 0687

ieî ion no. o.oRevision No. 0Date: October 17, 1988Page 1 of 3

6.5 Material Procurement and Control

CompuChem's Purchasing Department has two prime objectives: (1) maintain

sufficient supplies of all required Items as needed, and (2) encourage all formsof competition 1n order to aggressively seek the best total value 1n a

combination of supply, price, required quality, and service.

Procedures for Purchasing Materials: Department and laboratory managers have

primary responsibility for maintaining adequate Inventory of supplies and

ensuring that all supplies/equipment meet or exceed quality requirements.Managers work through the Purchasing Department to accomplish these objectives.CompuChem* uses competitive Inquiries or requests for bids, along with

appropriate negotiation, to provide equal opportunities for potential andcurrent suppliers to earn CompuChem's business and to allow the laboratory to

seek the best total value. Long-term considerations Include reliability, price,required quality and service. Vendors are encouraged to bring to CompuChem's

attention new or Improved materials, equipment and services. Suppliers mustmaintain the confidentiality of competitively sensitive Information which 1s

obtained from the Purchasing Department or other CompuChem* personnel. Pricesand related Information, whether accepted or not, will not be disclosed.

Each year, various vendors will supply the laboratory with sqlvent/chemicalsamples during the bidding process. The laboratory evaluates each vendor'ssample, as described 1n the next section, before the bid 1s considered by thePurchasing Department. If solvent/chemical quality 1s equivalent, then priceand service are considered. Prices are kept low because of the highlycompetitive market and the high volume used by the laboratory.

001

Revision No. 0Date: October 17, 1988Page 2 of 3

Material Quality Inspection: Managers Interact with the Quality AssuranceDepartment when purchasing supplies/equipment that could potentially affect dataquality, and therefore testing prior to use 1n the laboratory. The Director of

QA (or designated QA staff member) determines the appropriate test procedures

and evaluates the resulting test data. A similar validation process 1s used 1ntesting new Instrumentation, as described In Appendix A. All new lots of

standards, reagents, and glassware are tested as described 1n section 9.2 of theQA Plan and 1n the QA SOP Manual. The quality testing of solvents and other

high-volume chemicals 1s described further 1n the following section.Additionally, the laboratory continually evaluates the Integrity of thesematerials by performing the routine QC method blanks with every sample batch asdescribed 1n sections 9.2 and 9.3 of the QA Plan.

When variability 1s exhibited \r\ the quality of vendor-supplied materials orservices, the laboratory/department manager 1s responsible for working with the

Purchasing Department to find a suitable alternative.

Chemical and Standard Inventory Procedures; All chemicals other than organic

standards are Inventoried by appropriate laboratory manager and re-ordered asneeded, with adequate time allowed for order processing, shipment and qualitytesting. The vendor supplying extraction solvents first provides a test samplefrom a particular solvent lot. After testing by the laboratory, If the lot 1sapproved, several cases of the lot are purchased, with the remaining cases ofthe same lot stored by the vendor. The vendor 1s responsible for keepingInventory of the solvent lot, and when only a few cases remain, provides the

laboratory with a test sample from a new lot. The process 1s repeated so that

FAC 001 0689


a second approval lot 1s Immediately available once the first 1s consumed. Thelab manager maintains files of all test data to verify solvent purity. Allextractions are traceable to the approved solvent lot used 1n samplepreparation.

Organic standards are prepared Internally 1n the Standards Laboratory, and theStandards Laboratory Chemist 1s responsible for maintaining adequate Inventories

and Initiating standard purity testing and tests of each standard preparation

lot, as described 1n section 9.2 of the QA Plan and 1n the QA SOPs.

Solvent Storage and Waste Disposal: All solvents In use 1n the laboratory are

kept 1n solvent storage cabinets, which are vented and specifically designed forthis use. Adds are kept 1n a separate, specially designed storage cabinet.Solvents and other chemicals not 1n use are stored 1n the Solvent Storage Room,described 1n section 6.2. Periodically, a waste disposal firm removes, thelaboratory's waste, stored*1n 55-gallon drums, to a licensed hazardous waste

landfill.

FAC 001 0690


7.0 Data Generation

To assure that all data generated are scientifically valid, defensible,comparable, and of known precision and accuracy, the QA Plan provides for the

use of QA Project Plans and SOPs.

7.1 Quality Assurance Project Plans

In some cases, QA objectives specific to a client's project must be Identified.CompuChem* assists these clients 1n assembling specific QA Project Plans(QAPPs). When required, such QAPPs should contain the following Information, as

applicable:

— Title Page, with provision for approval signatures

—- Table of Contents

— Project Description—- Project Organization and Responsibilities— QA Objectives for Measurement Data, 1n terms of precision, accuracy,

completeness, comparability, and representativeness—- Sampling Procedures

— Sample Custody— Calibration Procedures and References— Analytical Procedures— Data Analysis, Validation, and Reporting—- Internal QC Checks— Performance and Systems Audit— Preventatlve Maintenance Procedures and Schedules— Specific Procedures to be used to routinely assess data precision,

completeness, accuracy, comparability, and representativeness ofspecific measurement paramenters Involved.

FAC 001 0691

ic- v. . w". I'u . / . IRevision No. 4Date: October 17, 1988Page 2 of 2

—- Corrective Action

— QA Reports to ManagementQA Project Plans provide for the review of all activities which could directlyor Indirectly Influence data quality and the determination of those operations

which must be covered by SOPs. They are prepared 1n document control format,with provision for revision, as needed, and with a record of the official

distribution. The quality requirements of proposal requests from prospectivecustomers shall be Identified upon the Initial review and evaluation of the

requests. When the quality requirements have been Identified, the designated QAstaff member shall ensure that they are adequately addressed 1n the QAPP.

The following are Quality Assurance Program objectives to be met as a projectbecomes operational:

— Development of QA Project Plan for the project, 1f required by thecustomer, or advisable per management request.

—- Assignment of responsibilities for achieving the required quality ofmaterials, services, and quality assurance.

— Organizing and staffing appropriately to Implement the quality assuranceactivities.

— Development of working plans and procedures (Including SOPs, 1fnecessary) to Implement the QAPP.

— Coordination of QA activities with the customer, subcontractors,suppliers and vendors, etc.

~ Periodic QA assessment as described 1n sections 4.5 and 10.0.

FAC 001 0692

Revision No. 4Date; October 17, 1988Page 1 of 3

~L2 Standard Operating Procedures

Introduction; SOPs are developed and used to Implement routine QC requirementsfor all monitoring, repetitive tests and measurements, §nd for Inspection and

maintenance of facilities, equipment, and services.

The Environmental Laboratories' procedures are documented by separate SOPmanuals; the Sample Preparation Procedures (SPPs) and Instrument Procedures(IPs) are contained 1n one volume, while the ten-analytical SOPs are contained1n a second set of volumes.

The Indices for both procedure manuals (SPPs/IPs and non-analytical SOPs) are

Included 1n Appendix C. These Indices should provide a good understanding of

how thorough the documentation of procedures 1s at CompuCtvem*; the documentationof procedures 1s considered to be critical to the assurance of data quality.

Standard Operating Procedures (SOPs) are distributed by area; each section of

the Environmental Laboratories receives Its own set of SOPs. Complete copies ofthe SOP Manual are maintained 1n the library and the Quality Assurance office.

The organization of the SOP Manual reflects the progress of a sample through thelaboratories. For Instance, a sample first arrives 1n the Receiving Area (SOPsIncluded 1n Production, Planning and Control); 1t 1s prepared as necessary foranalysis (SOPs Included 1n the Sample Preparation Laboratory); 1t 1s analyzed asnecessary (Included 1n separate sets of laboratory SOPs); the data 1s thenprepared, reviewed, and reported,.is Indicated.

If a question,arises concerning the procedure followed for an activity 1n one ofthese areas, the SOPs for that particular area are consulted to resolve the

Revlson No. 4Date: October 17, 1988Page 2 of 3

question. These SOPs are also a valuable source of material for trainingpurposes.

Completing the Initial Documentation Form: Each set of SOPs 1s accompanied by

an Initial Documentation Form. This form Is located at the end of each separate

set of SOPs and serves as the procedures' sign-off documentation, Indicatingthat the procedures are consistent with current laboratory practices. After thespecific laboratory manager has determined that the procedures are accurate,

he/she signs the Initial Documentation Form for those procedures and returns a

copy to the Communications Specialist 1n the Quality Assurance Department.

The Initial Documentation Form 1s also used to ensure that personnel understand

the tasks and responsibilities of their positions. All personnel review theSOPs for their positions and, after the area manager believes the personresponsible for these tasks has mastered the SOPs, both the manager and theemployee sign and date the form. Copies of the completed form are forwardedto the Communications Specialist and are filed 1n the employee's personnelrecord 1n the Human Resources Department.

Revising and Creating Standard Operating Procedures; Standard OperatingProcedures are updated as laboratory procedures change, and 1t 1s oftennecessary to create new SOPs, as new procedures are developed to meet theanalytical and Information needs of CompuChem's clients. The current proceduresfor revising and creating SOPs (Quality Assurance SOPs 3.2 and 3.3) can be found1n the back of each section of SOPs. The Communications Specialist 1sresponsible for Integrating new/revised SOPs Into proper document controlformat, and for maintaining a record of the official distribution (also done

001 0694

. ..„. .


for the QA Plan and other critical QA documentation).

The Quality Assurance Department supports all sections 1n developing, writing,editing, revising and maintaining current, accurate Standard Operating

Procedures. The Director of QA or QA Department deslgnee also reviews and

s1gns-off all new or revised SOPs. All SOPs remain the property of CompuChem*

Laboratories, Inc., and the content of all SOPs 1s strictly CONFIDENTIAL.

FAC 001 0695


8.0 Data Processing

This section summarizes the manner 1n which all aspects of data proccesslng are

managed and evaluated 1n order to maintain data Integrity and characterize data

quality. These processes Include data collection, validation, storage,transfer, and reduction. Specific details of the procedures used by theautomated data processing and computer systems operations are documented 1n the

Individual laboratory SOPs and the Report Preparation Department SOPs.

8.1 Collection

Analytical data are generated from the GC/MS computer software, GC computer, ICP

computer, Atomic Absorption Spectrophotometers, Autoanalyzers, and associated

laboratory Instrumentation. The outputs Include Identifications of compounds

or elements, concentrations, retention times, and comparisons to standards.

Outputs are 1n graphic form (chromatograms), bar graph (spectra) and printed

tabular form. The outputs are 1n standard format specified for each analysis

type and are monitored for consistency. If Incomplete or Incorrect output 1s

generated, corrective actions are taken according to SOPs established for each

type of analysis and consistent with the manufacturer's recommendations.

All outputs of each of the Instruments may be checked manually for eachprocedure (e.g., GC chromatographlc peak area Integration and calculations maybe reviewed manually for baseline designation and quantltatlon). In the datareview process (see section 8.2, Validation), the data produced are compared toInformation concerning the sample processing history, sample preparations,sample analysis, associated QC data, etc. to evaluate the validity of the

results.

FAC 001 0696


Ancillary data produced for Internal records and which may not be required by

the customers as part of the analytical data package Include the following:laboratory worksheets, laboratory notebooks, sample tracking system forms,

Instrument logs, calibration records, maintenance records, standard prepartlon

records, and associated quality control sample data. These data are availablefor Inspection during audits to verify the validity of data and are alsodeliverable, depending on the client's needs.

A complete record of each sample's history 1s available for documenting Its

progress through the laboratory from sample receipt to reporting. Document

control (see section 4.4 of the QA Plan) and cha1n-of-custody (see Appendix E)requirements present additional Information describing these documentation and

archiving processes.

FAC 001 0697


8.2 Validation

Data validation takes on two scales. First, the Quality Assurance Department 1s

charged with the responsibility of monitoring all laboratory QC activities, and

to verify that systems are 1n control. These responsibilities and the manner 1nwhich they are executed are described 1n the QA SOPs as well as this QA Plan.

The QP Department therefore plays a role 1n data validation 1n the context ofthe overall QA Program.

Of course, data validation also occurs on a sample-by-sample basis. This 1s theresponsibility of the various levels of data review taking place within thelaboratory. The first level of review occurs "at the bench"«th1s 1s theInitial review by the Instrument operator or analyst, responsible for assessingthe following:

- cross-checking all sample Identification numbers on worksheets, extractv1als/d1gestate bottles, and Instrument outputs

- calculation of surrogate recoveries and Internal standard responses (whenapplicable), and verification that QC acceptance criteria are met.

- verification that all calibration, tuning, linearity, and retention timedrift checks are within QC acceptance criteria

- verification that all target analytes are within the Instrument'sanalytical range and deciding on appropriate dilutions when necessary

- determination that peak chromatography and other Instrument performancecharacteristics are acceptable

- verification that cha1n-of-custody 1s Intact based on accompanyingpaperwork

The second level of review 1s performed by the 1n-lab Data Review staff. In the

GC/MS Laboratory, these reviewers are all experienced Mass Spectroscoplstsqualified to perform mass spectral Interpretation. GC Lab and Inorganics LabData Reviewers are degreed, senior-level chemists. The Senior Data Reviewer,

FAC 001 0698

ic- L iwfi aj . o. tRevision No. 3Date: October 3, 1988Page 2 of 3

Manager of Data Review or Lab Manager also audit a percentage of these dataprior to being released to the Report Preparation Department. In-Lab Data

Reviewers verify all assessments previously made by the operator/analyst, andalso evaluate the following:

- verification that all quality control blanks meet QC requirements forcontamination, and that associated sample data are appropriatelyqualified when necessary

- calculation of matrix spike recoveries and duplicate RPDs, andverification that accuracy and precision QC criteria are met

- comparison of all Injections of a sample, and comparison of matrix spikeswith the original unsplked sample, for acceptable replication

- qualitative Identification of all target analytes using specific SOPInterpretation criteria

- verification of computer quantHatlon of all target analytes, Includingevaluation of Extracted Ion Current Profiles (EICPs) and of chromatogramsfor proper resolution and Integration, when necessary

- verification that analytical worksheets have been completed by theoperator/analyst. Including date and Initials

- for pesticide GC/MS or GC confirmation analyses, verification that targetanalytes were within retention time windows and/or evaluation of spectrafor proper Identification, and comparison to Initial analysis

- for GC/MS analyses, evaluation of Library Search mass spectra,characterization of tentatively Identified compounds, and verification ofcalculations for estimated concentrations of these compounds

- verification that GLP was followed relative to the correct procedure 1nmaking changes to data

The completed data package, which has been reviewed on an analytical fractionbasis (I.e., volatlles, adds, base/neutrals, pesticides), 1s then forwarded tothe Report Preparation Department. The package 1s then Integrated with otherfractions from the same sample, and with associated deliverable Items asrequired by the client, and forwarded to the Final Technical Review staff for

FAC 001 0699

j Section No. 8.21 Revision No. 3[ Date; October 3, 1988I Page 3 of 3

'i

II!: the third level of review. The Final Technical Reviewer, also a senior chemist

and experienced data validation specialist, assesses the complete data report(or "case", for CLP-format reports) and double-checks all Hems previouslyvalidated by the 1n-lab Data Reviewer. Additional assessments Include thefollowing:

- review of all data summary documents and verification of correcttranscription from raw data

• comparative evaluation of data from Individual fractions of a sample, andof samples from the same site, project or case, for consistency ofanalytical results and resolution of discrepancies

- checks data report or case for completeness• for CLP-format reports, a "case narrative" must be written that

authorizes release of the data, provides end-users a "history" of thesample processing, documents the quality control process used andexceptions to Statement-of-Work criteria, and summarizes any correctiveactions taken.

Upon completion of all levels of review and authorization of data releas* by theFinal Technical Reviewer, the data report (or case of reports) 1s sent to theDellverables Department for mailing.

Senior members of the Quality Assurance Department are also required to auditapproximately 10% of all analytical data. The QA auditor performs the sameassessments as the Final Technical Reviewer. Findings from these data auditsare presented In a report to management, as described 1n section 10.0 of the QA

Plan.

FAC 001 0700


8.3 Storage

At every stage of data processing at which a permanent collection of data 1sstored, procedures are established to ensure data Integrity and security.Specific QA Project Plans Indicate how specific types of data are stored withrespect to media, conditions, locations, retention time, access. The followingchart Indicates general guidelines as detailed 1n Production, Planning Control

SOP 2.9:

Media

MagneticTape

Conditions

Hardcopy lockedwarehouse

lockedwarehouse(environmentcontrolled)

location

off-site

off-site

Retention Time

client-specific

Indefinitely

AccessDocument Custodianor other designatedpersonnel

Document Custodianor other designatedpersonnel

FAC 001 0701

Oc- . . w '. i>^ . G . ->Revision No. 3Date: October 3, 1988Page 1 of 1

8.4 Transfer

All data transcriptions for final reports to clients are perfomed by ReportPreparation Clerks. For non-CLP reports, the reportable data 1s reviewed and

approved by the Final Technical Reviewer, then word-processed by computer.

Validation of the word-processing function 1s performed by a proofreader prior

to release of the data. For CLP reports (whether to EPA or commercial clients),all raw data are reduced Into deliverable format by Report Preparation Clerks,Including the summary of data onto forms required by the Statement-of-Work.

Data summaries are accomplished by utilizing a PC-based software system thatextracts data directly from the laboratories' computers. The data are then sent

to the Final Technical Reviewer for validation. In either case, the Final

Technical Reviewer 1s provided with both the deliverable report and thenon-deliverable back-up data, and must validate all transcription processes.

PAC 001 0702


8.5 Data Reduction

Data reduction Includes all processes that change either the Instrument/computer-

generated values, quantity of data values or numbers of data Items, andfrequently Includes computation of summary statistics. Documentation of the

calculation process 1s required. In most cases, a programmable calculator,PC spreadsheet or computer program 1s used 1n this process. The documentation

allows the reviewer to verify the validity of the data reduction process. All

computer-generated compound lists containing the reportable results Include

formulae used 1n performing the calculations.

CompuChem's policies regarding the use of significant figures and roundlng ofresults are outlined 1n Appendix H. An extra significant figure 1s carriedthrough all calculations until the final, reportable result 1s generated.Analytical results are never corrected for blank (background) contamination, butare flagged and footnoted appropriately.

FAC 001 0703


9.0 Data Quality Assessment

9.1 General Quality Assurance Program Objectives

In order to accomplish the objectives of the QA program as described 1n theQuality Assurance Policy Statement, Section 3.0, the program must:

assess the capabilities of analytical methods for meeting user's needs1n terms of accuracy, precision, completeness, representativeness, andcomparability;

establish and monitor the routine operational performance of ourlaboratory through appropriate systems checks to ensure that allaspects of the QA Program are operative;

conduct both scheduled and unnanounced audits, as well as blindproficiency tests, to assess laboratory performance; and

assure that corrective actions are taken and that system control hasbeen restored prior to resuming sample analyses.

The first of these processes will be discussed 1n this section. Section 9.2describes the laboratory's methods for attaining routine quality controlrequirements, and section 9.3 describes the specific QC requirements used toensure that all aspects of the Organic and Inorganic programs are 1n control.Auditing programs, proficiency testing programs and corrective action proceduresare discussed 1n section 10.0.

The following 1s a general overview of the laboratory's QA objectives forprecision, accuracy, representativeness, comparability, and completeness.

Precision: The Laboratory objective for precision 1s to meet or exceedthe method-, or client-specified precision requirements as applied to samplesof similar matrix and concentration. Relative Percent Difference (RPD)criteria, published by the USEPA as part of the Contract Laboratory Program

001 0704


(CLP) statements-of-work for organic and Inorganic analyses, and those

determined from Internal laboratory performance data, are used to evaluateprecision between matrix spike duplicates. The formula for determining RPD 1s:

I MS - MSD I X 100 « Relative Percent DifferenceVi (MS +MSD)

MS • spike recovery for matrix spikeMSD « spike recovery for matrix spike duplicate

Accuracy:

The Laboratory objective for accuracy 1s to meet or exceed the method-,

contract-, or cllent-spedfled accuracy requirements as applied to samples ofsimilar matrix and concentration. Percent Recovery Criteria, published by theUSEPA as part of the CLP statements-of-work for organic and Inorganic analyses,those published 1n the Federal Register (40 CFR Part 136, October 26, 1984),and those determined from Internal laboratory performance data, are used to

evaluate accuracy 1n matrix spike, matrix spike duplicate, and blank spikeQuality Control samples. The formula for determining accuracy 1s:

US - US x 100 « Percent Recovery

MS • concentration of target analyte 1n spiked sampleUS « concentration of target analyte 1n unsplked sampleS • spike standard concentration

Completeness: CompuChem's objective for completeness 1s to be able to provide

unqualified data of the highest quality for 1001 of samples. Factors beyond thelaboratory's control that adversely affect completeness objectives Include:

— receipt of samples 1n broken containers;— receipt of samples In which cha1n-of-custody or sample Integrity 1s

compromised In some way;

001 0705


— samples received with Insufficient volume to perform Initial analyses orrepeat analyses should Initial efforts not meet QC acceptance criteria;

« Improperly preserved samples;

— samples held 1n the field longer than expected, thereby jeopardizingholding time requirements;

— Incorrect or Incomplete Information given to the laboratory, resulting1n the application of Incorrect methods; and

—- assessment by end-users using criteria other than those stated 1napplicable method references.

When requested, the completeness of an analysis can be documented by Including1n the test report sufficient Information to allow the data user to assess thequality of the results. This Information may Include such Hems as:chromatograms, mass spectra, a summary of quality control sample results, andthe tabulated analytical results. Additional results, up to and Including alldata sufficient to recreate the entire analytical process, are optional

deliverable Items. These may Include lab worksheets, calibration data, allquality control sample data, and Internal cha1n-of-custody documents. Thehighest level document emulates that required under the CLP, and 1s Intended asa legally defensible document 1n Itself. The raw data (prior to data reduction)are archived Indefinitely on magnetic tape and stored 1n a secured facility.

RepresentativenessRepresentatlvlness 1s a quality characteristic, and 1s considered a goal to beachieved rather than a quantitative measurement. It describes the degree towhich the analytical results of a particular sample are representative of theresults that might be expected from other samples taken from the same site at

the same point 1n time.

FAC 001 0706


For many sample types, true representativeness can be accomplished by careful

collection planning, sample compositing, and/or sample splitting. Soil samples,

and samples of complex or Inhomogeneous matrix, usually present the greatest

difficulties for samplers and analysts alike. Sampler should make every effort

to homogenize the sample during collection, and laboratory technicians must,whenever practical, homogenize or thoroughly mix the sample prior to removing

allquots for analysis. CompuChem's Sample Preparation SOPs Include specificprocedures for compositing and homogenizing as-received samples.

The manner 1n which the data are correlated to the particular sampling episode

and sample s1te(s) are major condlseratlons when evaluating representativeness.When the laboratory 1s aware of conditions adversely affecting datarepresentativeness, a QualHty Assurance Notice or Laboratory Notice 1s Included

1n data packages to qualify results and provide guidance 1n Interpreting data

useabHUy.

Comparability

The analytical results can be compared to results of other laboratories becausethe objectives of the laboratory for comparability are to:

— demonstrate traceabHUy of analytical/calibration standards to NBS, EPAor other certified sources;

— use standard methodology;— apply appropriate levels of quality control within the context of the

QA Program; and— participate 1n Interlaboratory studies and Independent proficiency

testing programs to document laboratory performance.

FAC n °707


By using traceable standards and standard methods, the analytical results can be

compared to other laboratories operating similarly. The QA Program documents

quality control performance, and the Interlaboratory studies document

performance compared to other laboratories. Additionally, Internal quarterly

blind proficiency studies are Instituted as a means of monitoring1ntralaboratory performance.


9.2 Methods for Attaining Routine Quality Control Requirements

The analytical and quality control requirements for each sample are achieved bymeans of the Computerized Laboratory Management System (CLMS) at CompuChem*.The CLMS, operated by one of the mainframe computers and accessible from any ofmore than 90 CRT terminals, uses a system of Analysis Codes to schedule theappropriate analytical procedures and the QC samples required to be processed

with each batch of samples.

The Analysis Codes have associated with them Instrument Procedure (IP) Codes,Sample Preparation Procedure (SPP) Codes and Quality Control Counters, all

defined 1n the CLMS system, to accomplish these requirements. The IP and SPPcodes are linked directly to the laboratory SOPs for these procedures. The QCCounters define the types and frequencies of QC samples associated with eachbatch, and are driven by method, contract, QAPP and/or statement-of-work (SOW)requirements. When specific methods are required, such as the CLP Organic andInorganic SOW methods, Test Methods for the Evaluation of Solid Waste (SW-846,3rd Ed.), or the Federal Register (40 CFR Part 136, October 26, 1984) methods,counters are defined to produce the types and frequencies of QCs and specified

1n the reference. Even when not specified by the method, the counters are•

defined to provide for the additional preparation and analysis of a LaboratoryControl Sample (Blank Spike), used to evaluate laboratory performance and samplematrix Interferences for each batch.

Counters may be redefined to allow for specific requirements of a QAPP, statecertifying agency or EPA region. Only the Director of QA has final authorityfor altering or creating new QC counter definitions.

PAC 001 0709


The following two sections provide additional details regarding the manner 1nwhich precision and accuracy are determined for organic jnd Inorganic analyses.

Surrogate and Spike Standard Recoveries

A minimum of three surrogate standards are added to each organic sample

requiring GC/MS analysis for volatile, add or base/neutral compounds. Forpesticide and herbicide analysis, one surrogate 1s add«d for each. Inorganic

and Organic Matrix Spikes and Blank Spikes (Laboratory Control Samples) are

similarly fortified with spike standard solutions containing target analytes of

Interest. The recovery of these standards 1s quantitatively measured duringanalysis, and historical records maintained on the percent recovery for each

sample. Surrogate and spike compound recoveries must meet acceptance criteriabefore the analytical data will be released. In some Instances the samplematrix may produce Interferences which adversely affect recoveries. Surrogaterecovery Interferences must be confirmed by repreparatlon and reanalysls of thesample. When a Matrix Spike test falls sp1k« recovery rrHer1a, the LCS must beanalyzed. If the LCS test falls, the batch must be reprocessed, 1f 1t passes,the matrix effect 1s confirmed and the affected data are qualified by a QualityAssurance Notice.

CalibrationsInstruments must be calibrated and recalibrated at regular Intervals asspecified by the applicable method, and consistent with tie manufacturer'srecommendations. The nature and frequency of such checks are specified 1n theInstrument Procedure SOPs. The laboratory maintains adequate records of allcalibrations, recallbratlons and In-service checks of Instruments. All

FAC 001 0710

Section No. 9.2Revision No. 5

1 Date: October 17, 1988Page 3 of 5

calibrations are traceable to primary standards of measurement. Where the

concept of traceablHty of measurement to primary standards 1s not appHcaple,tê laboratory provides satisfactory evidence of correlation or accuracy of testresults.

Analysts, 1n-lab Data Reviewers, Final Technical Reviewers, and QA staff verifythat Instrument calibration data meet all QA/QC objectives. Forms are checked

for calculation and procedural errors, and recurring errors are brought to the

attention of the senior laboratory staff members or laboratory management forcorrective action. Refer to section 9.3 for further discussion of calibration

verification of the GC/MS, GC, ICP, and AA systems.

Other measurement devices, such as balances and thermometers, are also

calibrated against certified sources and a certificate of the calibrationmaintained with the laboraotry manager and with QA records. All balances are

calibrated dally or with each use, using certified Class-S weights, andIndependently on an annual basis through the balance vendor's service contract.All thermometers are traceable to the laboratory's NBS-calIbrated thermometer,and the traceabllUy records maintained by the Sr. Standards Chemist. The

calibration of thermometers and balances 1s further described 1n the QA SOPManual.

The temperature calibration of all laboratory ovens 1s verified annually by theInstrument Maintenance Department. A calibrated thermocouple, linked to adigital temperature display, 1s used for this measurement and the readingsrecorded 1n a calibration logbook. Details of the calibration procedures and

temperature accuracy are described 1n the Instrument Maintenance SOP Manual.

pAC ooi 0711


£C Checks for Sources of Contamination

A method blank 1s prepared at the frequency specified by the referenced method.

The purpose of the method blank 1s to ensure that contaminants are notIntroduced by the glassware, reagents, standards, personnel, or samplepreparation environment. For volatile analyses, an Instrument blank 1s alsoanalyzed during each calibration shift to verify that contaminants are not being

Introduced by components of the Instrumentation or analytical laboratory.

Criteria for the evaluation of these blanks are presented 1n section 9.3.

Various routine QC checks are also 1n place to verify that new lots ofglassware, reagents and standards, decontaminated glassware, sample storage

areas (Including refrigerators), and water purification systems are

contaminant-free. Details of these QC checks are contained within the QA SOPManual.

QC Standards Preparation ChecksAll calibration standards are traceable to the National Bureau of Standards(N6S) or EPA whenever such standards are available. Commercial sources ofstandards and reagents are checked for purity, and approved, prior to their useIn sample preparation and/or analysis.

All organic standards prepared for use throughout the laboratory are assignedtwo code numbers, one Identifying the standard type, and a second Identifyingthe Individual preparation lot. The standard code numbers are entered 1n abound standard preparation logbook with all Information regarding thepreparation of that standard, I.e., date, technician, name of each compound andamount used, final volume, solvent used, and a vendor code. The vendor code

FAC 001 0712


traces the preparation of that lot to the vendor supplying the standard

material, the vendor's lot number, and the particular bottle or ampule fromwhich the material was taken. All standard containers are labeled with thestandard's Identification code and lot number code, Initials of technician, and

date of expiration.

The Instrument response obtained for each compound 1n a newly prepared standard

1s compared to the response obtained from the previously approved standard. Thetwo standards (for all but a few compounds recognized as being chromatographablyatypical) or the new standard may not be used until the discrepancy has beenresolved. The working lifetime of standard preparations are dependent upon thecompound types comprising the standards. Shelf-Hfe of standards 1s determinedduring storage stability studies carried out by the Standards Laboratory. Most

standards are prepared with far greater frequency than recommended by EPA, and

1n no case 1s the recommended frequency exceeded.

PAC 0713


9.3 Specific Routine Quality Control Requirements

Because of the large number of parameters and potential sample matrices, 1t 1sdifficult (and Impractical, under most applications) to develop precision andaccuracy objectives and control limits for every parameter 1n every matrix.

Therefore, 1t 1s necesary to extrapolate this Information from a limited numberof parameters and/or matrices. The laboratory accomplishes this by using

surrogate standards 1n all organic sample analyses, by spiking randomly chosen

samples with various target analytes, and by producing a laboratory control

sample (spiked blank matrix) with each batch of samples.

The QA Department plots control charts for Laboratory Control Samples (BlankSpike) and Blanks on a monthly basis as described 1n Section 10.0.

Additionally, control charts are plotted quarterly for Matrix Spikes andproduction samples for each sample matrix, concentration-level (Low/MediumLevel), and sample type (add, volatile, etc.) For all CLP analyses, precisionand accuracy data are required to be tabulated and reported on the "MS/MSD FormIII". These data are then statistically analyzed by the USEPA (EMSL-Las Vegas),and presented periodically to all CLP labs 1n "Spike-Exceptions Reports." Inthis way, both 1ntra-lab and 1nter-lab trends 1n QC results can be observed.

The following sections describe the primary QC requirements for both Organic and

Inorganic Programs.

Organic Program QC RequirementsGC/MS Calibration: The GC/MS Instruments must first be standardized (this word1s often used Interchangeably with "calibrated") according to the manufacturer'sprocedures using a standard called FC-43 (perflurotr1butylam1ne). Once every 12

FAC 001 0714


hours the GC/MS Instrument 1s "hardware" tuned using eitherDecaflurotrlphenylphosphlne (DFTPP) or Bromofluobenzene (BFB), depending on thetype of analysis being performed. Ths1 standardization assures that otherInstruments both within and outside the laboratory will be operating under

similar conditions, and assures comparability of data generated under thoseconditions.

The mass spectrum from the DFTPP or BFB analysis must meet the criteria

described 1n the USEPA CLP Organic Statement-of-Work (which are Identical to

those specified 1n SW-846 (3rd Ed.) and 40 CFR Part 136). For the analysis ofthe sem1volat1le extractable compounds, DFTPP 1s used 1n tuning the Instrument.

The DFTPP key 1on abundance criteria are:DFTPP KEY IONS AND ION ABUNDANCE CRITERIA

Mass Ion Abundance Criteria

51 30.0 - 60.0 percent of mass 19868 less than 2.0 percent of mass 6970 less than 2.0 percent of mass 69127 40.0 -60.0 percent of mass 198197 less than 1.0 percent of mass 198198 base peak, 100 percent relative abundance199 5.0-9.0 percent of mass 198275 10.0 - 30.0 percent of mass 198365 greater than 1.00 percent of mass 198441 present but less than mass 443442 greater than 40.0 percent of mass 198443 17.0 • 23.0 percent of mass 442

For the analysis of volatile organic compounds, BFB 1s used 1n tuning the

FAC 001 0715


Instrument. Key 1on abundance criteria for BFB are:

BFB KEY IONS AND ION ABUNDANCE CRITERIA

Mass Ion Abundance Criteria

50 15.0 - 40.0 percent of mass 9575 30.0-60.0 percent of mass 9595 base peak, 100 percent relative abundance96 5.0 • 9.0 percent of mass 95173 less than 2.0 percent of mass 174174 greater than 50.0 percent of mass 95175 5.0 - 9.0 percent of mass 174176 greater than 95.0 percent but less than 101.0

percent of mass 174177 5.0 • 9.0 percent of mass 176

The bar graph mass spectrum and mass listing serve to document the proper tuning

of the GC/MS syste-n.

Once the Instrument has met key 1on abundance criteria for the above mentioned

tuning compounds, the GC/MS 1s calibrated. Calibration curves are generated asoutlined 1n the CLP Statement-of-Work and 1n the Federal Register 600-ser1es and

500-serles methods.

After the Initial Calibration curve 1s established using several differentstandard concentrations (as specified 1n the method), the calibration linearityand system performance are verified every twelve hours by analyzing theContinuing Calibration standard. If significant variation 1n compound relativeresponse factors or loss of Instrument sensitivity has occurred, a new InitialCalibration curve must be generated. The criteria for determining acceptableContinuing Calibration responses are outlined 1n the CLP Statement-of-Work, theFederal Registers for wastewater and drinking water analyses, and SW-846 (3rd

Ed.).

FAC 001 0716


The analyst may not proceed with sample analyses until the Instrument has met

tuning requirements and the Continuing Calibration standard 1s shown to bewithin specific criteria when compared with the Initial Calibration curve.

6C Calibration: The GC Instrument (with EC detector) 1s calibrated for

pestle1des/PCBs analysis as described 1n the CLP Statement-of-Work, SW-846 (3rdEd.) and CFR Part 136. This calibration Includes a one-time (or each time a new

GC column 1s Installed) determination of retention time windows for each target

analyte and the surrogate compound, Dlbutylchlorendate (DBC). These retentiontime windows are used to make tentative Identification (followed by aconfirmation analysis on a dissimilar column). These data are retained by theGC Laboratory and made available during on-s1te laboratory evaluations.

The external standard method 1s used for all analyte and surrogate quantltatlons.Once the Initial retention time windows are established, the laboratory may

proceed with the routine calibrations following 40 CFR Part 136 or SW-846 (3rd

Ed.) requirements, or following the CLP requirements for a 72-hour sequence.

Certain "Evaluation Standards" and "Individual Standards" are used to verifyInstrument linearity, Endrin and/or 4,4'-DDT degradation, retention time shift

and windows for that sequence, and Instrument stability (based on variations 1ncalculated calibration factors for each target analyte) over the course of the72-hour sequence. Details of the composition and calibration of these standardspresented 1n the CLP Statement-of-Work and 1n the GC Laboratory SOP Manual.


Method Blank/Instrument Blank Assessment: CompuChem's policies for allowable

levels of contamination are more stringent than those specified 1n the CLPStatement-of-Uork. For common laboratory solvents (methylene chloride andAcetone) and phthalate esters, the maximum allowable level of contamination 1nmethod or Instrument blanks 1s twice the method detection limit, with certainexceptions. These criteria are waived 1f holding times are 1n Jeopardy of beingexceeded. Additionally, the analysis of low concentration levels of volatileorganlcs 1n soil presents a special case. This analysis Involves a heated purgeand trap technique and any contamination detected 1n the associated method blank1s always higher than an associated low level water blank, analyzed by roomtemperature purge and trap. The objective for the low concentration level soilmethod blank 1s to be no higher than twice the detection limit, however, 1f

three successive blank analyses Indicate levels of Methylene chloride or Acetonethat are consistently above that, but below five times the detection limit, thelaboratory 1s allowed to proceed. In this case, the analyst must qualify the

data with a Quality Assurance Notice.

For the remaining volatile, semlvolatlle and pesticide target analytes, the

concentration 1n a method or Instrument blank may not exceed one-half thedetection limit.

Precision and Accuracy Objectives for Organic Analyses: Organic surrogaterecoveries are used to determine whether the sample processing and analysisfunctions are 1n control. With a few exceptions, surrogate recoveries must bewithin control limits or the sample processing and analysis must be repeated.One exception Involves the pesticide surrogate, Dlbutylchlorendate (DBC), which

FAC 001 0718


1s used for advisory purposes only (as directed 1n the SOW for the ContractLaboratory Program), although recovery must be greater than 10X. The otherexception Involves the surrogates for add and base/neutral extractables: forCLP analyses, no more than one surrogate from each fraction (add or

base/neutral) may be outside control limits, and all recoveries must be greaterthan 101. All surrogate recoveries 1n volatile, add and base/neutral methodblanks must be within control limits.

Matrix spike control limits for organlcs samples associated with the EPA-CLP arealso "for advisory purposes." Samples processed following procedures designated1n 40 CFR Part 136 and those associated with SW-846 must meet acceptancecriteria specified therein. The CLP methodologies require the calculation anddocumentation of Relative Percent Differences (RPDs) between recoveries of thematrix spike (MS) and matrix spike duplicates (MSD), although acceptancecriteria are also "advisory." CompuChem* has adopted Internal accuracy andprecision criteria to be used as decision guidelines where the contract provides"advisory" criteria.

For SW-846 and CLP MS/MSD tests, at least one-half of the QC spiking compounds

must be recovered within acceptance criteria for each organic fraction.Similarly, at least one-half of the precision criteria (RPDs) must be met peranalytical fraction. If these criteria are not met, the matrix spike and matrixspike duplicate tests have to be repeated. For Federal Register requirements, amatrix spike, fortified with the full complement of target analytes, 1sperformed for organic analyses. A blank spike (or "Laboratory Control Sample")1s also processed with the batch. If all compounds 1n the matrix spike are not

FAC 001 0719


are not recovered within acceptance criteria, the blank spike 1s analyzed.If neither QC sample meets criteria, the entire batch 1s reprocessed. Asdescribed 1n this section, precision and acuracy acceptance limits for CLP(Contract Laboratory Program) organic and Inorganic analyses are

contract-mandated. Those same criteria have been Incorporated Into the thirdedition of SW-846 methods. CompuChem* also offers a variety of analytical

services using Federal Register methodologies, and of course, the QC

requirements for accuracy and precision are method-mandated. In 40 CFR Part

136, 1t 1s recommended that the laboratory periodically update these control

limits based on historical data. Updated control limits will be based on thefollowing formulae:

LCL « X - 3S

UCL « Y + 3S, where:

LCL » Lower Control Limit

UCL • Upper Control Limit

X « Mean Percent RecoverySO • Standard Deviation

Inorganic Program QC RequirementsThe Inorganic Program QC Requirements are similar to those outlined above forthe Organic Program. Metals, except Mercury, are analyzed using flame andfurnace Atomic Absorption (AA Spectroscopy and/or Inductively-Coupled ArgonPlasma (ICP or ICAP) Spectroscopy. The analysis procedure generally Involvestwo steps: sample digestion and subsequent Instrumental analysis.


The quality of these results 1s assured by several key procedures. Although

surrogate standards are not applicable to Inorganic analyses, the laboratory

uses Sample Spikes and Duplicates 1n much the same way as the Organic Program toassess data accuracy and precision. Additionally, a Laboratory Control Sample

(also referred to as a Blank Spike) and a Method Blank are produced with eachbatch of samples. These Quality Control samples are Involved 1n both the sample

digestion and analytical processes, and represent the conditions under which

associated samples were processed.

Calibration standards are obtained from the USEPA and other, Independent,certified sources. Inorganic standards are prepared by the Inorganic Laboratory

analysts, and the preparation 1s documented 1n the laboratory's StandardPreparation logbook. The standard container 1s labeled with the preparer'sInitials, date of preparation, and type of standard.

Instruments are calibrated following the requirements set forth 1n the CLP

Inorganic Statement-of-Uork, SU-846 (3rd Ed.) or other EPA-approved methods, asdescribed below. In-lab Data Reviewers and Final Technical Reviewers useguidelines documented 1n their respective SOPs for verifying compliance of

calibration data with QC requirements.

AA and ICP Instrument Calibrations: For Inorganic analysis by AAS and ICP,Initial calibration 1s performed using dilutions of stock metal solutions. ForAAS calibration, a blank and at least three calibration standards are employed.For ICP analysis a mldconcentratlon level standard 1s analyzed. On a quarterlybasis, a linear range verification check standard 1s analyzed for each element.The analytically determined concentration of the standard must be within 51 of

001 0721

iC. * ••!•• l«« . 3 . J


! the true value. This concentration, then, 1s the upper limit of the ICP linear

range. Results cannot be reported beyond that upper concentration level unless1 they are a result of an appropriate dHutlon/reanalysls.

After the AAS and ICP systems have been calibrated for every analyte, the

Initial calibration 1s required to be verified for accuracy. This 1saccomplished by Immediately analyzing an EPA Initial Calibration Verification

solution or any other Independent standard at a concentration other than that

used for calibration, but within the calibration range. An Independent standard

1s one prepared from a different source than those used 1n the Initialcalibration.

In order to assure calibration accuracy during the course of sample analyses, a

Continuing Calibration Verification Standard 1s analyzed at a frequency of 10»,

or every 2 hours during the analysis run, for each analyte. The analyteconcentrations 1n the Continuing Calibration Verification Standard are near themid-range level of the calibration curve. The Initial and ContinuingCalibration Verification Control Limits are:

INITIAL AND CONTINUING CALIBRATION VERIFICATIONCONTROL LIMITS FOR INORGANIC ANALYSES

Analytical Method

ICP Spectroscopy/Flame AASFurnace AASCold Vapor AASOther

Inorganic Species

Metals

MetalsMercuryCyanide

* of True ValueLower Limit

90

90so'85

(EPA Set)Upper Limit

110

no120115

FAC 001 0722


At the beginning and end of each ICP analysis shift, an ICP Interference Check

Sample also 1s analyzed. This analysis Interelement and background correctionfactors since 1t assesses analytes of Interest 1n the presence of highconcentration levels of other elements.

Additionally, for each batch of samples processed, an ICP Serial DilutionAnalysis Is performed. If an analyte 1s present at a sufficient concentration

(minimally a factor of 10 above the Instrumental detection limit), an analysis

of a 1:4 dilution must agree with 101 of the original determination. If not

within that Hmk, a chemical or physical Interference effect 1s likely, and the

associated data are qualified.

All QC sample results are tabulated Immediately following analysis and compared

to the contract-mandated, method-mandated, or client-mandated control limits forprecision and accuracy. Out-of-contrcl results are cause for Immediate

re-extraction and/or re-analysis. No outlying data are ever released until thelaboratory has verified that unacceptable results are attributable to the sample

matrix.

Additionally, on a quarterly basis, Instrument detection limits are determined

for each ICP and AAS system used for Inorganic analyses. This 1s accomplishedby multiplying by three (3), the average of the standard deviations obtained onthree (3) nonconsecutlve days from the analysis of a standard of each analyte 1nreagent water. The concentration of each analyte 1n the standard solution 1s atapproximately 3-5 times the estimated Instrument detection limit and seven (7)consecutive measurements, per day, per analyte are required.

FAC 001 0723


Also on a quarterly basis, Interelement and background correction factors are

determined for ICP analysis using an Interference Check Sample. This measure

determines the potential false analyte signals caused by the presence of highlevels of certain commonly occurring elements found 1n environmental samples.


COMMERCIAL ORGANIC AND ERA - CLP CONTRACT REQUIRED SURROGATE SPIKE CONTROL LIMITS'

Volatile Surrogates Solid L1ou1dD4-l,2-D1chloroethane 70-121 76-114

4-Bromofluorobenzene 74-121 86-115D8-Toluene 81-117 88-110

Base/Neutral Surrogates Solid Hguld

05-NUrobenzene 23-120 35-114

DIO-Pyrene 17-125 ** 40-130 **D14-Terphenyl 18-137 33-141

2-Fluoroblphenyl 30-115 43-116

Add Surrogates Solid Liquid

2-Fluorophenol 25-121 21-100

2,4,6-Trlbromophenol 19-122 10-123

05-Phenol 24-113 10-94

Pesticide Surrogate Solid L1gu1dDlbutylchlorendate (DBC) 20-150 *** 24-154 ***

Herbicide Surrogate Solid

2,4-DB 16-124

* as noted 1n the EPA-CLP SOU, dated 10/86 and 2/88 and subject tomodification based on data supplied In the CLP

** laboratory optional surrogate only; no action limits at this timeadvisory surrogate; minimum 10% recovery used as action limit

FAC 001 0725


EPA-CLP MATRIX SPIKE RECOVERY LIMITS*Fraction Matrix Spike Compound Water* Soil/Sediment*

VOAVOAVOAVOAVOA

BNBNBNBNBNBN

AddAddAddAddAdd

Pest.Pest.Pest.Pest.Pest.Pest.

*These limits a10/86 and 2/88

1,1-D1chloroetheneTrlchloroetheneChlorobenzeneTolueneBenzene

1,2,4-TrlchlorobenzeneAcenaphthene2,4-D1n1trotoluenePyreneN-N1troso-D1-n-Propylam1nel,4-D1chlorobenzene

PentachlorophenolPhenol2-Chlorophenol4-Chloro-3-Methylpheno14-N1tropheno1

LlndaneHeptachlorAldrlnDleldMnEndrln4, 4 '-DOT

re for advisory purposes only. They are not to be used to

61-14571-12075-13076-12576-127

39-9846-11824-9626-12741-11636-97

9-10312-8927-12323-9710-80

56-12340-13140-12052-12656-12138-127

(as noteddetermine

59-17262-13760-13359-13966-142

38-10731-13728-8935-14241-12628-104

17-10926-9025-10226-10311-114

46-12735-13034-13231-13442-13923-134

In the EPA-CLP SOW, dated1f a sample should be* • . • • * • » . . •«*reanalyzed. When sufficient multi-lab data are available, standard limits will

be calculated.

001 0726


EPA-CLP MATRIX SPIKE DUPLICATE RELATIVE PERCENT DIFFERENCE(RPD) LIMITS*

Fraction Matrix Spike Compound Water* Soil/Sediment*

VOAVOAVOAVOAVOA

BNBNBNBNBNBN

AddAddAddAddAddPest.Pest.Pest.Pest.Pest.Pest.

l,l-D1chloroetheneTrlchloroetheneChlorobenzeneTolueneBenzene1,2,4-TrlchlorobenzeneAcenaphthene2,4-D1n1trotoluenePyreneN-N1troso-D1-n-Propylam1nel,4-D1chlorobenzene

PentachlorophenolPhenol2-Chlorophenol4-Chloro-3-Methylphenol4-N1trophenolUndoneHeptachlorAldrlnD1eldr1nEndrln4, 4 '-DOT

*These limits are for advisory purposes only10/86 and 2/88. They are not to be used to

1414131311

283138313828

5042404250

15?022182127

(as noteddetermine

2224212121

231947363827

4735503350

503143384550

1n the EPA-CLP SOU, dated1f a sample should be

reanalyzed. When sufficient multi-lab data are available, standard limits willbe calculated.

001 0-721


SOLID QC ACCEPTANCE CRITERIA-COWERCIAL ORGANICS*

Parameter Percent Recovery RPDI,l-D1ch1oroethane 59 • 172 22TMchloroethene 62 - 137 24Chlorobenzene 60 • 133 21Toluene 59 - 139 21Benzene 66 - 142 21

1,2,4-Trlchlorobenzene 38 - 107 23Acenaphthene 31 - 137 192,4-D1n1trotoluene 28 - 89 47Pyrene 35 - 142 36N-N1troso-D1-n-Propy1am1ne 41 - 126 38l,4-D1chlorobenzene 28 - 104 27

Pentachlorophenol 17 - 109 47Phenol 26-90 352-Chlorophenol 25 - 102 504-Ch1oro-3-Methylphenol 26 - 103 334-N1tropheno1 11 - 114 50

Mndane 46 - 127 50Heptachlor 35 - 130 31Aldrln 34 - 132 43D1eldr1n 31 - 134 38Endrln 42 - 139 454,4'-DOT 23 - 134 50

2,4-D 56 - 1602,4,5-TP 61 - 1132.4,5-T 63 - 109

Mandatory limits based on acceptance criteria noted 1n the EPA-CLP SOU, dated10/86 and 2/88 except herbicides—based on historical performance records.

FAC 001 0728


WATER AND UASTEVATER QC ACCEPTANCE CRITERIA-METHOD 625 BASE/NEUTRAL EXTRACTABLES

Federal Register (October 26. 1984. 40 CFR Part 136)

ParameterAcenaphtheneAcenaphthyleneAnthraceneBenzo(a)anthraceneBenzo(b)fluorantheneBenzo{k)fluorantheneBenzo(a)pyreneBenzo(gh1)peryleneBenzyl butyl phthalateB1s(2-Choroethyl)etherB1s(2-chloroethoxy)methaneB1s(2-chloro1sopropy1)etherB1s(2-ethylhexyl)phthalate4-Bromophenyl phenyl ether2-Chloronaphthalene4-Chlorophenyl phenyl etherChryseneD1benzo(a,h)anthraceneD1-n-butyl phthalate1.2-D1ch1orobenzene1.3-D1ch1orobenzene1.4-D1chlorobenzene3,3'-D1chlorobenz1d1neDlethyl phthalateDimethyl phthalate2,4-D1n1trotoluene2,6-D1n1troto1ueneD1-n-octylphthalateFluorantheneFluoreneHexachlorobenzeneHexachlorobutadleneHexachloroethaneIndeno(1,2,3-cd)pyreneIsophoroneNaphthaleneNitrobenzeneN-N1trosod1-n-propylam1nePhenanthrenePyrene1,2,4-Tr1chlorobenzene

Percent Recovery47 - 14533 - 14527 - 13333 - 14324 - 15911 - 16217 - 163D - 2190 - 15212 - 15833 - 18436 - 1668 - 15853 - 12760 - 11825 - 15817 - 168D - 2271 - 118

32 - 129D - 17220 - 1240DD395042659D2440D212135D54

262114112139158146137121152116113171196133180230120

52 • 11544 - 142

001 0729


WATER AND WASTEWATER PC ACCEPTANCE CRITERIA—METHOD 625 ACID EXTRACTABLESFederal Register (October 26. 1984. 40 CFR Part 136)

4-Chloro-3-methylphenol2-Chlorophenol2,4-D1chlorophenol2,4-D1methylphenol2,4-D1n1trophenol2-Methyl-4,6-d1n1trophenol2-NUrophenol4-N1trophenolPentachlorophenolPhenol2,4,6-THchlorophenol

22 •23 •39 •320D29D14537

• 147• 134- 135119191181182132176112144

PAC 001 0730

Seccion No. 9.3Revision No. 3Date: October 3, 1988Page 7 of 9

MATER AND WASTEWATER QC ACCEPTANCE CRITERIA-METHOD 624 Volatlles

Federal Reg1ster(October 26. 1984. 40 CFR Part 136)

Parameter

BenzeneBromod1ch1oromethaneBromoformBromomethaneCarbon TetrachlorldeChlorobenzeneChloroethane2-Chloroethylv1nyl etherChloroformChloromethaneDlbromochloromethane1.1-D1chloroethane1.2-D1chloroethane1.1-D1ch1orothene(Total) l,2-D1ch1oroethene1.2-D1chloropropaneds-l,3-D1ch loropropenetrans-l,3-D1chloropropeneEthyl benzeneMethylene chloride1,1,2,2-TetrachloroethaneTetrachloroetheneToluene1.1.1-Trlchloroethane1.1.2-Tr1chloroethaneTrlchloroetheneVinyl chlorideAcrolelnAcrylon1tr1le

Percent Recovery

37 - 15135 - 15545 - 169D - 24270 - 14037 - 16014 - 230D - 30551 - 138D - 27353 • 14959 - 15549 - 155D - 23454 - 156D - 210D - 22717 - 18337 - 162D - 22146 - 15764 - 14847 - 16252 - 16252 - 15071 - 157

D - 251D - 150D - 150

FAC 001 0731


WATER AND WASTEUATER QC ACCEPTANCE CRITERIA—METHOD 608 PESTICIDES

Federal Register (October 26. 1984. 40 CFR Part 136)

ParameterAldrlnalpha-BHCbeta-BHCdelta-BHCgairroa-BHC (Llndane)Chlordane4,4'-ODD4,4'-DDE4,4'-DDTD1e1dr1nEndosulfan IEndosulfan IIEndosulfan SulfateEndrlnHeptachlorHeptachlor epoxldeToxaphenePCB-1016PCB-1221PCB-1232PCB-1242PCB-1248PCB-1254PCB-1260

Percent Recovery42 • 12237 - 13417 - 14719 - 14032 - 12745 - 11931 - 14130 - 14525 - 16036 - 14645 - 153D - 20226 - 14430 - 14734 - 11137 - 14241 - 12650 - 11415 - 17810 - 21539 - 15038 - 15829 - 1318 - 127

WATER AND WASTEWATER QC ACCEPTANCE CRITERIA-HERBICIDES*

2,4-D2,4,5-TP2,4,5-T

38 - 15235 - 14238 • 141

Âdvisory use only; minimum 10% recovery used for action limits,on historical performance records for the method.

Criteria based

PAC 001 0732


PRECISION AND ACCURACY OBJECTIVES*SU-846 ( 3rd. Ed. ) Methods

Method

8010**

8020

8140

8150

8280

Class of Compounds

Halogenated VolatileOrganics--Gc

Aromatic VolatileOrganlcs— GC

OrganophosphorusPest1c1des--GC

Chlorinated Herbicides—GC

D1benzo-P-D1ox1ns and

PrecisionAqueous

20

20

30

30

50

(RPD)Solid

30

30

50

50

60

Accuracy (t_R_)Aqueous60-150

60-150

30-140

30-140

40-150

Solid

50-170

50-170

20-150

20-150

30-160Dlbenzofurans—GC/MS

*cr1ter1a to be updated based on periodic reevaluatlon of lab performance statisticsfrom real-world samples analyzed as spikes and duplicates; See text for additionalexplanation.

**those compounds amenable to purge and trap analysis only.

FAC 001 0733


EPA-CLP SAMPIKE SPIKE ACCURACY AND DUPLICATE PRECISION « INORGANICS

Element Percent Recovery* Relative Percent Difference **All CLP Metals 75 - 125* +/- 20

* - If Spike recovery 1s not within 75 - 125*. the data of all samplesassociated with the spiked sample and determined by the same analyticalmethod must be flagged with an "N" on Forms I and V. If the sampleconcentration exceeds the spike concentration by a factor of four or morethe data 1s reported unflagged, even 1f the spike recovery 1s outside the75-125* range.

** - The +/- 20* RPD 1s used when the sample results are greater than five timesthe Contract Required Detection Limit (CRDL). A control limit of +/- theCRDL 1s used for samples less than the CRDL. If either sample 1s below theCRDL then the RPD 1s not calculated.


10.0 Corrective Action

10.1 Introduction

Generally, there are two types of corrective actions that may be required when

data quality falls below specified limits. The first type, and the simplest toImplement and document, 1s corrective action required because routine data

quality assessments are out-of-control. Surrogate and spike standard

recoveries, relative percent differences between duplicates, Internal standard

response variations, and unacceptable blank contamination are some of these

assessments 1n the first category. These are all performed on a sample-by-sample and/or batch basis, and corrective action 1s limited to evaluating thedata with respect to SOP criteria, and accepting or rejecting the sample/batch.

The decision that 1s made 1s clearly Indicated on analytical worksheets, and

unless a trend 1s observed during the course of data validation, additional

corrective action or documentation 1s not necessary.

The second type of corrective action 1s that required when other, more global

QC/QA assessments, are made. The assessments might typically Indicatesystematic defldences or those affecting data useabllUy for more than onebatch (I.e., glassware contamination checks, standards preparation errors, etc.).In most cases, assessments of this nature are made by reviewing peripheral QC/QAdocumentation, observing procedures for comparison with SOPs or GLPs, or

receiving feedback from data reviewers, management or those external to the

organization (clients, auditors).

The following sections describe the QA reporting and feedback channels designedto ensure that early and effective corrective action 1s taken 1n such Instances.

001 0735


In many cases, depending on the nature of the deficiency and the urgency for

remedial action, a Corrective Action Report (following this section) will be

completed. The report serves to document the deficiency, the required

corrective action, and accountability for the action.

For observations made over longer periods of time, the QA Department Issues

formal summary reports to management on a monthly or quarterly basis. Following

1s a brief discussion of the types of reports Issued to management to assess the

overall effectiveness of the QA Program and to reinforce the application of Good

Laboratory Practices (GLPs).

CORRECTIVE ftCTIQN REPORT

DATE:________

PROBLEM / DEFICIENCY!

IDENTIFIED BY:

REFERRED TOs ______________________________ < Q A >

CORRECTIUE ACTION Jfl g£ TAKEN: TARGET DATE:.

FQLLOU-UP AUDIT FINDINGS;

RESOLVED? _____ DATE*

SOP REQUIRED TO BE WRITTEN/MODIFIED? YES t 1 NO [ 3 TARGET DATE:.

This form to be filed with the Quality Assurance Clerk for permanent record.

FAC 001 0737

Section }(j.tRevision No. 4Date: October 3, 1988Page 1 of 1

10.2 Routine QC Check Reports

The following routine quality control checks (also discussed In section 9.2 ofthe QA Plan) are performed to verify that samples are not contaminated duringtransportation, preparation, analysis or storage, and that standards prepared

Internally are traceable to certified sources.

~ Vendor-Supplied Glassware Checks

— Glassware Decontamination Checks— Water Purification Systems Checks— Glassware Storage Cabinet Checks

—- Refrigerated Storage Systems Checks

— Reagent Purity Checks

—- Standards Prepartlon and TraceablHty Checks

The criteria for these QC checks and corrective action steps are detailed 1n the

QA SOP Manual. Results are tabulated and/or plotted on control charts, andrecords reviewed by the QA staff. A series of quarterly reports to management

summarize this Information and the status of these programs.

FAC 001 0738


10.3 Monthly QA Activity Reports

These reports are produced by all members of the QA staff, and summarize key QAactivities during the previous month. The reports are distributed to the

Director of QA, and are provided as an attachment and referenced 1n the

Director's report to the CEO, the Executive Staff and senior laboratorymanagement.

Included 1n these reports 1s a summary of significant quality problems observed

during the period, and the corrective actions taken to remove deficiencies. The

report stresses proactive measures that are being taken to Improve quality or

ensure compliance with QA program requirements.

Laboratory management uses the report to quantitatively measure monthlyperformance 1n terms of the number of samples processed, the frequency of

repeated sample analyses due to unacceptable QC performance, and the cause of

the unacceptable performance. These data are all presented 1n tables, Paretocontrol charts or attribute control charts, based on the characterization ofeach analysis 1n the Computerized Laboratory Management System (CLMS) using a

system of analytical "condition codes."

The Condition Code System 1s used to monitor sources of data failures.Condition code definitions are provided 1n an SOP to data generators andreviewers who are responsible for assigning the appropriate code to eachanalysis (see Appendix D). Each two-letter code 1s used to characterize thecause of a sample failure or the final status of the data package prior torelease to the client.

FAC 001 0739


Various computer programs may be used to sort condition code data according tosample matrix and method. This system 1s used to pinpoint sources of error,

provide feedback to management, reinforce good laboratory practices, and

document laboratory performance over time. The QA staff also note 1n the

Monthly QA Activities Report any corrective actions taken or necessaryprocedural changes, based on the application of condition codes.

Other Items Included 1n this report are:

— Summary of any changes 1n certification/accreditationstatus

— Involvements 1n resolution of quality Issues with clientsor agencies

— QA organizational changes

— Notice of the distribution of revised documents controlledby the QA Department (I.e., SOPs, QA Plan)

— Training and safety Issues, 1f not already covered 1naudit reports during the period

—- Performance of subcontractor laboratories (alsocommunicated 1n separate, detailed subcontractor auditreport to management)

— Positive feedback for acceptable performance onIntel-laboratory or Intralaboratory tests or successfulcompletion of audits.

FAC 001 0740


10.4 Laboratory Performance Reports

This quarterly report presents a statistical and graphical summary of the

laboratory's performance on batch-associated quality control samples analyzedover the period. Included are tables, Shewhart control charts and I-charts (forIndividual data points) for all surrogate and spike standard recoveries.

Additionally, a monthly report to the Director of QA presents control charts and

tables for all Laboratory Control Sample (Blank Spike) and Blank recoveries.

The charts and tables are used primarily to document historical performance,

update recovery control limits, and monitor long-range trends that might not be

apparent to data reviewers evaluating data on a sample/batch basis.

FAC 001 0741

Secnor, no. iu.sRevision No. 4Date: October 3, 1988Page 1 of 7

10.5 Laboratory Audit Reports

Quarterly audit reports are written by a member of the QA staff and distributed

to management, and summarize the results of Internal laboratory Performance

Audits, Systems Audits and Security/Access Audits. When external auditors are

Involved 1n Performance or System Audits, a report 1s written within the nextweek by the QA staff member coordinating the audit. The report, summarizing

audit results as discussed 1n the debriefing as well as other observations, 1s

distributed to the CEO and senior lab management. The report Includes

corrective actions required as a result of the audit, and a schedule forImplementation. A follow-up audit, usually within three weeks of the

distribution of this report, 1s conducted to verify that corrective actions have

been Implemented.

Performance Audits

Performance Audits are checks made by a QA staff member or other Independentauditors to evaluate the quality of the data produced by the analytical system.These audits are performed Independent of an 1n addition to routine quality

control checks, and reflect as closely as possible lab performance under normaloperating conditions.

These audits Involve the review of approximately 10% of all analytical datareports generated by the lab for calculation and data validation procedures, andoverall data quality. Errors observed during the audit are characterized as

"critical" or "correctable" and tabulated. If necessary, based on auditfindings, an amended data report may be sent to the customer. Following thissection 1s a copy of the QA Audit Summary used by auditors to tabulate the data

FAC 001 0742


for summary Into the Quarterly Performance Audit report. A thorough discussion

of these audits Is Included 1n the QA SOPs. The reports are used by laboratorymanagers to provide feedback to staff members and establish goals for Improved

performance.

A number 1n Inter laboratory and Intralaboratory tests are conducted routinely at

CompuChem*, and the results are Included 1n Individual Performance Audit reports

specific to each test. When new methods are available to the laboratory or newpersonnel are being trained, Laboratory Proficiency Tests are performed. These

tests consist of quadruplicate blank spikes, containing a full complement of

tests parameters to be analyzed by the method. The replicate results areanalyzed by a QA staff member, who generates a summary report to the Director

of QA. This report Includes the standard deviation and mean recovery for each

of the replicate parameters, and the data are used to statistically validate

method and/or personnel proficiency. For a thorough discussion of the method

validation procedures used, refer to Appendix A of the QA Plan.

On a quarterly basis, blind Intralaboratory check samples are Introduced Intothe system by the QA Department. Parameters and methods are chosen for thesestudies based upon Independent Hnterlaboratory) tests from certifying agencies

(Including the U.S. EPA and various state agencies), Laboratory Proficiency

Test results, Method Validation studies, or results from routine batch-relatedQC samples. The existence of these check samples 1n the system 1s known only tothose personnel Involved 1n preparing the samples and scheduling the analytical

requirements Into the CLMS. A thorough report, detailing the entire datageneration and support functions, 1s completed by the QA staff and reviewed by

FAC 001 0743


the Director of QA before distribution to the CEO and senior laboratory

management.

CompuChem* also participates 1n a number of external, Interlaboratory

performance studies. These are required as part of various agencies'

certification/accreditation programs. As a member of the USEPA's ContractLaboratory Program (CLP), the laboratory Is required to successfully analyze

quarterly, blind proficiency samples for both organic and Inorganic parameters.

The CLP program also requires an annual on-s1te Inspection by principals from

the USEPA (and their contracted agents). These audits generally follow thesame format described below, Systems Audits.

CompuChem* also participates In a number of state certification programs,

Including those for North Carolina, New Jersey, New York and Florida. All of

these programs require the laboratory to submit to annual on-s1te Inspections 1n

order to maintain certification to perform testing on samples originating 1n the

state. All states also require successful performance on Interlaboratory check

samples, submitted at least annually, though some reciprocity with the two NCprograms (one for drinking water and one for wastewater certification) and

USEPA-CLP 1s allowed under certain circumstances.

Several states utilize the laboratory's performance on the annual Water Supply

(WS) and Water Pollution (WP) proficiency testing series, orglnatlng out of theEPA Environmental Monitoring and Support Laboratory's performance on all

Interlaboratory and Intralaboratory check samples, tabulated by parameter andmethod, so negative performance trends can be readily pinpointed.

0744


System Audits

A System Audit 1s an on-s1te Inspection and review of the QA Program for the

total laboratory. While Performance Audits are a quantitative appraisal, System

Audits are for the most part qualitative 1n nature. The System Audit may be

either scheduled or unannounced before 1t 1s conducted, but occurs routinely onat least a quarterly basis. The auditor reviews the laboratories' SOPs to

verify compliance with procedures and activities actually 1n place. Personnel

and facilities are also evaluated during the System Audit. The auditor Is

required to Investigate anything which seems 1n conflict with the QA Plan, the

laboratory or QA SOPs, or Good Laboratory Practices.

If deficiencies are observed during a Performance Audit, and 1f deemed

necessary, the QA Department Initiates a System Audit. The audit emphasizes the

actions necessary to correct deficiencies noted 1n the Performance Audit. ACorrective Action Report 1s completed, detailing all remedial actions taken, andreviewed by the Director of QA. The report must Indicate the proposedImplementation date and the Individual(s) responsible for the action.

Many of the objectives of a routine System Audit are similar to those a clientor Independent auditor would hope to accomplish during an On-S1te Laboratory

Evaluation and Data Audit. These goals Include ensuring the following:

1. The quality control, Including necessary corrective actions , are beingapplied

2. Adequate facilities and equipment are available to perform the client'srequired scope-of-work

3. The personnel are qualified to perform the assigned tasks4. Complete documentation 1s available, Including sample cha1n-of-custody

FAC 001 0745


5. Proper analytical methodology 1s being applied6. Acceptable data handling techniques are being used

7. Corrective actions Identified 1n any previous on-s1te visits have beenImplemented, and

8. The Laboratory Management continues to demonstrate a commitment toquality.

These objectives may be documented by completing an EPA-approved Laboratory

Evaluation Checklist. In response to System Audits, any corrective actions

taken are noted with reference to the auditor's deficiency report and the lab's

Standard Operating Procedures.

FAC 001 0746

QUALITY ASSURANCE AUDIT SUMMARY

iii4

t

•

f

•

•

lO

11

II

13

14

tt

!•

17

IB

It

M

21

73

n

14

75

7*

77

n

SAMPLE NUMBER

•

EBACIIQI

»

1

'- -' LWI i «._ »»•»» - . • . « » . , „

(EJECT LOCATIOK /CAUSEi

COMMENTS

•

corr?5

allure

« • • • * . i

CT?*allure status

•

n*T*<

r-o

oo

CJ

i—._.;.

Hissing/Incorrect:

CAM/I Calculations missing/IncorrectCCM/I Condition code missing/IncorrectDFM/I Data footnote missing/IncorrectCFM/I Correction factor missing/IncorrectDWI Dry weight/percent moisture IncorrectFNI Filename IncorrectFFM/I Form 4 missing/IncorrectLSM/1 Library search missing/IncorrectQNM/I QA Notice missing/IncorrectRRM/I Reportable run missing/IncorrectSPM/I Spectrum missing/IncorrectSRM/I Sample receiving Information missing/IncorrectSSM/I Surrogate Summary Form missing/IncorrectSTM/I Standard package missing/IncorrectTFM/1 Tuning Form missing/IncorrectUNM/I Units missing/IncorrectWSM/I Worksheet m1ss1ng/1ncorrect/1ncompleteOAM/I OADS m1ss1ng/1ncorrect/1ncomplete

Qualitative/Quantitative Errors:

HNR Hit not reported, but should have beenHRE Hit reported 1n error, should not have been reportedHAI Hit amount reported IncorrectlyCFN Correction factor not applied to hitSFI Significant figures (or roundlng off) IncorrectTRE Transcription error

Miscellaneous Errors:

ISF Internal standard area monitor Indicates failureODI OWA date or time IncorrectRNL RIC not labeledSOL Surrogate(s) actually outside limitsUOU Uhlteout used on documents (dellverables)NSO Not signed offCNI Change not Initialed

Condition Code Applications:CS Carryover suspectedCT Contamination evidentRU Repeated unnecessarilySF Spikes failedUN Unacceptable, not needed

ooi 0-748


11.0 Implementation Requirements and Schedule

The Implementation of this QA Plan 1s complete following the signed approval of

the Director of QA and CompuChem* Corporation's CEO, and distribution of the

document to laboratory management and staff.

FAC 001 0749


12.0 References

1. Interim Guidelines and Specifications for Preparing Quality AssuranceProject Plans. December 29, 1980, Office of Monitoring Systems and QualityAssurance, ORD, U.S. EPA, QAMS-005/80, Washington, DC 20460.

2. Guidelines and Specifications for Preparing Quality Assurance Program Plans.September 20, l950~, Office of Monitoring Systems and Quality Assurance, ORD,U.S. EPA, QAMS-004/80, Washington, DC 20460.

3. Preparation of State Lead Remedial Investigation Quality Assurance ProjectPlans for Region V. April 4, 1984, Office of Monitoring Systems and QualityAssurance, U.S. EPA, Washington, DC 20460.

4. Chemistry Quality Assurance Handbook. July 2, 1987, U.S. Department ofAgriculture Food Safety and Inspection Service, Volume I.5. WMtehead, R. J., "Statistical Quality Control for the AnalyticalLaboratory," Proceedings from the Analytical Techniques and ResidualsManagement jjn Water Pollution Controlspecialty Conference. Water PollutionControl Federation, April 20, 1988.

6. Guidance for USAFOEHL Laboratory Quality Assurance/Quality Control (QA/QCAudits (DRAFTTTJune 1988.

7. Manual for the Certification of Laboratories Analyzing Drinking Water(Criteria and Proce3uT-es--Qual1tyTs'Turance). October. 1982. Office of DrinkingWater, U.S. EPA, EPA-570/9-82-002, Washington, DC 20460.8. Gautler, M. A. and Gladney, E. S., "A Quality Assurance Program for Healthand Environmental Chemistry," American Laboratory. July 1987. pp. 17-22.

9. Quality Assurance Handbook for A1r Pollution Measurement Systems. Vol. 1:Principles. EPA-600/9-76-005. March 1976.10. Quality Assurance; A Laboratory Practice Manual. The American Council ofIndependent LaboratorlesT May 1986.11. "Principles of Environmental Analysis,' American Chemical Society.Analytical Chemistry. Vol. 55, No. 14. December 1983. pp. 2210-2218.

"•?. Dux, J. P., "Quality Assurance 1n the Analytical Laboratory," AmericanLaboratory. July 1983. pp. 54-63.

FAC 001 0750

Secfton: Appendix ARevision No. 2 C 300928Date: October 17, 1988Page H of 8

JPPEKDIX A

METHOD VALIDATION STUDIES

FAC 001 0751

beet tor,. AppeMu IA MRevision No. 2Date: October 17, 1988Page 2 of 8

General Approach for the Validation ofAnalytical Methods by the Laboratory

Introduction

Historically our laboratory has determined the viability of published proceduresby performing lab proficiency tests; I.e.-full analyte spikes are added toquadruplicate allquots of laboratory pure water or "blank" soil, the samples areprepared/extracted and then analyzed by the appropriate Instrumentation. TheInstrumentation would Include GC/MS, GC, with appropriate detectors, and 1n theInorganic area, ICP/AAS/cold vapor AAS.

The laboratory proficiency testing program has been beneficial 1n demonstratingto ourselves and to Interested clients that our applications of specifiedanalytical methodologies are capable of producing acceptable data. Theacceptable data 1s further characterized with statements of accuracy andprecision; mean percent recoveries and standard deviations, respectively.A necessary complement to the laboratory proficiency tests would be a formalizedmethod detection limit study.Before describing the rudiments of a recommended "Generic Method ValidationStudy," certain definitions of terms are required. John K. Taylor (1) of NBSpresents the following definitions of the hierarchy of methodology; from thegeneral to the specific:(1) A Technique 1s a scientific principle, usefjl for providing compositional

Information.(2) A Method 1s a distinct adaptation of a technique for a selected measurement

purpose.(3) A Procedure 1s composed of the written directions necessary to utilize a

method.(4) A Protocol 1s the most specific name for a method and contains a set of

definitive directions that must be followed, without exception, 1n orderthat the results be accepted for a given purpose.

Additionally, 1n an article entitled "Principles of Environmental Analysis" (2),a distinction 1s made between verification and validation:

(1) Verification 1s a general process used to decide the capability of a methodfor producing accurate and reliable results.

(2) Validation 1s an experimental process which Involves external corroboratlonby other laboratories (Internal or external) or methods or the use ofreference materials 1n order to evaluate the suitability of methodology.

PAC 001 0752

Section: Appendix ARevision No. 2 1300QT/Date: October 17, 1988 v^*JlPage 3 of 8

Our laboratory 1s embarking on a second generation of testing requirements whichwill serve to formally "validate" the "methods" we employ for new productofferings. The "Generic Method Validation Study" will serve to supply the dataneeded to satisfy ourselves and our clients that the laboratory's approach 1ssound. The Impetus will be on the Individual laboratories to prepare thespecific experimental design, based on the method being validated.Additionally, the Individuals actually performing the sample preparation,Instrument calibration, analysis and data reduction processes will be requiredto utilize laboratory notebooks. The purpose of the laboratory notebooks 1sfourfold:

(1) To record observations concerning problems encountered 1n applying theexperimental design as written,

(2) To note recommendations which may serve to eliminate the problemsexperienced,

(3) To serve, with the experimental design, as a basis for the StandardOperating Procedures (SOPs) which will subsequently be required, and

(4) To provide a basis for the preparation of an "Equivalency" petition to besubmitted to the EPA.

(Note: as Indicated above under the definitions of the hierarchy ofmethodology, a Procedure should not be able to be wr1tt«n until a Method hasbeen utilized; I.e. - until the laboratory testing of the Method 1s accomplishedand the details of the tests; problems/observat1ons/recom,iendat1ons, as written1n laboratory notebooks, are evaluated).In validating a method, the kinds of samples (matrices) to be processed shouldbe clearly described. As a result of the validation process, statements ofprecision and accuracy will be generated. It should be realized that these dataserve only as an estimate of the typical performance expected.In being able to judge the suitability of a method, other factors have to beconsidered: sensitivity to Interferences, limits of detection and useful rangeof measurement (1).Interferences may come from two sources: those that are Inherent In the matrixand laboratory artifacts, Introduced during the sample processing.By running appropriate method blanks and/or unsplked controls, the Interferencescan be characterized.The concepts of detection limits and quantltatlon limits require elucidation(2).

The Limit of Detection (LOO) 1s defined as the lowest concentration levelthat can be determined to be statistically different from a blank.

PAC 001 0753

Section: Appendix ARevision No. 2Date: October 17, 1988Page 4 of 8

C300931The Method Detection Limit (MDL) 1s the lowest concentration of analytethat a method can detect reliably 1n a sample or blank.

The Instrument Detection Limit (ID) 1s defined as the smallest signal abovebackground noise that an Instrument 1s able to detect reliably.The Limit of Quantltatlon (LOQ) 1s defined as the level above which aspecified degree of confidence may be otalned for the quantitative results.

Our lab has historically used published detection limits or contract requireddetection limits. In situations where we are validating methods for which thereare no detection limits (method or contractually defined), 1t will be ourresponsibility to correctly develop detection limits. It 1s Important tounderstand the concepts since the reportable results will fall Into differentregions of reliability.

The "General Method Validation Study" write-up which follows 1s written forthose methods which have already been written; the data produced from the studypresents our application of the method. If methods are truly developed by us,the number of samples will be required to Increase since statisticalconsiderations suggest that at least six degrees of freedom (ordinarily sevenmeasurements) should be Involved at each decision point.Classical validation processes Involve the use of standard reference materials(SRM) after generating preliminary data. This approach 1s more viable when theSRM are similar 1n all respects to the test samples. The use of SRM may beappropriate as a final validation step 1f the number and type of anjlytes, andthe matrix 1s the same. However, since many of the methods to be validated mustencompass a variety of matrices and a cross-section of analytes, SRM may not beavailable. This will not preclude the use of those materials as part of a QAprogram to periodically Insure us that our analytical systems are under control.

Generic Method Validation ProcedureThe procedure being presented here 1s applicable for the GC/MS, GC, andInorganics laboratories. The purpose of the testing program 1s to generateprecision, accuracy and recovery data on an aqueous and solid matrix, spikedwith analytes of Interest at one specified concentration. It should be used togain experience and to demonstrate our laboratory's capabilities 1n applyingprocedures which have already been written; e.g. SW 846 Methods, Method 601,602, etc. If our laboratory 1s truly developing a new method, another testingscheme would be applied.Validation of an organic method using only water and sand matrices 1s Judged tobe suitable only for those Instances where one or more surrogates can be used tomonitor the effectiveness of the method 1n more complex matrices. For thoseorganic methods where surrogates are not employed, testing additional matrices,e.g. - clay, planter's mix should be Incorporated Into the validation process.

FAC 001 0754


0300933A method validation study requires that laboratory notebooks be utilized 1norder to record any observations/problems encountered. Realistically, our SOPs,should not be written until we have experience 1n applying the method beingevaluated.The conduct of, and the results from, each step are to be documented 1nlaboratory notebooks. The notebooks should also serve to record anyrecommendations which can be made concerning a better application of the sampleprocessing, analysis, or data evaluation steps. The steps to be taken 1n thisvalidation process are as follows:

1. Desk Top Review

The method as written 1s read by a chemist familiar withextraction/work up procedures and the Instrumental detection systemsrequired. During this revelw, the chemist will particularly look for:A. Safety hazards.

B. Applicability of available Instrumental systems.C. New equipment/systems required that are not available.D. Discrepancies 1n the write up which do not appear to make sense

from a chemical analysis standpoint. Exceptions to the write upneed to be clearly Identified.

E. QA/QC requirements

2. Preparation of Lab PlanThe lab plan 1s essentially the testing approach to be taken andIncludes the proposed members of the "team" conducting the study andthe specific exceptions, 1f any, to be taken from the method aswritten. The lab plan will be presented for approval to a reviewcommittee consisting of the Laboratory Manager, the General Manager ofOperations, and the Director and/or Manager of Quality Assurance.

3. Preparation of Draft MethodThe draft method will be written. Use of a xerographic copy from astandard manual 1s acceptable.As an appendix to this draft method, the laboratory manager or projectmanager shall present the compounds to be spiked Into the matrices to betested. The analytes composing the spiking solutions should be allthose (organic or Inorganic) for which the method 1s being validated.

FAC 001 0755


C30Q933Subsequent laboratory proficiency tests or standard referencematerials, will be used on a routine basis to provide additional data onour application of the procedure.

4. Laboratory Analysis

The matrices being evaluated are clean sand and laboratory pure water.Method blanks consisting of allquots of the sand and water arerequired.Surrogate(s) are required for all organic procedures being evaluated.

When spiking these test samples, a minimum of one hour should elapseafter spiking and thoroughly mixing and before the sample preparationprocess. Recommendations for modifications to volatile spikingrequirements will be considered.The spiked matrices shall be prepared and analyzed using the methodwrite-up prepared under Item 3 above. If our method differs from thepublished method, both must be run.The spiking level to be analyzed 1n quadruplicate 1s:

An exact spiking level cannot be specified because the overallmethod recoverablHty 1s not known. Approximations of therecoverabHUy can be made and used to prepare the spiking level.Alternatively, preliminary data points can be obtained bygenerating some recovery data on one or more spikes, using anestimate of a mid-level concentration.

5. Detection Limit Run

After the data from section 4 (Laboratory Analysis above) 1s obtained,a formalized Method Detection Limit Study should be performed followingthe design specified by the EPA (for both water and sand matrices) 1nOctober 26, 1984 Federal Register.

6. Summary Report RequirementThe written report, documenting the experimented effort, will besubmitted to the Vice President, Laboratory Operations, for review.This report will Include as a minimum:a. Safety requirements for routine operation of the method 1n the

laboratory.

FAC 001 0756

Section: Appendix ARevision No. 2Date: October 17, 1988P a 9 e 7 o f 8 C300D34

b. A full description of the method Including all procedures andequipment used. This description must highlight deviations fromthe method as written 1n the applicable government regulation ormanual (e.g. SW-846 Manual, etc.).

c. A description of the matrices tested.

d. A comparison of results obtained with our method 1f different fromthe published method. Data should be tabulated to present actualresults per test sample per compound/element and the meanrecoveries and * RSD data. These reports should be as detailed aspossible since they will serve a threefold purpose:

- They will serve as the basis for the preparation of written SOPs,

- They will be used 1n marketing efforts for new product offeringsand will clearly demonstrate the extra effort which CompuChem*takes 1n providing analytical data of the highest quality, and

- Serve as the basis for documenting requests for equivalency ofCompuChem* methods to EPA published methods (1f necessary).

e. An assessment of any factors which may Interfere with or limit theproposed method.

f. A description of QC procedures necessary to ensure sensitivity,accuracy and precision. This may Include surrogate and QC spikingcompounds, acceptance criteria, continuing laboratory proficiencytesting, the use of SRMs, etc.

g. Recommendations and conclusions. Item b through g above arecritical 1f we must submit equivalency petitions to the Agency.

h. An estimate of time/cost of conducting the method Including specialcosts of reagents or standards required. The time estimates shouldInclude separate Items for sample preparation, Instrumentcalibration, software requirements, analysis and datareduction/assessment.

ManagementThe studies will be managed as follows: The Vice President, EnvironmentalOperations, will assign laboratory managers or project managers specific methodsneeding validation and approve the selection of the subsequent "team* members.The project manager or the laboratory manager will be designated to guide theeffort and will be responsible for the preparation of the required reports.

FAC 001 0757


REFERENCES 0300831

1. Taylor, John K., Analytical Chemistry, 1983, 55, "Validation of AnalyticalMethods", 600A - 608A.

2. ACS Committee on Environmental Improvement, "Principles of EnvironmentalAnalysis", Analytical Chemistry, 1983, 55, 2210 - 2222.

3. Long, Gary L., VMnefordner, J.D., "Limit of Detection: A Closer Look at theIUPAC Definition", Analytical Chemistry 1983, 55, 713A - 724A.

4. Kratochlrl, Byron, Taylor John K., "Sampling for Chemical Analysis",Analytical Chemistry, 53, 1981, 925A - 938A.

5. Taylor, John K., "Quality Assurance of Chemical Measurements", AnalyticalChemistry, 53, 1981, 1588A - 1596A.

6. Glaser, John A., et-al., "Theory and Application of Method Detection Limit",Environmental Science and Technology, 1981, 51, 1426 - 1435.

PAC 0758

Appendix BRevision No. 4Date: October

C 3 0 0 9 4 0

17, 1988

Richard L. BloomDirector, ProductionCompuChem* Corporation

Responsibility:

Education:

Experience:

As Director of Production, Mr. Bloom 1sresponsible for the production/schedulingoperation, assuring the timely turn-around ofsample analyses 1n order to satisfy customercommitments.Mr. Bloom received an BA degree 1nBusiness Administration from NorthCarolina State University In 1978.

Before being promoted to his currentposition,'Mr. Bloom was employed as Manager,Production Planning and Control withCompuChem* Laboratories.Prior to Joining CompuChem*, Mr. Bloom wasemployed by Data General Corp., where he heldpositions as a Production Control Supervisorand as a Material Requirement Planner.

FAC 001 0759

Appendix BRevision No. 4Date: October 17,

C3000411988

Robert E. MelererDirector Quality AssuranceCompuChem* Corporation

Responsibilities:

Education:

Experience:

Since 1983, Mr. Melerer has been the Directorof Quality Assurance and responsible forassuring that all Corporate laboratories(CompuChem* Laboratories and ChemWestLaboratories) consistently produce highquality and reliable data and that allnecessary certification and licensingrequirements are met by the laboratories.Mr. Melerer received an Associate degree1n Industrial Chemistry from the ErieCounty Technical Institute 1n 1963, and anundergaduate degree 1n Chemistry from theState University of New York at Buffalo 1n1971. He has taken advanced studies 1nAnalytical Chemistry and BusinessAdministration from the State Universityat Buffalo.Prior to joining CompuChem*, Mr. Melererheld positions as Laboratory Manager withRadian Corporation and as Department Head,Aialytlcal Laboratory; SpecialContamination Monitoring, The CarborundumCompany from 1969 - 1980.In his previous position with CompuChem*as Technical Development Scientist, Mr.Melerer was responsible for providingtechnical assistance to operationallaboratories for procedure development andImplementation and problem solving. Mr.Melerer has previously been employed withCompuChem* as Manager of AnalyticalLaboratories where he was responsible fordirecting the efforts for the SamplePreparation Laboratories, the InorganicLaboratory, the GC Laboratory, and theStandards Laboratory.Through the variety of laboratory positionsMr. Melerer had held, he has gained ten (10)years of experience In the Interpretation ofmass spectra gathered 1n GC/MS analysis.Additionally, Mr. Melerer has gained six (6)years experience 1n the preparation ofextracts from environmental or hazardous

001 0760

Appendix BRevision No. 4Date: October 17, 1988

0 3 0 0 0 3 0

APPENDIX

Resumes and Experience

Of Key Technical Personnel

1 FAC 001 0761t


030093?The Environmental Protection Agency (EPA) requires the following experience

levels for technical personnel who analyze EPA samples. Please note thatCompuChem*'s laboratory staff exceed these requirements.

ORGANICS:

a. The Contractor's GC/MS operators performing work on this contract shall eachhave at least 9 months experience 1n the operation of the GC/MS/DS onenvironmental samples.

b. The Contractor's mass spectral Interpretation specialist performing work onthis contract shall have at least 2 years of experience (as used herein,"experience" 1s deemed to mean, "more than 50 percent of the personnel'sproductive work time") 1n the Interpretation of mass spectra gathered 1nGC/MS analysis.

c. The Contractor's extraction and concentration specialist performing work onthis contract shall have at least 1 year experience 1n the preparation ofextracts from environmental or hazardous waste samples.

d. The Contractor's purge and trap specialist performing work on this contractshall have at least 6 months experience using the purge and trap techniquefor volatile organlcs.

e. The Contractor's pesticide residue analysis specialist performing work onthis contract shall have at least 2 years experience 1n organochlorlnepesticide residue and PCB analysis, Including clean-up procedures such ascolumn chromatography, on environmental samples.

INORGANICS:a. The ICP Spectroscoplst responsible for work under this contract must have at

least 1 year experience 1n the operations of the ICP on environmentalsamples.

b. The Flameless Atomic Absorption (AA) Spectroscoplst responsible for the workon this contract must have at least 1 year experience 1n the operation offTameless AAS on environmental samples.

c. The Flame and Cold Vapor Atomic Absorption Spectroscoplst responsible forthe work on this contract must have at least 9 months experience 1n theoperation of flame and cold vapor AA on environmental samples.

d. The Inorganic Sample Preparation Expert performing sample preparation forthis contract must have at least 3 months experience 1n the preparation ofICP and AA samples and standards.

I i

j

FAC 001 0762


C 3 0 0 9 3 6e. The Classical Inorganic Techniques Analyst (Cyanide Analyst) responsible for

work on this contract must have at least 6 months experience 1n themeasurement of cyanide 1n environmental samples.

PAC 001 0763


0300039G.C. VERKERK

Chief Executive Officer and PresidentCompuChem* Corporation

Responsibilities:

Education:

Experience:

Or. Verkerk 1s Chief Executive Officerand President and 1s responsible for the dayto day operations of CompuChem's analyticallaboratories and the management of the totalbusiness function.

Mr. Verkerk received his Doctorandus (Drs.)degree 1n Economics and BusinessAdministration from Vrlje University,Amsterdam, the Netherlands 1n 1977.

Prior to joining CompuChem*, he wasemployed as Vice President and ChiefFinancial Officer at Signal EnvironmentalSystems, where he was accountable forfinancial management and results.Mr. Verkerk has held various financialgeneral management positions atM. W. Kellogg 1n the United States andEurope.

and

FAC 001 0764

Appendix BRevision No. 4Date: October

C 3 0 0 9 4 0

17, 1988

Richard L. BloomDirector, ProductionCompuChem* Corporation

Responsibility:

Education:

Experience:

As Director of Production, Mr. Bloom 1sresponsible for the production/schedulingoperation, assuring the timely turn-around ofsample analyses 1n order to satisfy customercommitments.Mr. Bloom received an BA degree 1nBusiness Administration from NorthCarolina State University 1n 1978.Before being promoted to his currentposition,'Mr. Bloom was employed as Manager,Production Planning and Control withCompuChem* Laboratories.Prior to Joining CompuChem*, Mr. Bloom wasemployed by Data General Corp., where he heldpositions as a Production Control Supervisorand as a Material Requirement Planner.

FAC 001 0765


C 3 0 0 0 4 11988

Robert E. MelererDirector Quality AssuranceCompuChem* Corporation

Responsibilities:

Education:

Experience:

Since 1983, Mr. Melerer has been the Directorof Quality Assurance and responsible forassuring that all Corporate laboratories{CompuChem* Laboratories and ChemWestLaboratories) consistently produce highquality and reliable data and that allnecessary certification and licensingrequirements are met by the laboratories.

Mr. Melerer received an Associate degree1n Industrial Chemistry from the ErieCounty Technical Institute 1n 1963, and anundergaduate degree 1n Chemistry from theState University of New York at Buffalo 1n1971. He has taken advanced studies 1nAnalytical Chemistry and BusinessAdministration from the State Universityat Buffalo.Prior to joining CompuChem®, Mr. Melererheld positions as Laboratory Manager withRadian Corporation and as Department Head,Aialytlcal Laboratory; SpecialContamination Monitoring, The CarborundumCompany from 1969 - 1980.In his previous position with CompuChem®as Technical Development Scientist, Mr.Melerer was responsible for providingtechnical assistance to operationallaboratories for procedure development andImplementation and problem solving. Mr.Melerer has previously been employed withCompuChem* as Manager of AnalyticalLaboratories where he was responsible fordirecting the efforts for the SamplePreparation Laboratories, the InorganicLaboratory, the GC Laboratory, and theStandards Laboratory.Through the variety of laboratory positionsMr. Melerer had held, he has gained ten (10)years of experience 1n the Interpretation ofmass spectra gathered 1n GC/MS analysis.Additionally, Mr. Melerer has gained six (6)years experience 1n the preparation ofextracts from environmental or hazardous

001 0766


1300942

Experience cont'd.

Publications:

waste samples. Further, he has gained three(3) years experience 1n organochlorlnepesticide residue and PCB analysis, Includingclean-up procedures such as columnchromatography, on environmental samples.

Melerer, R.E., "Laboratory Data Credibilityand Reliability," the paper presented 1nMilwaukee, Wisconsin on March 8, 1980, at theFederation of Environmental TechnologistsConference.Melerer, R.E., Myers R.L., WMtehead, R.J.,"Quality Assurance Studies Based On Analyti-cal Condition Codes," paper presented to theFifth Annual ERA Contract Laboratory ProgramConference, U.S. EPA, August 1, 1985.Melerer, R.E., "GC/MS: Applications For TheDetermination of Organic Constituents InHazardous Waste," paper presented at theTwelfth Annual Conference on WasteTechnology, NSWMA, October 18, 1983.

Melerer, R.E., Ragsdale P.L., and Mills,P.E., "Quality Assurance of SupportFunctions In A Large Hazardous WastesAnalytical Laboratory," paper presentedbefore the division of EnvironmentalChemistry, American Chemical Society,March 29, 1982.

Shaffer, P.T.B., Melerer, R.E., McGee, C.D.,"Virus Recovery From Natural Water" JAWWA.,69 (10). 528-531 (1977).Cook, G.A., Melerer, R.E., and Shields, B.M."Combustibility Tests on SeveralFlame-Resistant Fabrics 1n Compressed A1r,Oxygen Enriched A1r, and Pure Oxygen."Textile Research. 37:591 (1967).Cook, G.A., Melerer, R. E., Shields, BM.,and Nevlns, H.E. "Effects of Gas Compositionon Burning Rates Inside DecompressionChambers at Pressures Up To 350 Feet of SeaWater." Paper presented at 54th AnnualMeeting, Under-Ocean Technology, January 17,1967 (Published by the Compressed GasAssociation).

FAC 001 0767


Robert J. WhlteheadManager of Quality AssuranceCompuChem* Laboratories

Responsibility:

Education:

Experience:

As the Manager of Quality Assurance,Mr. Whltehead 1s responsible for managing theEnvironment QA and Forensic Drug Testing QAoperations.Mr. Whltehead received an undergraduate degree1n Biology, with a secondary emphasis 1nChemistry, from the University of NorthCarolina at Chapel H111. Mr. Whltehead hasalso participated 1n a number of ContinuingEducation Programs and symposia associatedwith Statistical Quality Control, AnalyticalQA/QC, Analytical Techniques, Waste Testingand Quality Assurance, Quality CirclesConcepts, and Advanced Leadership Training.Before his promotion to Manager of QualityAssurance, Mr. Whltehead was employed atCompuChem* Laboratories as a Sr. QASpecialist, responsible for ensuring that datagenerated by all lab stations complied withestablished acceptance criteria. Prior tothis, Mr. Whltehead was employed at CompuChem*Laboratories as a GC/MS Operator, withresponsibility for the operation of a GC/MSsystem, spectral Interpretation, andquantitative data analyses. Prior to JoiningCompuChem* Laboratories on a full time basis,Mr. Whltehead had been employed 1n the GC/MSLab on a part-time basis, during his senioryear 1n college.Mr. Whltehead has 2 years of experience 1n theoperation of the GC/MS/DS on environmentalsamples and 8 years of experience 1n theInterpretation of mass spectra gathered 1nGC/MS analysis. Mr. Whltehead also has 2years of experience using the purge and trap

FAC 001 0768


13909441988

Experience cont'd.:

Publications:

technique for volatile organlcs and 1 year ofexperience 1n the preparation of extracts fromenvironmental or hazardous waste samples.Additionally Mr. WMtehead has 5 yearsexperience 1n conducting QA systems andperformance audits, and has been directlyInvolved 1n the development of numerous QAProject Plans and QA Program Plans followingQAMS-005/80 and QAMS-004/80 guidelines.

Whltehead, R. J., "Laboratory Data Credibilityand Reliability," the paper presented InMHqaukee, Wisconsin on March 8, 1980, at theFederation of Environmental TechnollglstsConference.Whltehead, R. J., "Statistical Quality Controlfor the Analytical Laboratory," Proceedingsfrom the Analytical Techniques and ResidualsManagement In Water Po11ut1on~Contr7rSpec 1la 1ty"Conference. Water Pollution ControlFederation, April 20, 1988.

PAC 001 0769


03009451988

Peter H111Quality Assurance SpecialistCompuChem* Laboratories

Responsibilities:

Education:

Experience:

As a Quality Assurance Specialist, Mr. H111ensures that laboratory generated datacomplies with established acceptancecriteria and he assists 1n resolvingproblems Identified with data.

Mr. H111 received an undergraduate degree1n Chemistry 1n May 1982, at GullfordCollege.Before Mr. H111 was promoted to QA Specialist1n October 1987, he was a Technical Reviewer.The Technical Reviewer's position was a finalreview of data packages for completeness andcompliance to protocol. This position washeld from August 86' to October 87'. Prior tojoining CompuChem* Mr. H111 held the positionof Chemist from March 85' to August 86'atEnvironmental Testing Inc. Hisresponsibilities Included the collection,analysis and reporting of samples whichIncluded air, water, soil and sludge, Thesesamples were analyzed via GC, AA, classicalwet chemistry at gravlometrlc.

FAC 001 0770


Roh1n1 JoshlQuality Assurance SpecialistCompuChem* Laboratories

Responsibilities:

Education:

Experience:

As a Quality Assurance Specialist, Ms. Joshlensures that laboratory generated datacomplies with established acceptancecriteria and she assists 1n resolvingproblems Identified with data.Ms. Joshl received an undergraduate degree 1nChemistry from Gujarat University. Ahmedabad,India. Ms. Joshl also received a Mastersdegree 1n organic Chemistry from GujaratUniversity.Prior to her promotion to QA Specialist,Ms. Joshl was employed at CompuChem* as aTechnical Reviewer and a GC/MS OperatorTrainee, holding the responsibility ofdata review and producing timely andaccurate sample analysis using the GC/MSsystem. Prior to Joining CompuChem*,Ms. Joshl was employed by the North CarolinaDepartment of Agriculture Food 4 DrugProtection Agency and held the title ofInstrumentation and Wet Chemist.Ms. Joshl has 1 year of experience 1n theoperation of the GC/MS/DS on environmentalsamples and experience 1n Instrumentationand wet chemistry. In addition, Ms. Joshl has4 years laboratory QA/QC managerialexperience.

FAC 001 0771


0300947

Joe ButngarnerManager of Sample Preparation Laboratory

CompuChem® Laboratories

Responsibilities;

Education:

Experience:

In 1988 Mr. Bumgarner was promoted to hispresent position where he manages thepreparation of Samples 1n his department, aswell as managing the Organic CharacterizationLaboratory where the analyses of TotalPetroleum Hydrocarbons (TPH), Total OrganicCarbon (TOO, and Total Organic Holldes (TOX)1s performed.Mr. Bumgarner received an undergraduatedegree In Biology from Garner-Webb College 1n1985.Mr. Bumgarner joined CompuChem* 1n May, 1985as Senior Laboratory Assistant. In October1985, he was promoted to Supervisor of theSample Preparation Laboratory, where he wasresponsible for the supervision of theactivities of the Sample Preparation Labensuring that high quality work was performed1n a timely and efficient manner.

002


C300948Debra L. Stanley

Supervisor Sample Preparation Laboratory (2nd shift)CompuChem" Laboratories

Responsibility:

Education:

Experience:

Ms. Stanley was promoted to her presentposition on June 1, 1986 and 1s responsiblefor the supervision of the activities of theSamples Preparation Laboratory ensuring thathigh quality work 1s performed 1n a timely andefficient manner.

Ms. Stanley received an A.A.S. degree 1nMedical Technology from Career Academy,Atlanta, GA 1n 1972.

From 1972 to 1979, Ms. Stanley was employedas Medical Technician at Spring Hope Clinic.From 1976 to 1979, she was employed asPed1atr1c Nurse with Drs1. Poole, Wlnslow,and Brown.

Since joining CompuChem* on May 12, 1980, Ms.Stanley has held positions as LaboratoryTechnician, GC/MS Operator Trainee, and GC/MSOperator.

001 0773


C300&49Stephen G. Ualburn

Manager Organlcs LaboratoryCompuChem* Laboratories

Responsibility:

Education:

Experience:

Mr. Walburn has held the position of Manager1n the GC/MS Laboratory since January 1987.In this capacity he 1s responsible for themanagement of all technical aspects of thethree-shift environmental GC/MS Laboratories.

Mr. Walburn received a B.S. degree 1nChemistry and a B.S. degree 1n TextileChemistry from N.C. State University 1n 1974.He pursued advanced organic chemistry studiesat N.C. State University from 1974 - 1977.From October 1977 to June 1981, Mr. Walburnwas employed as Senior Chemist with NorthropServices, Inc..Mr. Walburn joined CompuChem* asSpectroscop1st In June of 1981. He alsoheld the position of Assistant Manager GC/MSLaboratory.

FAC 001 0774


Charles T. MannSupervisor of the GC/MS LabCompuChem* Laboratories

C300950

Responsibilities:

Education:

Experience:

On 2/29/88 Mr. Mann became Supervisor of theGC/MS Laboratory, where he 1s responsible forensuring that the production of theSemi-Volatile Laboratory on a single shift 1sconducted 1n a timely and accurate manner.This Includes coordinating the productioneffort with the Supervisors on other shifts.Mr. Mann 1s responsible for evaluating anddeveloping methods for Improving the qualityand quantity of the data produced. Otherresponsibilities Include: providing technicalguidance and Input for new contractrequirements and/or new products; planning andscheduling work assignments according toanalysis requirements; assigning Individualwork schedules based on analysis requirementsand capabilities of the department staff;being responsible for Interviewing, selectingorienting, and training new employees;determining training needs of currentemployees and defining a plan of action toaddress the training requirements; providingrecommendations for promotions and lateraltransfers; conducting performance appraisals,recommending merit Increases and reviewingmerit Increases with employees; beingresponsible for communicating and ensuringthat all departmental employees understand andadhere to all company policies and procedures;maintaining an awareness of all Federal,State, and local rules and regulations thatpertain to employment practices. I.e., Wageand Hour laws, Equal Employment Opportunity,and OSHA regulations; and being responsiblefor safety attitudes and practices; and forthe overall houskeeplng of the Semi-VolatileLaboratory.

Mr. Mann received a B.A. 1n Chemistry fromWake Forest University 1n 1985.Mr. Mann joined CompuChem* as a GC/MSTechnician during the summer of 1984 and onweekends prior to his permanent employment on

FAC 001 0775


C3009S1Experience cont'd.: May 28, 1985. He has over one (1) year of

experience 1n the operation of a GC/MS/DS onenvironmental samples. Mr. Mann was promotedto this present position on June 3, 1986 wherehe was responsible for performing timely andaccurate analysis of samples using GC/MS.

001 0776


8111 D. L1v1ngstonSupervisor 2nd Shift GC/MS LaboratoryCompuChem* Laboratories

0300952

Responsibilities:

Education:

Experience:

In his current position, he 1s responsiblefor analyzing and Interpreting samples usingGC/MS.

Mr. L1v1ngston received a B.S. degree 1nBiology with a minor 1n Chemistry fromGardner-Webb 1n 1981.

From 1981 to 1983, Mr. L1v1ngston worked asChemical Technologist with Roche B1omed1calLaboratories.Mr. L1v1ngston joined CompuChem* 1n Februaryof 1983 as B1omed1cal Technician. Since thenhe has held positions as GC/MS OperatorTrainee and GC/MS Operator.

PAC 001 0777


C300953Susan Bass

Manager Volatile LaboratoryCompuChem* Laboratories

Responsibilities:

Education:

Experience:

As Manager of the Volatile Laboratory, Ms.Bass 1s responsible for the preparation andanalysis of environmental volatile samplesutilizing GC/MS and for the generation ofcomplete data packages. She 1s responsible forfor managing the multi-shift VolatileLaboratory ensuring that timely and accurateproduction 1s achieved.

Ms. Bass received her B.S. degree 1nChemistry from Meredith College 1n 1978.

Prior to working for CompuChem*, Ms. Basswas employed by the North CarolinaDepartment of Agriculture as a ChemicalAnalyst from 1979 - 1980. Also, she wasemployed by Becton Dlckerson and Company asa Research Assistant from 1980 - 1981.Ms. Bass Joined CompuChem* April of 1981 asa Junior GC/MS Operator and held positionsof GC/MS Operator and Senior GC/MS Operatorbefore being promoted to her current position ofProject Volatile Manage.

pAC 001 0778


Guy R. Lambert Jr.Chemist II

CompuChem* Laboratories

C300984

Responsibilities:

Education:

Experience:

On January 27, 1986, Mr. Lambert was promotedto Chemist II being responsible for theanalysis of environmental volatile samplesutilizing GC/MS and for the generations ofcomplete data packages 1n an accurate andtimely manner. This position also serves as aTechnical Advisor to other GC/MS Operators andTrainees on a particular shift.

Mr. Lambert received an A. B. degree 1nBiology from Duke University 1n 1982.

Mr. Lambert Joined CompuChem* 1n 1983 and hasheld positions as GC/MS Operator andB1omed1cal Technician 1n the OperationsLaboratory.

Mr. Lambert has received two years training 1ngeneral and organic chemistry. Additionally,he has received experience 1n public schoolteaching. He has gained three months ofexperience 1n the preparation and analysis ofsamples from biological matrices. Mr. Lamberthas also gained three (3) years and nine (9)months of experience 1n the operation of theGC/MS/DS on environmental samples.

FAC 001 0779


0300955Alberto MaldonadoChemist II


Responsibility: As a Chemist II, Mr. Maldonado 1s responsiblefor the analysis of environmental volatilesamples utilizing GC/MS 1n an accurate andtimely manner.

Education: Mr. Maldonado received his B.S. 1n Chemistryat Intramerlcan University of Puerto R1co 1n1986.

Experience: Prior to CompuChem*, Mr. Maldonado wasemployed by RDU Airport as a Driver fromJuly, 1986 - April, 1987.

FAC 001 0780


Owen K. StudtChemist II


0300956

Responsibility:

Education:

Experience:

Mr. Studt 1s responsible for the analysis ofenvironmental volatile samples utilizing GC/MS1n an accurate and timely manner.

Mr. Studt received an undergraduate degree 1nPhysics from Elon College 1n 1983 and Ispursuing studies 1n Business ComputerProgramming at Durham Technical Institute.Mr. Studt received a certificate 1n ElectronicAssembly (72 hours) from Durham TechnicalInstitute 1n 1985.On 7/18/88 Mr. Studt became a GC/MS Operatorresponsible for analyzing and Interpretingsamples using GC/MS.

Prior to accepting his present position, Mr.Studt was employed at AKD Gardens as aSupervisor/Analyst from 1983-1984.Mr. Studt .'olned CompuChem* on May 22, 1985.Mr. Studt was promoted to GC Technician onJune 30, 1986 and was responsible forproviding technical support for the GC Lab.He performed routine equipment and computerchecks. Studt was responsible for the generaloperation of the GC Lab which Includedprioritizing samples analysis. He alsoperformed standard evaluation checks andevaluated GC Screens both qualitatively andquantitatively.

FAC 001 0781


William R. DesjardlnsManager,- GC Projects


C300957

Respons1b1l11es:

Education:

Experience:

Mr. DesJardlns 1s employed at CompuChem* asManager of GC Projects, 1n the GC Laboratory,with responsibility for the development andapplication of GC methods for samplesrequiring analysis using ECO, FID, NPD and PFDdetectors.

Mr. DesJardlns received a B.S. degreeBiology from Gullford College 1nGreensboro, NC 1n 1980.

1n

Prior to coming to work art CompuChem*,Mr. DesJardlns was employed by theOccupational Health Studies Group as a LabTechnician, where his duties Includedperforming GC analysis of dust, solvent andair samples.Mr. DesJardlns has 1 year of experience 1n thepreparation of extracts from environmental orhazardous waste samples and 5 years experience1n organochlorlne pesticide residue and PCBanalysis, Including clean-up procedures suchas column chromatography on environmentalsamples.

PAC 001 0782

Append ix BRevision No. 4Date: October 17, 1988

C300958Douglas P. McCormack

Chemist IIICompuChem* Laboratories

Responsibilities:

Education:

Experience:

Mr. McCormack was promoted to Chemist III onApril 7, 1986 and 1s responsible fordeveloping and applying gas chromatographlcmethods for the analysis of pesticides andother toxic materials, Including Interpretingthe resulting data.

Mr. McCormack received an undergraduate degree1n Environmental Chemistry and Biology fromEast Carolina University and a Masters Degree1n Plant Pathology from North Carolina StateUniversity.From 1981 - 1984 Mr. McCormack was employed atNorth Carolina State University as a ResearchAssistant. From 1977 - 1981. Mr. McCormackwas employed at Durham County HealthDepartment as a Sanitarian II.

FAC 001 0783


Mellssa TyndallGC Chemist II

CompuChert* LaboratoriesC300959

Responsibility:

Education:

Experience:

Ms. Tyndall 1s responsible for analyzing601/602 data.Ms. Tyndall received a BA degree 1nChemistry/Zoology at UNC-Chapel H111, NC.Ms. Tyndall has life years of clinical analysisexperience.

001


Bruce H. RohrbachManager Inorganics Laboratory


C300960

Responsibility:

Education:

Experience:

Mr. Rohrbach Joined CompuChem* onFebruary 2, 1987 and 1s responsible formanaging the Inorganics Laboratory ensuringthe production of accurate data 1n a cost andtime effective manner so that laboratory goalsare met.

Mr. Rohrbach received an BA degree 1nChemistry from West Chester State University1n 1972.

From 1986-1987 Mr. Rohrbach was InorganicsLaboratory Manager with Ecology andEnvironment, Inc. Additionally, he wasemployed as a Research Chemist with AlliedCorporation from 1980-1986. Mr. Rohrbach wasemployed with Allentown Testing Lab as ChiefChemist/Laboratory Supervisor (1975-1980);Chemical Testing Laboratory Manager(1973-1975); and Analytical Chemist(1972-1973).

FAC 001 0785


John C. TzavarasDevelopmental Chemist IICompuChem® Laboratories

0300901

Responsibilities:

Education:

Experience:

As Developmental Chemist II, Mr. Tzavaras has.been responsible for the training of all labIndividuals 1n the preparation and analysesof samples of all types for the determinationof metals, cyanide, phenols and any otherInorganic constituent using Instrumentationavailable 1n the Inorganics laboratory. He 1salso responsible for the review of data from atechnical quality standpoint.Mr. Tzavaras received an undergraduate degree1n Chemistry from Tufts University 1n 1976and an A.A.S. degree from Durham TechnicalInstitute 1n Electronics EngineeringTechnology 1n 1985.From 1977 - 1980 Mr. Tzavaras was employed byInstrumentation Laboratory as a ProductSpecialist. From 1976 - 1977. Mr. Tzavaraswas employed by Herbert V. Shuster, Inc. as anAnalytical Chemist.

FAC 001 0786


C300962Donald Stogner

Chemist IICompuChem* Laboratories

Responsibilities: Mr. Stogner 1s responsible for analyzingsamples by Furnace, ICAP, Technlcon, ColdVapor and the transferring of data to DataBase.

Education: Mr. Stogner received an undergraduate degree1n Chemistry from N.C. State University.

Experience: Prior to being promoted to Junior Chemist,Mr. Stogner was employed at CompuChem* as aSenior Inorganics Technician after beingpromoted from an Inorganics Technician.

FAC 001 0787


Mark Crews C30 0-963Chemist II

CompuChem® Laboratories

Responsibility: As a Chemist II, Mr. Crews 1s responsible forperforming sample analysis using ICP andflame/furnace AAS.

Education: Mr. Crews earned a B.S. 1n Chemistry from WakeTechnical School 1n 1987.

Experience: Mr. Crews worked as a Chemist from 1986 - 1987at Basslck Sack, and 1s presently employed asa Chemist II as of 1987.


James E. MedUn C300964Inorganic Chemist II


Responsibilities: As an Torganlc Chemist II, Mr. MedUn 1sresponsible for the analysis of Inorganicsamples by Flame AA, Graphite Furnace AA,ICAP, and Cold Vapor Hg.

Education: Mr. MedUn received a BS 1n Chemistry atAppalachian State Unv1ers1ty 1n 1987.

Experience: Mr. Hedlln has experience 1n Instruction andexperience 1n Atomic Absorption and six monthsas an Inorganic Technician.

001 0789


Angela ChlldressManager, Production Planning & Control


C300965

Responsibility:

Education:

Experience:

As Manager, of the Production Planning and ControlDepartment, Ms. ChUdress 1s responsible formanaging the dally activities of the production andscheduling function to ensure schedules orcommitments are met.

Ms. ChUdress received a Master of BusinessAdministration degree at the University ofArkansas, July 1983. She received a BS degree 1nIndustrial Management from the University ofArkansas, May 1980.

From August 1987 to November 1988 Ms. ChUdress wasemployed as an Industrial Engineer at CompuChem*Laboratories where she Initiated the first costanalysis for 80* of the Environmental productline. She also served as management trainer forthe Zenger-MUler Supervisory Training Program.She Initiated the first labor standards for use 1nscheduling, capacity planning, and lab floorcontrol, and she coordinated with the ProductionPlanning & Control manager 1n establishing thefirst centralized scheduling program. Ms.CMldress developed work station lay-outs withinthe environmental and clinical laboratories toIncrease employee efficiency through Improved flow.Ms. Chlldress coordinated with and assisted theCoopers & Lybrand consulting team 1n analysis ofthe current environmental laboratory operation.From July 1987 to August 1987, Ms. Chlldress was aself employed Management Consultant at Johnson &Johnson - Chlcopee Division, Benson, NC, where sheconducted a warehouse utilization study thatreviewed space allocation, personnel/equipmentutilization, and product flow with recommendationsfrom Increased efficiency, Improved laborutilization, and smoother material flow.From April 1984 to June 1987 Ms. Chlldress workedas an Industrial Engineering Supervisor at Johnson& Johnson - Chlcopee Division, North Little Rock,AR. At this company she monitored N.L.R. Incentiveplan affecting 110 wage personnel. She superviseda technician and an Incentive clerk, and determinedlabor and production rates for new and revisedproduct cost estimates.

FAC 001 0790


C300906

Experience cont'd.: Ms. ChUdress also performed I.E. project work for2 plants 1n N.L.R. (400 people), 1 plant 1n Camden,AR (150 people), 4 1 plant 1n Benson, NC (200people). She also served as speaker for localschools.From July 1980 to February 1984 Ms. ChUdress wasemployed as a Work Management Coordinator, atLittle Rock Municipal Water Works 1n Little Rock,AR. She designed and Implemented a computergenerated work order system used by 60 fieldpersonnel. Ms. ChUdress developed and conductedtraining for a new work order system, standards,and Quality Circles. She designed 4 Implemented a"real time" Inventory control system and served asthe first Quality Circles facilitator at thefacility. Ms. Chlldress established Initial 49times standards 4 optimum work methods for fieldpersonnel and served as speaker for the NationalWater Works Association conference 1n Las Vegas,the Central Arkansas Compensation Association, andthe Arkansas Water Managers' Association.

FAC 001 0791


Anh T. ChanManager Data Review


C300967

Responsibilities:

Education:

Experience:

Ms. Chan has held the position of Manager ofData Review since January 1987. In thiscapacity she 1s responsible for ensuring thesteady flow of the reviewed data from theGC/MS lab to the Production, Planning andControl Departments 1n order to meet theprojected deadline, to make technicaljudgements and decisions on anomalous data, tomaintain close contacts with the QualityControl and Quality Assurance Departments witha view to producing the highest quality data,to serve as a feedback mechanism to the GC/MSlab, and ensure completion of data withoutdelay.Ms. Chan received her B.A. degree 1nGeneral Science with emphasis 1n Chemistryfrom Brandels University 1n 1977.Prior to joining CompuChem*, Ms. Chan wasemployed by the'Research and AnalyticalLaboratory, School of Public Health,University of North Carolina, Chapel H111as a Senior Research Technician from July,1979 - October, 1979.Ms. Chan Joined CompuChem* November 1979as a GC/MS Operator and also held theposition of Senior GC/MS Operator andSpectroscoplst before being promoted toAssistant Manager of GC/MS. In October 1986Ms. Chan was responsible for the supervisionof Environmental GC/MS data review. She wasthen promoted to Manager of Data Revelw.

FAC 001 0792


0300963Michael Mattocks

Data Review SpecialistCompuChem* Laboratories

Responsibilities:

Education:

Experience:

As a Data Review Specialist Mr. Mattocks 1sresponsible for assuring the technical qualityof commerlcal data by performing technicalaudits and monitoring laboratory trends.

Mr. Mattocks received a B.S. 1n Chemistry fromNorth Carolina Central University 1n 1986.

From February 1983 to September 1986, Mr.Mattocks was employed as Lab Technician withNIEHS. From September 1986 to May 1986, Mr.Mattocks was employed with Duke University asLaboratory Assistant.Mr. Mattocks joined CompuChem" as GC/MSTrainee on June 29, 1986. On March 30, 1987,he was promoted to GC/MS Operator and wasresponsible for analyzing and Interpretingsamples using GC/MS.

FAC 001 0793


Ann Marie FlahertyManager, Report Preparation/Tech Review

CompuChem* LaboratoriesC300969

Responsibilities:

Education:

Experience:

On November 14, 1988 Ms. Flaherty becameManager of the Report Preparation/TechnicalReview Department, responsible for theIntegration, technical review and audit, wordprocessing and full service dellverablespackage of the data generated by Compuchem'sanalysis procedures.Ms. Flaherty received an undergraduate degree1n Industrial Relations/Psychology from theUniversity of North Carolina at Chapel H1111n 1982.Ms. Flaherty was employed at IBM 1n 1982 as aPP4C Clerk. Prior to being promoted to hercurrent position, Ms. Flaherty held positionsas Scheduling Clerk, Report Integration Clerkand Supervisor Scheduling and Sample Saver.Ms. Flaherty was promoted to Manager ofProduction Planning and Control on October 20,1986 and was responsible for managing dallyactivities of the Production and Schedulingfunctions.She has attended several seminars IncludingFundamentals of Supervision (24 hours) atCapital Associated Industries 1n 1985,Advanced Leadership Development Program (27hours) at CAI 1n 1985, and Zenger MUlerFrontline Leadership Training (24 hours) 1n1988.

FAC 001 0794


Jeanne C. AlstonFinal Technical ReviewerCompuChem* Laboratories 0300970

Responsibilities:

Education:

Experience:

On December 14, 1988 Ms. Alston joinedCompuChem* Laboratories as a Final TechnicalReviewer, responsible for the review of EPAand commercial organic samples and commercial,Commercial CLP and EPA Inorganic samples suchthat adherence to contract protocols andInternal quality guidelines are met. Sheresolves Issues/Incidents noted 1n the reviewprocess with the director/manager to ensureInternal quality of deliverable data. Ms.Alston also documents and tracts theIssues/Incidents noted 1n the review processto communicate with lab managers. Ms. Alston1s also responsible for Interpretation ofcurrent contract requirements and currentstatement of work documents.Ms. Alston received a B.S. degree 1n chemistryfrom the University of North Carolina 1nChapel Hill, NC on August 12, 1985.Prior to Joining CompuChem*, Ms. Alston wasemployed by Triangle Laboratories beingresponsible for the extraction and clean-up(via liquid chromatography techniques) ofdloxWfuran samples. Later she learned tooperate a VG-.magnetic high resolution 6C/MSfor dloxln/furan analysis, then she learned tooperate a VG-low resolution quadropole GC/MSfor volatile analysis. Ms. Alston trainedagain 1n the wet lab to learn SOPs for theextraction of SV and Pesticide samples,afterwhlch, she rotated between positions asneeded. Ms. Alston's other responsibilitiesIncluded the preparation and spiking of XADtraps and VOST (volatile organic samplingtrain) tubes.

FAC 001 0795

Appendix CRevision No. 2Date: August 11, 1986Page 1 of 47

C300971

APPENDIX C:

Table of Contents To TheSOP Manual: Environmental

And The

SOPs For The Preparation. Analysis. AndData Assessment Of Environmental Samples

FAC 001 0796


0300972

Standard Operating Procedures

Environmental

CompuChem* LaboratoriesP. 0. Box 12652

3308 Chapel Hill/Nelson HighwayResearch Triangle Park

N.C. 27709

Copy Number:Issued To:

Date:Returned To:

Date:

FAC 001 0797


C300973

Standard Operating ProceduresFor

Production Planning and Control

ConpuChea Laboratories

FAC 001 0798


T . b l e O f C o n t e n t s C300974Production Planning and Control: Introduction

Production Planning and Control SOP 1.1: Logging In Samples

Production Planning and Control SOP 1.2: Storing Samples

Production Planning and Control SOP 1.3: D1ox1n Samples

Production Planning and Control SOP 1.4: Purging Samples

Production Planning and Control SOP 1.5: SampleSaver* Preparation

Production Planning and Control SOP 1.6: SubcontractorsSubcontractor Analysis CodesShipping Subcontracted SamplesReturning Raw Samples

Production Planning and Control SOP 1.7: Sample Custodian

Production Planning and Control SOP 1.8: Purging and Storing Extracts

Production Planning and Control SOP 1.9: Handling Sample Requests

Production Planning and Control SOP 2.0: The Extraction Worksheet(Sample Custodian)

Production Planning and Control SOP 2.1:

Production Planning and Control SOP 2.2: The Control Clerk

Production Planning and Control SOP 2.3: Worksheet Audit

Production Planning and Control SOP 2.4: Counter Pages

FAC 001 0799


T a b l e O f C o n t e n t s ( C o n t . ) C300975

Production Planning and Control SOP 2.5: Distributing Paperwork

Production Planning and Control SOP 2.6: Auditing The CLMS

Production Planning and Control SOP 2.7: Scheduling RepeatsPaperwork For RepeatsRescheduling Samples In TheCLMS

Production Planning and Control SOP 2.8: Coordinating SamplesIssuing SamplesMonitoring the Progress ofSamples

Handling Repeats

Production Planning and Control SOP 2.9: Document ControlInventorying Sample FoldersStoring DocumentsData Inquiries

Production Planning and Control SOP 3.0: Collection, Packaging & Disposalof Hazardous & D1ox1n WasteHazardous WasteD1ox1n Waste

Production Planning and Control SOP 3.1: pH Checking Procedures for InorganicWater Samples

Quality Assurance SOP 3.1: Initial Documentation For SOPs: IncludingDesignated Personnel Responsibilities

Quality Assurance SOP 3.2: Revision of Standard Operating Procedures

Quality Assurance SOP 3.3: Creation of Standard Operating Procedures

Production Planning and Control Appendix

FAC 001 0800


0300976


Glassware Preparation

CoapuCheoP Laboratories

FAC 001 0801


T a b l e O f C o n t e n t s C300977

Glassware Preparation SOP 1.1: Preventing Laboratory Contamination

Glassware Preparation SOP 1.2: Preparing Plastic Caps, Teflon Discs,and Teflon-Lined Septa

Glassware Preparation SOP 1.3: Preparing SampleSaver® Glassware(Including QC Testing)

Glassware Preparation SOP 1.4: Preparing Glassware For The SamplePreparation Laboratory

Glassware Preparation SOP 1.5: Preparing Glassware For The Inorganics(Metals) Laboratory

Glassware Preparation SOP 1.6: Cleaning Procedure For Sampling Equipment

Quality Assurance SOP 3.1: Initial Documentation for SOPs: IncludingDesignated Personnel Responsibilities



FAC 001 0802


0300978


Sample Preparation Laboratory

CompuCheffl* Laboratories

FAC 001 0803

Appendix CRevision No. 2Date: August 11, 198<Page 9 of 47

T a b l e O f C o n t e n t s C300979Sample Preparation Laboratory SOP 1.1: Calibration of pH Meter; Lab-Bench

Version

Sample Preparation Laboratory SOP 1.2: Distillation of Received AcetoneIn-House; Lab-Bench Version

Sample Preparation Laboratory SOP 1.3: 36/37 Commercial B/N and Add Water;Lab-Bench Version

Sample Preparation Laboratory SOP 1.4: 31/32 Commercial B/N and Acid Water;Low Detection Limit; Lab-BenchVersion

Sample Preparation Laboratory SOP 1.5: 42/43 IBM Poughkeepsie Low Level B/Nand Add Water; Lab-BenchVersion

Sample Preparation Laboratory SOP 1.6: 056 SV Waters New EPA ProtocolLab-Bench Version

Sample Preparation Laooratory SOP 1.7: 137/138 Commercial B/N and Add Soils;Lab-Bench Version

Sample Preparation Laboratory SOP 1.8: Generation of 1:1 Acetone/MethyleneChloride Solvent System; Lab-BenchVersion

Sample Preparation Laboratory SOP 1.9: 717 SV Only; New EPA Caucus LowLevel SV; Lab-Bench Version

Sample Preparation Laboratory SOP 2.0: 717/716 New EPA Caucus Low Level SVand Pesticide Split Incorporating A153 Screen Split; Lab-Bench Version

Sample Preparation Laboratory SOP 2.1: 154 Medium Level SV (New EPA ProtocolFor SV Soils); Lab-Bench Version

Sample Preparation Laboratory SOP 2.2: 157 For PH Measurement According ToNew EPA Caucus Protocol; Lab-BenchVersion

0804

Appendix CRevision No. 2Date: August 11, 198fPage 10 of 47

T a b l e Of C o n t e n t s ( C o n t. ) 0300930

Sample Preparation Laboratory SOP 2.3:

Sample Preparation Laboratory SOP 2.4: Preparation Procedure: 50% Sulfur1cAdd; Lab-Bench Version

Sample Preparation Laboratory SOP 2.5: Preparation Procedure: 504 SodiumHydroxide; Lab-Bench Version

Sample Preparation Laboratory SOP 2.6: Preparation Procedure: Extracted Water;Lab-Bench Version

Sample Preparation Laboratory SOP 2.7: Mixing Raw Samples

Sample Preparation Laboratory SOP 2.8: Resolving Soil Matrix Problems

Sample Preparation Laboratory SOP 2.9: Sample Problem Techniques For Water

Sample Preparation Laboratory SOP 3.0: Preparation of Furnaced Sodium Sulfate

Sample Preparation Laboratory SOP 3.1: Preparation of Laboratory Glasswool




FAC 001 0805


C300981


ForHigh-Hazard Laboratory

CompuChenP Laboratories

FAC 001 0806


C300982

TABLE OF CONTENTS

High-Hazard Laboratory SOP 1.1: Cleanup Procedure: D1ox1n Spills

High-Hazard Laboratory SOP 1.2: Waste Disposal (Laboratory)

FAC 001 0807


C300983


The Inorganics Laboratory


FAC 001 0808


C300984


GC/MS Laboratory


001 0809


I A B L E o r c o H I E H I S C3009S5GC/MS LABORATORY SOP 1.0: HARDWARE COMMANDS

System FunctionsEmergency Shut-OffReset LightLED Failure IndicatorsPower SwitchPageLocation and Use of Other Power Switches

Printer FunctionsPrinter FunctionsTo form feed paperTo change paper 1n the printer

. To set the paper 1n the printer

Disk Drive FunctionsTo turn on the disk driveTo load and unload a disk driveTo remove a diskTo Insert a disk

Computer FunctionsTo boot the system

Nova 3Nova 7Setting the jlme

To Initialize a dllkGC/MS LABORATORY SOP 1.1: SOFTWARE COMMANDS

General ProgramsTo check system statusTo check the status tableTo set scan parameterTo select a MID descriptor (MI and/or MT)To change GC files and parameters

The AC ProgramTo acquire dataTo answer AC prompts

SpectraRaw SpectraEnhanced SpectraDual SpectraScan Averaged Spectra

FAC 001 0810


Mass ListingsRaw Mass ListingsEnhanced Mass Listings C 3 00986List Averaged Mass Listing

Library SearchesRaw Library SearchEnhanced Library SearchScan Averaged Library SearchComparative Library Search and Dual Spectra

Reconstructed Ion Chromatogram (RIC)Full RICPartial RICPartial RIC with Masses

Quant1tat1on of MassesManual Quant1tat1on of Masses

Extracted Ion Current Profile (EICP)

GC/MS LABORATORY SOP 1.2: PROCEDURAL CONVENTIONS

Sequencing a Tune

Naming A FileGC/MS LABORATORY SOP 1.3: PRODUCTION DOCUMENTATION

Reading A Worksheet

Completing A WorksheetCompleting the Run Log

GC/MS LABORATORY SOP 1.4: COMPOUND ADDITIONS

Internal Standards

Surrogates

FAC 001 0811


GC/MS LABORATORY SOP 1.5: LIBRARY CONVENTIONS

Definition of a Library

Building a Library

Changing a Library's Parameters

Changing a Library's Retention Times

Using the Quant Routine RKUsing Linkers and an Eleven-Table with RK

GC/MS LABORATORY SOP 1.6: SAMPLE QUANTITATION

Quant Hating a SampleReading a Quant1tat1on Report

Reproducing a Quant Report

Confirming the Quant Report's ResultsProducing the Dellverables

Contents of a Completed Sample Data Package

GC/MS LABORATORY SOP 1.7: CORRECTIVE ACTIONS

Checking a Standard

Finding an Absent CompoundFinding and Reading Retention Time

Updating a Standard

Using a Multipoint

Contents of a Completed Standards PackageGC/M5 LABORATORY SOP 1.8: INSTRUMENT TUNING

Purpose of DFTPP and BFB

Making the Tuning Compounds Meet

C300987

PAC 001 0812


GC/MS LABORATORY SOP 1.9: INJECTION TECHNIQUE 0300988

Injecting a Compound

Making a Dilution

Making a VOA Blank, Standard, and Sample

Performing Combination for Semi-Volatile Analysis

GC/MS LABORATORY SOP 2.0: COLUMN INSTALLATION

GC/MS LABORATORY SOP 2.1: DOCUMENTING REQUIRED MANUAL SEARCHESAND QUANTIFICATIONS

GC/MS LABORATORY SOP 2.2: MAXIMUM ACCEPTABLE INTERNAL STANDARD AREA FORSEMI-VOLATILE, BASE-NEUTRAL, AND ACID ANALYSES

GC/MS LABORATORY SOP 2.3: DOCUMENTING INSTRUMENT FAILURE

QUALITY ASSURANCE SOP 3.1: INITIAL DOCUMENTATION FOR SOPs: INCLUDINGDESIGNATED PERSONNEL RESPONSIBILITIES

QUALITY ASSURANCE SOP 3.2: REVISION OF STANDARD OPERATING PROCEDURES

QUALITY ASSURANCE SOP 3.3: CREATION OF STANDARD OPERATING PROCEDURES

GLOSSARY/INDEX

FAC 001 0813


C300989


GC Laboratory

ConpuChen Laboratories

FAC 001 0814

T a b l e O f C o n t e n t s


GC Laboratory SOP 1.1: Sample Flow Description C300990

GC Laboratory SOP 1.2: Samples and Standards

GC Laboratory SOP 1.3: In-Lab Sample Preparation

GC Laboratory SOP 1.4: Preparation of Sample Extracts

GC Laboratory SOP 1.5: Summary of GC Parameters

GC Laboratory SOP 1.6: GC Setup

GC Laboratory SOP 1.7: Data Review

GC Laboratory SOP 1.8: Arochlor (PCB) Analysis By GC/ECD

GC Laboratory SOP 1.9: Case Review

GC Laboratory SOP 2.0: File Copy

GC Laboratory SOP 2.1: Writing Sequences

GC Laboratory SOP 2.2: Volatile Organic Analysis Screen With HexadecaneExtract

GC Laboratory SOP 2.3: Treating Samples With Mercury To RemoveSulfur (General Procedure)

GC Laboratory SOP 2.4: Documenting Instrument Failure




001 0815


C300991


Drta Entryand

Report Preparation

CoapuCheo* Laboratories

FAC 001 0816


T a b l e O f C o n t e n t s0300-992

I. Standard Operating Procedures: Data Entry

Data Entry SOP 1.1: Entering StandardsDetermining Standard TypesComputing ChecksumsThe Header PageScreens Two And Three

Data Entry SOP 1.2: Loading QC Surrogate Data For Commercial Fractions(For Volatlles, Adds, and Base-neutrals)

Computing ChecksumsThe Header PageScreens Two And Three

Data Entry SOP 1.3: Loading Sample Data For Commercial PesticideSurrogates

The Header PageScreens Two And Three

Data Entry SOP 1.4: Loading Commercial TCDDsThe Header PageScreens Two And Three

Data Entry SOP 1.5: Loading EPA QC and Production DataComputing ChecksumsThe Header PageScreens Two And Three

Data Entry SOP 1.6: GC/MS Calculation ReportsDatabase Summary ReportsCalibration Data Reports

Data Entry SOP 1.7: Integrating Commercial ReportsReceiving FractionsQuality Control SummariesIntegrating The Commercial Report

Data Entry SOP 1.8: Auditing EPA Sample ReportsEPA Case AuditThe Case NarrativeThe Quality Control SummaryThe Sample Data PackageThe Standards Data PackageRaw QC DataAdministrative Forms

PAC 001 0817


T a b l e O f C o n t e n t s ( C e n t . )

Data Entry Appendix I:

Data Entry Appendix II:

C300993OWA Filenames and Legal PrefixesStandards PrefixesProduction Fraction Prefixes

Standards IDs For Standards Data EntrySemi-volatile StandardsVolatile Standards (Liquid)Volatile Standards (Solid)

II. Standard Operating Procedures: Report Preparation

Report Preparation SOP 1.1

Report Preparation SOP 1.2:



Report Integration SOP 1.5:


Using The MainframeOvervlewLogging OnSelecting From The MenusThe Counter PagePostInterpreting QC Sample InformationGathering QC Sample InformationGenerating The OADS For QC SamplesEntering Volatile Sample SpikesEntering Semi-volatile Sample SpikesEntering Pesticide Sample SpikesEntering Blanks

Preparing Integrated QC ReportsThe Integrated QC PackageThe Matrix Form - For Sample SpikesCompleting The Integrated PackageDocumenting EPA Fraction ReceiptOvervlewLogging In FractionsGenerating The OADS For EPA SamplesNaming Volatile FractionsEntering Semi-volatile FractionsEntering Pesticide FractionsAssembling Integrated PackagesContents of the PackageUpdating The Audit Review Board

PAC 001 0818


T a b l e O f C o n t e n t s ( C o n t . ) C300994





Quality Assurance SOP 3.1:



EPA Surrogate RecordingOverviewGenerating Gather ReportsRecording EPA Surrogate Percent Recoveries

Preparing StandardsSemi-volatile StandardsVolatile StandardsPesticide Standards

Word Processing For Commercial Reports.OverviewThe Fraction Package.Booting The CTP 8000The Cover LetterPrinting on the CPT 8000Report of DataThe Compound ListLibrary SearchesThe Quality Control SummaryThe Asrembled ReportPreparing DellverablesCommercial DellverablesEPA DellverablesInitial Documentation for SOPs: IncludingDesignated Personnel Responsibilities

Revision of Standard Operating ProceduresCreation of Standard Operating Procedures

PAC0819


C300995


D1ox1n Coordination And Reporting

ConpuChea Laboratories

PAC 001 0820


C300996


D1ox1n Coordination and Reporting SOP 1.1: Data Package Preparation(EPA D1ox1n)

D1ox1n Coordination and Reporting SOP 1.2: Posting and Updating the HP-300Dloxln IMS System (EPA Dloxln

D1ox1n Coordination and Reporting SOP 1.3: Preparation of B Report Forms OnHP-150 Personal Computer(EPA D1ox1n)

D1ox1n Coordination and Reporting SOP 1.4: Final Report Preparation(EPA D1ox1n)

D1ox1n Coordination and Reporting SOP 1.5: How to Prepare a Case for Mailing(EPA D1ox1n)

D1ox1n Coordination and Reporting SOP 1.6: Final Report Sequence (EPA D1ox1n)

D1ox1n Coordination and Reporting SOP 1.7: Releasing Samples 1n the System forBilling (EPA D1ox1n)

D1ox1n Coordination and Reporting SOP 1.8: Document Inventory Control SummaryForms (EPA D1ox1n)




FAC 001 0821


0300997


EPA Technical Review

ConpuChenP Laboratories

FAC 001 0822


TABLE OF COKTENTS

Technical Review SOP 1.1:

Reviewing Organic EPA Case Samples


Reviewing Inorganic EPA Case Samples


Conducting EPA Quality Assurance Audits


Documenting Personnel Employment Dates


Initial Documentation for SOPS: IncludingDesignated Personnel Responsibilities

Quality Assurance >OP 3.2:

Revision of Standard Operating Procedures


Creation of Standard Operating Procedures

0300998

FAC 001 0823


EPA Customer Inquiry

ConpuChem* Laboratories


C300000

FAC 001 0824


C301000T a b l e O f C o n t e n t s

EPA Customer Inquiry SOP 1.1: Responding To EPA Customer Inquiries




FAC 001 0825


C301001


Comnerclal Technical Review

CompuCheffl* Laboratories

FAC 001 0826


C301002T a b l e O f C o n t e n t s

Introduction

Technical Review SOP 1.1: Reviewing Silver and Gold ReportsSample RecordData ReportsDocumenting the Technical Review

Technical Review SOP 1.2: Proofreading Final ReportsThe Cover LetterThe Laboratory ChronicleThe Table of ContentsMethod ReferenceCompound ListQuality Control SummaryChain of Custody RecordError ReportThe Proofreading LogThe Dally Production Log




PAC 001 0827


C301003


For

Comerclal Customer Inquiry

CcmpuChen^ Laboratories

001 0828


0301004

TABLE OF CONTENTS

Commercial Customer Inquiry SOP 1.1: Resolving Commercial Customer Inquiries

FAC 001 0829


C301005


Quality Assurance

CompuChen* Laboratories

FAC 001 0830



Quality Assurance SOP 1.1: New Lot Standard Approval SystemAdd Base-Neutral StandardsVolatile StandardsPesticide StandardsDio-Anthracene StandardAc1d/Base-neutral Surrogate StandardAnomalous Compounds

Quality Assurance SOP 1.2: Approval of New Standard Lots Received

Quality Assurance SOP 1.3: Introduction of New Quality Control CounterNumbers

Quality Assurance SOP 1.4: Introduction of Condition CodesQuality Assurance Action

Quality Assurance SOP 1.5: Introduction of Catcodes/Ana lysis Codes

Quality Assurance SOP 1.6: Resolution of Problem Samples

Quality Assurance SOP 1.7: Technical Assistance To MarketingEvaluation of Requests for ProposalsHandling Problem SamplesCustomer Inquiries

Quality Assurance SOP 1.8: Preparation and Use of Quality AssuranceNotices

Quality Assurance SOP 1.9: Resolution of Anomalous Quality AssuranceData

Quality Assurance SOP 2.0: On-S1te Audits

Quality Assurance SOP 2.1: Compiling Quarterly Quality Control Statistics

Quality Assurance SOP 2.2: Technical Data Audit

Quality Assurance SOP 2.3: Quality Control of VOA Bottle Batches

001 0831


0301007T a b l e O f C o n t e n t s (Cont.)

Quality Assurance SOP 2.4: Quality Control of VOA Storage Cabinet

Quality Assurance SOP 2.5: Quality Control of Metals Sample Bottles

Quality Assurance SOP 2.6: VOA Storage Stability Tests

Quality Assurance SOP 2.7: Liter Bottle Preparation Tests

Quality Assurance SOP 2.8: Performance Evaluation Samples

Quality Assurance SOP 2.9: Internal, Blind Quality Control Samples

Quality Assurance SOP 3.0: Test Samples




Quality Assurance SOP 3.4: Subcontractor Requirements

Quality Assurance SOP 3.5: Standards TraceablHty

Quality Assurance SOP's Appendix ICondition CodesFailure Codes For All Production andQuality Control SamplesFinal Codes For Production SamplesFinal Codes For Quality Control SamplesChronicle of Revisions

FAC 001 0832


0301008


For ThePreparation, Analysis and Data Assessment

ofEnvironmental Samples

Prepared by the Staff ofCompuChem Laboratories, Inc.

Approved byRobert E. Melerer, Director of Quality Assurance

Copy Number:Approved For Release By:Issued To:

FAC 001 0833

Appendix CRevision No. 2Date: August 11, 1986 #>**,*«**Page 41 of 47 0301009

5. Metals

a. Sample Preparation Procedure 136 - "Preparation of SolidSamples for the Determination of Metals by Inductively CoupledPlasma (ICP), Flame and Flameless Atomic AbsorptionSpectrophotometry (AAS)."

b. Sample Preparation Procedure 162 - "Preparation of SolidSamples for the Determination of Mercury."

6. Other Parametersa. Sample Preparation Procedure 139 - "Sample Preparation

Procedure for Cyanides 1n So1l/Sed1ment/S1udge."

b. Sample Preparation Procedure 150 - "Sample PreparationProcedure for Phenols 1n So1l/Sed1ment/Sludge."

B. Liquids

1. SemlvolatHes

a. Sample Preparation Procedure 001 - "Preparation of WaterSamples for the Analysis of Add and Base/Neutral Compounds byGC/MS."

b. Sample Preparation Procedure 908 - "Preparation of As-ReceivedAdd and/or Base/Neutral Extracts for Analysis by GC/MS."

c. Sample Preparation Procedure Oil - "Priority PollutantSemlvolatHes, Matrix Spike - Water."

d. Sample Preparation Procedure 020 - "Processing of AqueousSamples to Achelve Lower Than Normal Detection Limits ForSolvent Extractable Organic Compounds (Special Compounds).

e. Sample Preparation Procedure 030 - "Processing of AqueousSamples to Achelve Lower-Than-Normal Detection Limits for Addand B/N Compounds (1 Liter Extraction)."

2. Pest1c1des/PCBs/Herb1c1desa. Sample Preparation Procedure 002 - "Extraction of Water

Samples for Analysis of Pest1c1des/PCBs."b. Sample Preparation Procedure 009 - "Method for Chlorophenoxy

Add Herbicides 1n Drinking Water."

FAC 001 0834


c. Sample Preparation Procedure 402 - "Dilution of 011 Sample forAnalysis of Pestlddes/PCBs."

d. Sample Preparation Procedure 922 - "Preparation of As-ReceivedPesticide Extracts for Analysis by GC."

e. Sample Preparation Procedure 21 - "Preparation of AqueousSamples for the Analysis of Priority Pollutant Pesticides atLower Than Normal Detection Limits."

3. 2,3,7,8-Tetrachlorod1benzo-p-d1ox1n (TCDD)

a. Sample Preparation Procedure 027 - "Preparation of an AqueousSample for the Determination of 2,3,7,8-TCDD."

4. Metals

a. Sample Preparation Procedure 029 - "Preparation of WaterSamples for the Determination of Metals by Inductively CoupledArgon Plasma (ICAP), Flame and Flameless Atomic AbsorptionSectrophotometry (AAS)."

5. Other Parameters

a. Sample Preparation Procedure 060 - "Formaldehyde Determination1n Aqueous Samples."

IV. Instrument Procedures - All Fractions; Solid and Liquid Matrix

A. Fractions; Solid and Liquid Matrix

1. Volatlles

a. Instrument Procedure 205 - "Low Level Solid Volatile Organlcs."

b. Instrument Procedure 201 - "Low or Medium Liquid VolatileOrganlcs."

c. Instrument Procedure 250 - "Low or Medium Liquid VolatileOrganlcs *• Xylenes."

d. Instrument Procedure 705 - "Low or Medium Liquid VolatileOrganlcs + Matrix Spike."

e. Instrument Procedure 703 - "Low or Medium Liquid VolatileOrganlcs + Library Search."

FAC 001 0835

Appendix CRevis ion No. 2 0301011Date: August 11, 1986Page 43 of 47

f. Instrument Procedure 221 - "Low or Medium Liquid VolatileOrganlcs; Library Search Only."

g. Instrument Procedure 260 - "Low Level Solid Volatile Organlcs;Library Search Only."

h. Instrument Procedure 709 - "Low Level Solid Volatile Organlcs+ Library Search."

1. Instrument Procedure 251 - "Low Detection Limit LiquidVolatile Organlcs."

J. Instrument Procedure 712 - "Low Detection Limit LiquidVolatile Organlcs + Library Search."

k. Instrument Procedure 713 - "Low Level Solid Volatile OrganlcsMatrix Spike."

1. Instrument Procedure 251 - "Low Detection Limit LiquidVolatile Organlcs + Xylenes."

m. Instrument Procedure 238 - "Low Level Solid Volatile Organlcs+ Xylenes."

n Instrument Procedure 258 - "Medium Level Solid VolatileOrganlcs (Methanollc Extraction)."

2. SemlvolatHesa. Instrument Procedure 202 - "Solid or Liquid Add Extractables."

b. Instrument Procedure 203 - "Liquid or Solid Base/NeutralExtractables."

c. Instrument Procedure 701 - "Adds; Method 625 & Library Search."

d. Instrument Procedure 702 - "Base/Neutral, Method 625 & LibrarySearch."

e. Instrument Procedure 222 - "20 Peak TentativeIndent1f1cat1on-Ac1d Fraction."

f. Instrument Procedure 223 - "20 Peak Tentative Indent1f1cat1on-Base/Neutral Fraction."

FAC 001 0836


g. Instrument Procedure 252 - "Add Extractables-Lower DetectionLimit."

h. Instrument Procedure 253 - "Base/Neutral Extractables LowerDetection Limit."

1. Instrument Procedure 710 - "Adds - Lower Detection Limits &Library Search."

j. Instrument Procedure 711 - "Base/Neutral - Lower DetectionLimits & Library Search."

k. Instrument Procedure 248 - "TCDD Instrument Procedure."

3. Pest1c1des/PCBs/Herb1ddes

a. Instrument Procedure 101 - "Solid or Liquid Pest1dde/PCBAnalysis."

b. Instrument Procedure 103 - "Solid or Liquid Herbicide Analysis.

c. Instrument Procedure 111 - "As Received Extract Pest1c1de/PCBAnalysis."

4. Metalsa. Instrument Procedure 001 - "Determination of Metals By

Flame/Furance Atomic Absorption Spectrophotometer."

b. Instrument Procedure 005 - "Determination of Mercury 1n LiquidSamples and Dlgestates from So11s/Sed1ments/Sludges (AutomatedCold Vapor Technique)."

c. Instrument Procedure 308 - "Determination of Metals byInductively Coupled Plasma."

5. Other Parametersa. Instrument Procedure 501 - "Determination of Cyanide, Total 1n

Liquid Samples."*b. Instrument Procedure 502 - "Determination of Phenol1cs, Total

Recoverable 1n Liquid Samples."*c. Instrument Procedure 551 - "Spectrophotometrlc Measurement of

Formaldehyde."*App11cab1e for analysis of aqueous distillates from manual distillation ofsolids or liquids.

FAC 001 0837


V. QA/QC Policies

A. QC Assessment-SemlvolatHes, Adds, Base/Neutrals

B. QC Assessment-Volatlles

C. QC Assessment-Pesticides

D. Surrogate Control Limits - Liquids/SolIds

E. Liquid QC Spike Acceptance CriteriaF. Solid QC Spike Acceptance Criteria

G. Metals/Cyan1de/Phenols (Colorlmetrlc) QC Acceptance Criteria

H. Holding Time Requirements

I. Compound Lists

J. Surrogate Standards

K. Internal Standards

Appendix CRevision No. 2 0301014Date: August 11, 1986 «*•«!«Page 46 of 47

TABLE OF CONTENTS

I. Sample Preparation and Instrument Procedures for Soils and Sediments byEPA-CLP Protocols (Organlcs).

1. Screen Preparation, VOA; S/S; Hexadecane (-158)..................... 12. Screen Analysis, VOA; GC/FID (112)..................................103. Extraction; S/S; L.L. Screen; EPA Caucus (-153J.....................134. GC Screen; S/S; L.L. S-V; EPA Caucus (122)..........................205. Low Level VOA Prep; S/S; EPA Caucus (-155)..........................216. GC/MS; S/S; Low Level VOA; EPA Caucus (257).........................237. VOA Solid QC Dellverables (Not An IPP or SPP)8. Ext Prep; S/S; Low Lev. S-Vs; EPA Caucus (-717).....................259. GC/MS; S/S; Low Lev. S-Vs; EPA Caucus (255).........................3010. Sem1-Vol. Solid Dellverables (Not An IPP or SPP)11. Ext. Prep.; S/S; L.L. Pest/PCBs; EPA Caucus (-716)..................1312. GC; S/S; L.L. Pest/PCBs; EPA Caucus (124)...........................3513. Pesticides Pending; S/S (Not An IPP or SPP)14. Pest Sol. Low Lev. QC Deliver (Not An IPP or SPP)15. pH Determination of Soils (-157)....................................3916. Dry Weight Determination; S/S/S (-143)..............................41

II. Sample Preparation and Instrument Procedure for Waters by EPA-CLPProtocols (Organlcs).

1. Screen Prep.; VOA; Water; Hexadecane (-57)..........................422. Screen Analysis; VOA; GC/FID (112)..................................453. Extraction; Water; A+B/N; EPA Caucus (-56)..........................484. GC/MS; Water, Semi-Volatile; EPA Caucus (254).......................535. Sem1-Volat1les Reported (Not An IPP or SPP)6. Extraction; Water; Pest/PCBs; EPA Caucus (-55)......................587. GC; Pest/PCBs; Water; EPA Caucus (123)..............................638. Pesticides Pending; Water (Not An IPP or SPP)9. Pesticides Reported (Not An IPP or SPP)10. GC/MS; Water; Low Level VOA; EPA Caucus (256).......................6711. VOA Reported (Not An IPP or SPP)

III. Sample Preparation and Instrument Procedures for Inorganics by EPA-CLPProtocols.1. Metal Preparation-Water (-29).......................................692. Metal Analys1s-L1q-ICAP (308).......................................71

FAC 001 0839


TABLE OF CONTENTS (Cont.)

3. Metal Analys1s-L1q-Flame1ess AAS (1)................................804. Metal Preparation-Water (-29).......................................865. Metal Analys1s-L1q-ICP (308)........................................886. Metal Analys1s-L1q-Flameless AAS (1)................................977. Cyan1de-Techn1con-L1qu1d (501).....................................1038. Metal Preparation-Solid (-136).....................................1099. Metal Analys1s-Sol-ICAP (308)......................................11110. Metal Analys1s-Sol-Flameless AAS (D...............................12011. Solid Prep-Cyanide (-139)..........................................12612. Cyan1de-Techn1con Solid (501)......................................12913. Dry Weight Determination; S/S/S (-143).............................13514. Metal Preparation-Solid (-136).....................................13615. Metal Analys1s-Sol-ICAP (308)......................................13816. Metal Analys1s-Sol-Flameless AAS (D...............................14717. Dry Weight Determination; S/S/S (-143).............................153

IV. Sample Preparation and Instrument Procedures for 2,3,7,8 TCDD.1. EPA High Hazard TCDD Prep (-135)...................................1542. Solid TCDD Full Analysis, GC/MS (248)...... .......................1633. L1q Prep. For TCDD Commercial (-27)................................1764. TCDD Anal.-L1qu1d-GC/MS-Commerdal (248)...........................181

FAC 001 0840

Appendix D C 301016Revision No. 2Date: August 11, 1986Page 1 of 12

APPENDIX D

CONDITION CODES

FAC 001 0841

Appendix DRevision No. 2Date: August 11, 1986Page 2 of 12

Appendix D

Condition Codes

CompuChem* Laboratories uses condition codes to signify either

the cause of a sample fraction's failure or the final status of a sample beforerelease (see page 4). The "comments" here describe the consequences of a con-

dition code, the type of analysis for which the code applies, and/or specialInstructions for using the code. These codes are entered 1n the Computerized

Laboratory Management System (CLMS) under the "COND" column of the "Sample

Detail" database and govern the release of the report to the client.

This code 11st 1s divided Into three sections. The first group of codes are

"failure" codes; they apply to all samples repeated because certain criteria

have not been met. The codes appear 1n the Prior (P) slots of the Sample

Detail. The next group of codes are "Final" codes used for production samplesthat have met criteria and may be reported to the client: reports for samples

having these condition codes may or may not Include the standard Quality

Assurance Notices supplied to each laboratory station. The third group of codes

are for Quality Control samples: part A 1s composed of codes also used for pro-

duction samples; part B lists codes that apply to quality control samples only.

This final 11st covers Quality Control data that do not meet all Quality Controlcriteria but are "salvageable" by Quality Assurance 1f the associated productionsamples are not affected. Codes from groups II and III appear exclusively 1nthe final (F) slots of the Sample Detail.

At the end of this section 1s a chronicle of the changes In the Condition

Codes over the last year. It 1s critical to the laboratory system that only themost recently revised 11st be used 1n each department. This chronicle also ser-

FAC 001 0842

C301018.Date: August 11, 1986Page 3 of 12

ves to resolve misinterpretations and misuses of the codes and to explain theapplications of the codes further.

The Individual laboratory stations are responsible for assigning codes to

all Issued paperwork, even 1f no Injection 1s made. As well, every scheduling

detail must have an assigned Condition Code. Any questions concerning ConditionCodes are addressed to the Senior Quality Assurance Analyst, who monitors the

codes periodically to ensure correct application and to pinpoint problem

trends for management.


^301019

CODES COMMENTS

I. FAILURE CODES FOR ALL PRODUCTION AND QUALITY CONTROL SAMPLES

AH * add surrogates high

AL * add surrogates low

BB = bad associated blank

BF » blank requires florlsll cleanup

BH * base/neutral surrogates highBL * base/neutral surrogates low

BS * bad associated spike

BU « back-up extract; screenedmed1 urn

CA » cancelled

CL « needs secondary cleanup

CO * concentration requiredCS » carryover suspected from

previous analysisCT » contamination suspected

DI « requires dilution

DW « wrong dilution used

Verify vial volume and I.S. areas.Use only when not a chromatography relatedproblem (PC).

Use for samples which are not analyzedbecause associated with a bad blank—seechronicle

Used when associated pesticides florl-sllledSee AH codeSee AL code

Use for samples reprepared due to badassociated sample spikeExtracted low level, but not run ,

Applies to all samples (Including QualityControl's) cancelled and never analyzed(fill out form)

TCDDs needing alumina cleanup

V1a1 volume above markRelnject If rest of data 1s acceptable--see chronicleApplies only to effected samples 1n whichcontamination 1s verified

GC/MS usually dilutes sample but may wantsample reextracted using less raw sampleLab must rerun at correct dilution

FAC 001 0844


C301020

ED * extract went to dryness

FH « 2-fluorophenol high only

FL « 2-fluorophenol low only

FO • foamed during purging

IF « Instrument failure; data lostIH * Internal standard(s) high

IL » Internal standard(s) low

IM « Internal standard(s) missing

IR * 1on ratios outside range

IU « wrong InstrumentJS * relnjectlon matches previous

analysisLA « lab accident; sample data lost

LS * screened low, but really highlevel

Usually reextract

Must re-extract unless I.S. problem

Same as above; verify all areasVGA's, reprep at dilution, repurge

Describe failure 1n commentsRelnject unless I.S. solution added; alsosee IL

If extract standard not appropriate,relnject or reextract

Solution not added during preparationTCDDs

Injected on wrong OWA - relnjectUse 1f data falls for same reason; seechronicleDescribe LA 1n comments section

GC/MS run Indicates medium level

MS = screened med, but really clean GC/MS results Indicate low level

NM « no match to prior run orduplicate

OT « other

Applies to appearance of sample extractsor RICs, not t recoveriesDescribe failure 1n comments

FAC 001 0845


0301021

OW » wrong original used forQuality Control sample

PC * poor chromatography

RI « recovery Indeterminate

RN » re-analyzed neat; was rundiluted

RO * s1gnal-to-no1se ratio out

RU * repeated unnecessarily

SF * Spike recoveries failed

SH * Surrogate(s) uniformly high

SI * Spiked InadvertentlySL « Surrogate(s) uniformly low

SM « surrogate or spike standardmissing

SW * Wrong standard(s) used

UP » unacceptable precision betweenQCs

VC « purge vessel crackedVR * verify results

Automatic re-extraction

Perform maintenance 1f necessaryTCDOs

Used for relatively clean RIC

TCDDs

An acceptable prior run exists; seeChronicle

See SOPs for approval criteria

See AH, AL codes and chronicle

Automatic reextractlon

See AH, AL codes and chronicle

Solution not added Inadvertently

Usually automatic reextractlon

For comparing SSs or Duplicates(RPDs between spikes, hits, surrs.)

VOAs' reprep sample and repurgeSample repeated to verify hits, etc.

001 0846


II. FINAL CODES FOR PRODUCTION SAMPLES: DATA TO BE REPORTED

DA « dilution acceptable Sample required reanalysls as a dilution;criteria met/qualified

EA"« reextractlon data acceptable For sample reextracted at least once,even 1f also relnjected

EB°* reextractlon data blllable Recovery 1s within +/- 51 of the fallingsurrogate's recovery

ES°* reextractlon same as prior QAN required; "matrix" effects confirmed;extraction all data comparable

JA°* relnject data acceptable For sample only extracted once and reln-jected successfully

NS « no sample left for reextractlon QAN required; lab responsible for deter-mining del1verab1!1ty of data

OK°* data acceptable first time Never use for repeat status; first In-through jectlon acceptable as 1s

RP * reportable prior run Edit failure code to RP 1f run 1sreportable; (see Chronicle)

III. FINAL CODES FOR QUALITY CONTROL SAMPLES*

Quality Controls that meet criteria or require laboratory-supplied qualifier:

AN * quality control acceptable but Blanks and blank spikes tripped by systemnot reported and run but not needed

CA » quality control cancelled and All samples (Includes Quality Controls)not reported cancelled and never analyzed (fill out

form)

DA « dilution acceptable Quality Control required rerun asdilution; criteria met/qualified by lab

EAe» reextractlon data acceptable For Quality Control sample reextracted;all criteria met/qualified by lab

•These are the codes for runs which have valid surrogate data to be entered Intothe system and used for updating surrogate control limits.*These are the only codes that will allow associated production samples to"blast" Into Phase II. All other codes will hold samples 1n Phase I.

FAC 001 0847


C301023

EB°« reextractlon data b1lTable

JA°« relnjectlon data acceptable

OK°« data acceptable first timethrough

RP « reportable prior run

UN « Quality Control unacceptablebut not used

Recovery 1s within +/- 54 of the fallingsurrogate's recoveryQuality Control relnjected; all criteriamet/qualified by labFirst Injection of first Quality Controlextract; met/qualified by labEdit failure code to RP 1f run 1sreportable; see Chronicle

Blanks and blank spikes tripped and runbut not needed (See AN code)

Quality Controls that don't meet criteria and/or require special QualityAssurance Intervention (Quality Assurance approval or Quality Assurancesupplied qualifier) for production sample release:

DQ * Quality Control requireddilution and qualified

EQ « Quality Control reextractedand qualified

JQ » Quality Control re Injected andqualified

NQ * No sample left for reextractlonof Quality Control

OQ z Quality Control 1s OK andqualified

Not acceptable unless Quality Assuranceapproves or Inserts special NoticeNot acceptable unless Quality Assuranceapproves or Inserts special NoticeNot acceptable unless Quality Assuranceapproves or Inserts special NoticeNot acceptable unless Quality Assuranceapproves or Inserts special NoticeNot acceptable unless Quality Assuranceapproves or Inserts special Notice(see Chronicle)

•These are the codes for runs which have valid surrogate data to be entered Intothe sysem and used for updating surrogate control limits.*These are the only codes that will allow associated production samples to"blast" Into Phase II. All other codes will hold samples 1n Phase I.

FAC 001 0848


BW « (Bob WhUehead's area). Was used for tracking purposes,but will have QA Queue now.

GB * (Lab Go-Back). Used for tracking, but obsolete.Codes added to 11st —

EQ « needed to qualify Quality Control data that didn't meetall criteria, but couldn't or shouldn't be repeated.

DQ * same as above.JQ * same as above.

AN/UN « breakdown of old NR code; needed to determine how oftenQuality Control samples are run unnecessarily and whetheror not they passed.

CA * same as above, but for those Quality Controls never run;must complete a System Cancellation Form and submit toScheduling and Control.

RU » needed to track repeat request errors and repeats notactually needed.

SE « for semlvolatlle and volatile screens which were notcovered 1n old contract.

TH/TL/EL/EH « New Caucus surrogates which are no longer advisory.

Changes/clarifications of existing codes --JS « cannot be used as an acceptable final code; always must

be used to Imply repeat 1s necessary. For example, 1freinserting to see 1f peaks are result of carryover, andre Inject looks exactly the same, use JA or JQ codes, notJS (even though results are the "same").

DA « when applying to pesticide data, only use for thosesamples that require rerun as dilution.

BB » use only for samples (not blanks) associated with, andnever run because of, a bad blank.

CT « use for contaminated blanks that affect whole batches, orsamples that were Individually contaminated when theblanks were acceptable; also, when verifying carryover 1nblanks by relnjectlng, and the peaks are actually foundto be contaminants present 1n the extract, change priorCS code to CT.

PAC 001 0849

8.. 2 C30I°25Date: August 11, 1986Page 11 of 12

CS « use only when carryover has been verified by relnjectlon(see CT code above).

NS • Individual lab stations are now responsible for deter-mining the validity and Mdel1verab1l1ty" of any existingdata; a Quality Assurance Notice must be Inserted by thelab.

NM * use the UP code when RPD values fall, and the NM codewhen the posslbllty exists that 1) different samples wereused to prepare duplicates; or 2) the repeat of a priorextraction/preparation may have been prepared from a dif-ferent sample.

SH/SL * applies also to pesticides and herbicides now, Instead ofthe DL code, which was redundant.

Revised 3-28-85:

Code deleted from system —

SE * screen error; this code now subdivided Into several morespecific codes

Codes added to system —

BU = backup sample; the sample was extracted low level, but 1snot needed at this time because screen Indicates MediumLevel. This code 1s needed for the Low Level extractionqueue.

FS « screen failure; the blank or blank/spike 1n the batchscreened Medium Level, or the original used for spikesscreened Medium and spikes must be reextracted as aresult.

IW » sample or blank Injected on wrong Instrument and must bereInjected.

LS « screened low, but GC/MS results Indicated Medium Level 1smore appropriate.

MS « screened Medium, but GC/MS results Indicated Low Level 1smore appropriate.

OQ « Quality Control 1s OK (first attempt), but needs to bequalified with Quality Assurance Notice or needs QualityAssurance approval.

FAC 001 0850

/ Appendix DI Revision No. 2

Date: August 11, 1986, Page 12 of 12\

RA * RIC appearance 1s unacceptable; pertains usually to highbaseline, large solvent peaks, etc.

Revised 5-14-85:Codes added to system --

BS « used when the sample sp1ke{s) and blank spike failed; the" entire batch 1s reextracted and all associated samples

get the BS code; the spikes are assigned the normalfailure code.

EB « reextractlon results Pass, but one or more surrogaterecoveries are within +/- 5% from the falling surrogate's

, recovery (same as ES, but data passes).

NF * the final Injection 1s not the one being reported; for aprevious run which 1s later found to pass or 1s quali-fied so 1t can be reported; this code will appear 1n a"P" slot, even though 1t was run last.

RP = reportable previous Injection; used 1n conjunction withNF; the failure code once assigned to this run must beedited to RP on the paperwork and 1n system. This willbe the code appearing 1n the "F" slot.

Revised 1-9-86:Codes added to system -

VR * used when sample repeated to verify hits or peaks found1n run (particularly for pesticide confirm).

OM * original screened medium, QC needs to be repeated.OL « original screened low, QC needs to be repeated.

RB « report both runs; use when EPA blank 1s run on two dif-ferent Instruments but both runs are reportable.

Codes deleted from system —DH • obsoleteEH,EL,PH,PL,Th,TL,NH,NL,YH,YL - specific surrogate failures

will be tracked using recovery QUIZ reports. Just useSL.SH.AL.AH.BL.BH codes for surr. failures.

FS « OM and OL will be used 1n most cases.NF - will use VR Instead; this 1s a prior code even though Its

the final run.RA « obsolete, most should be PC 1n most cases.

FAC 001 0851

030102?

APPENDIX E

Chaln-of-Custody

FAC 001 0852

Section: Appendix ERevision No. 2Date: October 3, 1988Page! of 2 0301028

Cha1n-of-Custody

The basic components for maintaining sample cha1n-of-custody (C-O-C) are:1) samples must be relinquished Into the possession of an authorized laboratory

staff member, or

2) samples must be within the authorized staff member's I1ne-of-s1ght, or3) samples must be locked 1n a secured storage area with restricted access.

Furthermore, any change of possession or custody must be documented on

appropriate cha1n-of-custody forms. This documentation must Include both the

Initials of the Individual relinquishing the sample and those of the Individualreceiving the sample, as well as the date of the custody transfer.

CompuChenr* accomplishes these objectives through an elaborate document controlsystem. This system Includes procedures for documentation of the receipt of the

sample Into the laboratory using preprinted, numbered cha1n-of-custody records

(although many clients provide their own C-O-C records which suffice). These

records Include Information about the Individuals collecting the samples, thecollection date, time and location, and the type of analyses required.CompuChem's clients are responsible for field cha1n-of-custody, samplecollection, handling and shipping.

When the samples are received 1n the laboratory, the C-O-C documents are signed

and dated by the Receiving Clerk. The samples are logged Into the ComputerizedLaboratory Management System (CLMS), and assigned unique sample Identificationnumbers. The samples are then relinquished to the possession of a SampleCustodian, who has sole access to the locked sample storage refrigerators. The

CLMS schedules the appropriate analyses and tracks the progress of sample

001 0853

C301029

APPENDIX F

Drinking Water Requirements

FAC 001 0854

Appendix DRevision No. 0Date: November 16, 1987Page 1 of 4

APPENDIX F 0301030

Drinking Water Requirements

Samples Identified by the client as "Drinking Water Samples" (I.e., fordrinking water compliance monitoring) require certain special handling andreporting procedures, but are otherwise handled by the Computerized LaboratoryManagement System (CLMS) 1n much the same way as non-compllance samples.The Sales Representatives 1n the Marketing Department are responsible forplacing the order 1n the CLMS, ensuring that the appropriate analysis codes arechosen. Only analysis codes describing EPA-approved drinking water methods maybe used. The tables on the following pages Identify the particularmethodologies utilized 1n processing drinking water samples.For compliance monitoring 1n North Carolina, following the "Rules GoverningPublic Water Supplies" (amended February 1, 1987), all certified commerciallaboratories are required to report results of analyses to both the Public WaterSupply Branch and the supplier of water (client). The rules specify theparticular reporting forms to be used and the time period 1n which reports areto be submitted.

In evaluating drinking water sample data, the QC criteria applied are asspecified 1n the referenced method. Where unspecified, CompuChem* employs thosecriteria outlined 1n the Federal Register (October 26, 1984 600-ser1es methods)for "Water and Wastewater", presented 1n Section 9.5 of the QA Plan. Once adatabase of sufficient size 1s generated, control limits for precision andaccuracy will be generated based on historical data for aqueous sample analyses.In order to continue providing analytical services for compliance monitoring,CompuChem* must maintain certification through the various drinking/potablewater certifying agencies. The North Carolina Department of Human Resources(NCDHR), Division of Health Services, regulates certifications, performanceevaluations and annual on-s1te laboratory Inspections for these services 1nNorth Carolina. CompuChem* also maintains drinking water certifications 1n anumber of other states, many of which accept reciprocal certification throughthe NCDHR.

001

Appendix FRevision No. 0Date: November 16,Page 2 of 4

C3010311987

METHODS USED BY COMPUCHEM*FOR POTABLE WATER ANALYSIS

Volatile Organic Contam1nants/THMSBromobenzeneBromochloromethaneBromdlchloromethaneBromoformBromomethanesec-Butylbenzenetert-ButylbenzeneCarbon tetrachlorldeChlorobenzeneChlorodlbromethaneChloroethaneChloroformChloromethaneo-Chlorotoluenep-Chlorotoluene1,2-D1bromo3-ChloropropaneDlbromethaneo-D1chlorobenzenem-Dlchlorobenzenep-D1chlorobenzeneD1chlorod1fluoromethane1.1-Dlchloroethane1.2-D1chloroethane1.1-Dlchloroethyleneds-1,2-D1chloroethylenetrans-1,2-D1chloroethy1eneDlchloromethane1.2-Dlchloropropane1.3-D1ch1oropropane2,2-D1chloropropanel,l-D1chloropropane1,3-D1chloropropaneEthylbenzeneEthylened1brom1deFlurotrlchloromethaneHexachlorobutad1eneIsopropylbenzene

Method Used *524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1504,524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1504,524.1524.1524.1524.1

* MMethods for the Determination of Organic Compounds 1n Finished DrinkingWater and Raw Source Water", September, 1986, EMSL-CI, U.S.EPACincinnati, Ohio 45268.

FAC 001 0856

Appendix FRevision No. 0Date: November 16,Page 3 of 4

C301032

1987

METHODS USED BY COMPUCHEM*FOR POTABLE WATER ANALYSIS

(continued)

Volatile Organic Contam1nants/THMS

n-PropylbenzeneStyrene1,1,1,2-Tetrachloroethane1,1,2,2-TetrachloroethaneTetrachloroethylene1,1,1,-THch loroethaneTrlchloroethyleneToluene1,1,2-Trlchloroethane.1,2,3-TrlchloropropaneVinyl chlorideo-Xylenem-Xylenep-XyleneChlorodanePolychlorlnated Blphenyls

Method Used *

1

524.1524.1524524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1524.1608608

Inorganic Contaminants

IronManganeseArsenicBariumCadmiumChromiumFluorldeLeadMercuryPHSeleniumSilverSodium

Method Used **

270,272,

236.2243.2206.2208.2213.2218.2340.2239.245150.1

273.2

* "Methods for the Determination of Organic Compounds 1n Finished DrinkingWater and Raw Source Water", September, 1986, EMSL-CI, U.S.ERACincinnati, Ohio 45268.

** "Methods for Chemical Analysis of Water and Wastes," EPA EnvironmentalMonitoring and Support Laboratory, Cincinnati, Ohio, 45268(EPA-600/4-79-020), March 1979. Available from ORD Publications, CERI,EPA, Cincinnati, Ohio 45268. For approved analytical procedures formetals, the technique applicable to total metals must be used.

FAC 001 0857

Revision No. 0Date: November 16, 1987Page 4 of 4

APPROVED METHODOLOGY FORORGANIC CONTAMINANTS

Additional Organic Contaminants Method Used

Chlorinated Hydrocarbons 1Endrln 1Llndane 1Methoxychlor 1Toxaphene 1

Chlorophenoxy, Adds 22,4,-D 22,4,5-T 2

'Methods for Organochlorlne Pesticides and Chlorophenoxy Add Herbicides 1nDrinking Water and Raw Source Water," Available from ORD Publications,CERI, EPA, Cincinnati, Ohio 45268. (pp. 1-19)

Ibid. (pp. 20-35)

FAC 001

C30102I

APPENDIX G

Subcontracted Services

FAC 001 0859

030103.Section: Appendix GRevision No. 0Date: October 3, 1988Page 1 of 1

Subcontracted Services

Subcontracted services are regulated to comply with the requirements of the

Quality Assurance Program. The Marketing Department establishes, with Inputfrom the laboratory, when subcontract requirements are needed. The QA

Department verifies that the subcontractor complies with the methods written 1ntheir referenced SOPs and with their own QA Plan requirements. This 1s

accomplished by an on-site Inspection of the subcontractor facility. The same

criteria and objectives used during an Internal Systems Audit are used for the

subcontractor audit. Prior to the approval of a laboratory for Its analyticalservices, blind PE samples are submitted and must be successfully completed as

part of their performance audit.

The Director of QA has final authority ove^ the approval of all subcontractor

services. The documentation of subcontractor certification 1s maintained 1n QA

Department files and is made available to clients upon request. Subcontractorsare not used when specifically restricted by a client's QAPP, statement-of-work,or contract, and clients are notified whenever a subcontractor 1s to provide

analytical services.

°°1 0860