Remedial Investigation/Feasibility Study FINAL …final reports. - Technical review of analytical...

I (Remedial Investigation/Feasibility Study

FINAL QUALITYASSURANCE PROJECT

PLANAddendum to Attachment 5

(Quality Assurance Manual/Laboratory Analytical Methods)To Approved November 1990 QAPP

OCCIDENTAL CHEMICAL CORPORATIONPottstown, Pennsylvania

January 1991

BCMEngineers, Planners, Scientists

and Laboratory Services

DLI DLT

DinCT3

BCM Laboratory Effective Date: 7/2/90QA Program Plan Superceded Date: NEW

QUALITY ASSURANCE PROGRAM PLAN

BCM LABORATORY

NORRISTOWN, PENNSYLVANIA

Approved By: Prepared By:Reviewed By:

Technical Director Date Quality Assurance Manager /Date(

Laboratory Director Dae

BH30U72

ATTACHMENT 5 ADDENDUM

QUALITY ASSURANCEMANUAL/LABORATORY ANALYTICAL METHODS

NOTE: This document provides the Quality Assurance Manualand Laboratory Analytical Methods for BCM Laboratories.This Attachment 5 1s presented as an Addendum to the QAPPoriginally submitted and approved, dated November 1990.That original submlttal Included only the Quality AssuranceManual and Laboratory Analytical Methods for the RadianCorporation Laboratory.

BCM Laboratory QA Program Plan Effective Date: 7/2/90Superceded Date: NEW

TABLE OF CONTENTS

OVERVIEW . . . . . . . . . . . . . . . . . . . . . . . . . . . Section 1

STAFF ORGANIZATION AND RESPONSIBILITIES. . . . . . . . . . . . Section 2

HEALTH AND SAFETY. . . . . . . . . . . . . . . . . . . . . . . Section 3

QUALITY CONTROL. . . . . . . . . . . . . . . . . . . . . . . . Section 4

TRAINING AND STANDARDIZATION . . . . . . . . . . . . . . . . . Section 5

QUALITY ASSURANCE AUDITS . . . . . . . . . . . . . . . . . . . Section 6

STANDARD OPERATIONG PROCEDURES . . . . . . . . . . . . . . . . Section 7

DOCUMENT CONTROL . . . . . . . . . . . . . . . . . . . . . . . Section 8

SAMPLE CUSTODY, SAMPLING & SAMPLE TRACKING . . . . . . . . . . Section 9

USING QUALITY CONTROL IN THE LABORATORY. . . . . . . . . . . . Section 10

DATA QUALITY CALCULATIONS. . . . . . . . . . . . . . . . . . . Section 11

DATA REDUCTION & REPORTING . . . . . . . . . . . . . . . . . . Section 12

PREVENTIVE MAINTENANCE . . . . . . . . . . . . . . . . . . . . Section 13

CORRECTIVE ACTION. . . . . . . . . . . . . . . . . . . . . . . Section 14

SOP/EPA METHOD REFERENCES LISTING. . . . . . . . . . . . . . . Section 15

REFERENCES . . . . . . . . . . . . . . . . . . . . . . . . . . Section 16

PROFESSIONAL PROFILES OF LABORATORY PERSONNEL. . . . . . . . . Section 17

SOP METHOD: EXTRACTION FOR CLP SEMIVOLATILE ANALYSIS. . . . . Section 18

SOP METHOD: CLP SEMIVOLATILE ANALYSIS . . . . . . . . . . . . Section 19

SOP METHOD: EXTRACTION FOR CLP PESTICIDES/PCB'S ANALYSIS. . . Section 20

SOP METHOD: CLP PESTICIDES/PCB'S ANALYSIS . . . . . . . . . . Section 21

BCM Laboratory QA Program Plan Effective Date: 7/2/90Superceded Date: NEW

TABLE OF CONTENTS (Continued)

SOP METHOD: TOTAL DISSOLVED SOLIDS (TDS). . . . . . . . . . . Section 22

SOP METHOD: CHEMICAL OXYGEN DEMAND. . . . . . . . . . . . . . Section 23

SOP METHOD: TOTAL SUSPENDED SOLIDS. . . . . . . . . . . . . . Section 24

SOP METHOD: REACTIVITY. . . . . . . . . . . . . . . . . . . . Section 25

SOP METHOD: IGNITABILITY/FLASHPOINT . . . . . . . . . . . . . Section 26

SOP METHOD: TOTAL CYANIDE (COLORIMETRIC, AUTOMATED UV). . . . Section 27

SOP METHOD: TOTAL CYANIDE (DISTILLATION). . . . . . . . . . . Section 28

SOP METHOD: AQUEOUS SAMPLE PREPARATION FOR METALSANALYSIS BY GRAPHITE FURNACE. . . . . . . . . . . Section 29

SOP METHOD: AQUEOUS SAMPLE PREPARATION FOR METALSANALYSIS BY FLAME OR ICP SPECTORSCOPY . . . . . . Section 30

SOP METHOD: SOLID OR SEMI-SOLID SAMPLE PREPARATIONFOR METALS ANALYSIS BY GRAPHITE FURNACE . . . . . Section 31

SOP METHOD: GRAPHITE FURNACE ATOMIC ABSORPTION(GFAA) USING ZEEMAN CORRECTION. . . . . . . . . . Section 32

SOP METHOD: SOLID OR SEMI-SOLID PREPARATION FOR METALSANALYSIS BY FLAME OR ICP SPECTROSCOPY . . . . . . Section 33

SOP METHOD: MERCURY ANALYSIS FROM SOLID AND SEMI-SOLIDSAMPLE MATRICES . . . . . . . . . . . . . . . . . Section 34

SOP METHOD: MERCURY ANALYSIS FROM AQUEOUS SAMPLE MATRIX . . . Section 35

SOP METHOD: DETERMINATION OF PURGEABLE HALOCARBONSBY GAS CHROMATOGRAPHY . . . . . . . . . . . . . . Section 36

SOP METHOD: DETERMINATION OF PURGEABLE AROMATICS BYGAS CHROMATOGRAPHY. . . . . . . . . . . . . . . . Section 37

SOP METHOD: CLP VOLATILE ANALYSIS . . . . . . . . . . . . . . Section 38

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BCM Laboratory QA Program Plan Page 1 of 3Section 1: Overview Effective Date: 7/90

Superceded Date: NEW

1.0 Overview

1.1 Purpose

The purpose of this Quality Assurance Program Plan is to describeand provide a management mechanism for controlling and evaluatingthe the process of gathering and validating analytical data on aroutine basis. This comprehensive program is used by the BCM

Laboratory Division for its analytical services.

1.2 Objectives

The objectives of the program are to ensure, document, and assessdata quality. The program achieves these objectives through

three distinct, interrelated functions:

1) Providing quality control protocols used to determineprecision and accuracy.

2) Controlling data quality within acceptable limits, and

3) Auditing all laboratory functions.

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BCM Laboratory QA Program Plan Page 2 of 3Section l: Overview Effective Date: 7/90


This plan mandates the adherence to the laboratory's StandardOperating Procedures (SOPs) which are based on methods published

by the U.S. Environmental Protection Agency and other authoritiesand describes the quality control procedures to be used with

them. It is not a manual of standard operating procedures.Rather, it describes the general approach used by BCM to ensurethat the objectives of its QA/QC program are met.

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BCM Laboratory QA Program Plan Page 3 of 3

Section l: Overview Effective Date: 7/90Superceded Date: NEW

1.3 Major Components of the QA Process

The major components of this program are designed to provideguidance to the laboratory in all aspects of operation. Thosecomponents are as follows:

- QA/QC acceptance/rejection criteria

- Standard Operating Procedures- Technical Training/Seminar Program

- Document Generation and Control

- Sample Custody and Control- Data Reduction and Reporting .

- Quality Assurance Audits

- Corrective Action Procedures

- Data Quality Calculations- Performance Evaluation Audits

- Health and Safety

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Section 2: Staff Organization Effective Date: 7/90and Responsibilities Superceded Date: NEW

2.0 Organization and Responsibilities

Section 2.1 summarizes the responsibilities of key managementstaff.

2.1 Management Staff and Responsibilities

Laboratory Director

The director administers and oversees laboratory servicesprovided to industrial, municipal, and commercial clients, andstate and federal environmental agencies. The Director ensures

that the laboratory's Quality Assurance Process couples

production goals with a high quality product and service.

BCM Laboratory QA Program Plan Page 2 of 11Section 2: Staff Organization Effective Date: 7/90

and Responsibilities Superceded Date: NEW

Technical Director

The Technical Director oversees all laboratory analyses,providing technical support and guidance. He coordinates incomingprojects, assesses laboratory capabilities, and acts as technicalliason between the laboratory and project engineers.

Responsibilities also include:

- Developing and overseeing technical training/seminar program

- Review and approval corrective action plans, progress andfinal reports.

- Technical review of analytical SOPs

- Direction of the laboratory's Quality Assurance department.Ensures that laboratory analytical departments conform toto QA/QC requirements.

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Director of Organic Operations

The Director of Organic Operations oversees all organiclaboratory operations and environmental testing, which include

GC, HPLC and GC/MS analyses of water, soil, sludge, and wastesamples. Responsibilities include:

- Scheduling technical training/seminars

- Development,implementation and documentation of corrective

actions

- Technical and operational review of analytical SOPs

- Maintaining thorough technical review of data and conformance

to QA/QC requirements

- Maintaining proper documentation/document control program

- Coordination of analyses and projects

- Maintaining strong lines of communication between thelaboratory's Quality Assurance department and all organiclaboratories.

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Director of Inorganic Operations

The Director of Inorganic Operations oversees all inorganic andAsbestos laboratory operations and environmental testing, whichinclude analysis of water, soil, sludge, asbestos-bearingmaterials, and waste samples.Responsibilities include:

- Scheduling technical training/seminars

- Development,implementation and documentation of correctiveactions

- Technical and operational review of analytical SOPs

- Maintaining thorough technical review of data and conformanceto QA/QC requirements

- Maintaining proper documentation/document control program

- Coordination of analyses/projects

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- Maintaining strong lines of communication between thelaboratory's Quality Assurance department and all inorganicdepartment laboratories.

Manager of Laboratory Quality Assurance

Pro-actively acts as a support resource to lab managementproviding help and guidance on an as needed basis to assist labmanagers and supervisors to implement and conform to QCrequirements.

The Laboratory Quality Assurance Manager is responsible for theimplementation of the laboratory's Quality Assurance program. Hisresponsibilities include:

- Comprehensive application of statistical quality controlmethods for establishing acceptance/rejection criteria;

- Administering the SOP process

- monitoring data bases to ensure conformance to laboratory andanalytical protocols.

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maintaining strong communication with other levels of laboratory

management.

- maintaining all laboratory certifications

- administration, maintenance and reporting of thelaboratory's single and double blind proficieny program

- Planning, execution and administration of internal audits

Sample Control Manager

The Sample Control Manager oversees the operation of the SampleManagement department. Responsibilities include

- Maintaining proper sample bottle preparation

- sample custody/control

- sample custody/control documentation.

- liason between laboratory and field personnel regarding:

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- upcoming sample analyses

- analytical protocols to be used

- sample handling and preservation protocols.

Manager Client Services

The Client Services Manager is responsible for managing allaspects of client services. When a contract or purchase order is

received, the Client Services Manager contacts the client andestablishes a relationship and communications to satisfy the

client's needs. Responsibilities include:

- Expediting projects

- Ensuring compliance with deadlines and

- Maintaining lines of communication with client

Manager Organics Department

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The Manager of Organic analyses is responsible for thescheduling, coordinating, and supervising GC and GC/MS analysisof environmental samples. Responsibilities also include:

- Adherence of all personnel to analytical SOPs

- Data review

- Implementation and documentation of corrective actions

- Generation of organic analytical SOPs

- Maintenance of calibration and standardization programs

- use of QA/QC acceptance/rejection criteria to validate analyses

- Preventive maintenance program and

- Technical training of department personnel.

- Scheduling and coordination of analytical work in thisdepartment

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Industrial Hygiene Manager

The Manager of Industrial Hygiene is responsible for scheduling,

coordinating, and supervising staff members in the bulk andairborne asbestos testing, as well as all work involvingTransmission Electron Microscopy. Responsibilities also include:


- Data review

- Technical training



- Preventive maintenance program

- Scheduling and coordination of analytical work in thisdepartment

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Manager, Metals Department

The Manager of the Metals Department oversees metals analysis onwater/wastewater, soils, sludge, and filter samples by atomicabsorption spectrophotometry, utilizing flame and graphitefurnace techniques. Responsibilities also include:


- Data review


- Maintenance of calibration and standardization programs

-use of QA/QC acceptance/rejection criteria to validate analyses

- Preventive maintenance program and

- Technical training of department personnel.

- Scheduling and coordination of analytical work in this

department

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Manager, Wet Chemistry Department

The manager of the Wet Chemistry Department is responsible forall wet chemistry testing, including COD, TOC, TOX, total

petroleum hydrocarbonsand microbiological testing.Responsibilities also include:

- Scheduling, and coordination of projects within this department



- Data review


- Maintenance of standardization and calibration programs.

- Development of a preventive maintenance program

- Technical training of department personnel

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Section 3: Health & Safety Effective Date: 7/90Superceded Date: NEW

3.0 Health & Safety

Typical projects require BCM staff to handle, mix, process,and analyze toxic chemicals and samples which contain suchchemicals. The safe and secure execution of these programsrequires knowledge and experience with state-of-the-art

hazardous materials handling. This includes the operationof safety and health systems,(i.e. employee healthmonitoring program, safety showers, eye wash stations, etc.,

waste disposal areas in the laboratory, spill clean-upprocedures, and evaluation of personal protective clothingagainst hazarous chemicals). Information regarding the

handling, disposing, and personal protection for each

hazardous chemical bought is available on Material SafetyData Sheets (MSDS) provided by the vendors. Actual field

sample handling is governed through OSHA standards and isimplemented by personnel through the Health and SafetyDepartment at BCM Engineers in Plymouth Meeting,

Pennsylvania.BCM's health and safety programs are designed to fully

achieve the following goals:

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BCM Laboratory QA Program Plan Page 2 of 3Section 3: Health & Safety Effective Date: 7/90


Protect the employee;

Protect the public; andProtect the environment.

These goals are achieved through a hierarchy of health andsafety programs beginning with the Health and Safety

Department and proceeding through the laboratory safetycommittee. This achievement is based upon both regulatorycompliance and the development and maintenance offacilities, techniques, and capabilities.

federal ^The handling of hazardous materials subject BCM toregulations such as OSHA and RCRA. The following is asummary of these regulations:

OSHA Safety and Health Standards (29 CFR 1910) — OSHAregulations specify the general industry safety standardsapplicable to all workplaces. In addition, the OSHA

regulations contain one subpart specifically applicable towork involving hazardous materials.

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BCM Laboratory QA Program Plan Page 3 of 3Section 3: Health & Safety Effective Date: 7/90


sSubpart Z, "Toxic and Hazardous Substances" contains

standards for handling specific chemicals classified asoccupational carcinogens, and standards for communicating toemployees information regarding the hazards posed by these

chemicals.

Resource Conservation and Recovery Act (RCRA) — The

regulations promulgated under RCRA define the requirementsfor management, storage, transport, and disposal of

hazardous wastes.The hazardous materials health and safety program at BCMutilizes current regulations as minimum requirements only.

The laboratory has designated and trained individuals tomaintain an effective hazardous waste disposal system.

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BCM Laboratory QA Program Plan Page 1 of 12Section 4: Quality Control Effective Date: 7/90


4.0 Quality Control Protocols

BCM analytical protocols call for a level of quality control

which meets that specified within the particular regulation towhich they apply (i.e. CERCLA, RCRA, etc.). This includesroutine analysis of spikes, duplicates, field and trip blanks,

and QC standard checks for inorganic and organic procedures.

4.1 Notebooks

Manually obtained data are recorded by the analyst in bound,volume-numbered laboratory notebooks. The analyst must

accurately record all data directly into the notebook. Benchsheets which are later transcribed into the notebook are

forbidden. Should there be errors, a single line through theerror(s) will be made along with the analysts initials anddate. This procedure documents:

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\- An error was made

- A correction was effected, and

- Readable documentation of the error has been maintained toensure data documentation integrity.

The notebook will be signed and dated at the bottom right-handportion of the page when that page is completed or theanalyses for that day are completed. Should a portion of thepage not be used, a diagonal line will be drawn acrossportion of the page. Data generated will be validated byanother analyst/supervisor. The page will then becountersigned and dated; this review will occur no later than

the following work day.

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Automated Data Acquisition

Many analyses performed in the laboratory are computerized. Notebooksfor 'recording data' in these instances are not needed. The notebook

as 'run chronicle' is required by the BCM laboratory. Its content isspecified by the department management to allow efficient data

retrieval and cross-referencing. Generally, the run chronicle willindicate the position of the sample(s) in the analytical run, dateanalyzed, dilutions, and batch numbers. The automated data

acquisition system must contain, at a minimum, the followinginformation:

- Calibration standards

- Instrument conditions

- Date of analysis

- Analyst identification

- Continuing calibration verification standards

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u IBCM Laboratory QA Program Plan Page 4 of 12Section 4: Quality Control Effective Date: 7/90


- Method Blanks

- Spiked Method Blanks

- All other Quality Control samples

An automated data acquisition system can be used in lieu of anotebook provided that all information required for proper andcomplete data reporting is provided.

The notebook 'run chronicle' tracks a sample through samplepreparation, analysis, and concise information required for datapackage reporting.

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Section 4: Quality Control Effective Date: 7/90Superceded Date: NEW

4.2 Standard Preparation

All standards (stock, working and calibration) must have thefollowing documentation:

- Stock standards must have date of purchase, expiration dateand date opened recorded on the bottle and in adesignated notebook.

- Working standards' preparation must be recorded in a

standards' notebook. The information must include:

- Solvent used- Dilutions- Final concentration- preparer's initials- Date of preparation

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Standard containers must contain at a minimum the following:

- Solvent used- Standard name

- Final concentration- Date of preparation- preparer's initials

4.3 Quality Control Samples

The BCM Laboratory's various analytical departments will maintsufficient stock and distribute quality control samples at thedepartment manager's/supervisor's discretion. These samples willbe analyzed concommitantly with real samples. The results of

these standards will be used to determine process analyticalaccuracy.

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4.3.1 Proficiency Samples

These are single blind samples issued by an organization of thestate or a separate accrediting/certifying agency. Successfulanalysis of these samples enables the laboratory to operate

within the jurisdiction of the issuing agency. Once the analysishas been completed, the data shall be reviewed and transcribed to

the reporting form by a senior member of that department thensubmitted to the Lab Quality Assurance department for a final

review. The QA department will review for completeness and

possible transcription errors.

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4.4 Analytical Balances

The laboratory must maintain a service contract for allanalytical balances. The balances are serviced by a qualified

serviceman every six months. Each balance shall be initialled bythe serviceman and a receipt for each service will be filed inthe lab's quality assurance department.

Prior to use and once per day the analyst must check the accuracyof the balance using class 'S' weights. One weight in themilligram weight range and one in the gram weight range. Shou]discrepancies between actual weight and observed weight be notec

the QA department should be notified and the balance will beserviced.

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4.5 Thermometers

Thermometers used at the BCM Laboratory shall be 'precision1thermometers by manufacture. The thermometers for chemical use

will have graduations not greater than 0.5 degrees C increments.The liquid column of the glass thermometer will have noseparations. The BCM Laboratory will have at least one 'NIST1

certified thermometer.

New thermometers will be initially calibrated against a certifiedthermometer following BCM Lab's SOP for thermometer calibrations.Thermometers will then undergo an 'ice-point check" every year

against a certified thermometer.

4.6 Spectrophotometers

All laboratory Spectrophotometers (e.g. uv/vis, IR ) will becalibrated at least yearly following the appropriate calibrationSOP.

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4.7 Temperature Control Devices

All ovens, refrigerators and incubators shall be monitored fortemperature consistency and conformance. These records shall berecorded in the form of control charts which shall be posted on

or near the temperature control device.

4.8 Laboratory Water System

The laboratory purification system at BCM consists of the

following:

A carbon filter bed

Cation filtration bedAnion filtration bed and

Two mixed (40% cations and 60% anion resins) filtrationbeds

The water is monitored daily for specific conductivity and

monthly for all possible organic and inorganic contaminants.

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4.9 Control Charting

The BCM Laboratory is required to monitor analytical trends inthe various quality control samples used for all analyses. The

following quality control parameters are routinely monitored:

- Percent recovery from matrix spikes

- Relative percent difference obtained from matrix spikedulicate

- Percent recovey of all analytes used in 'spiked method

blanks'

- Percent recovey of surrogates compounds used in method

blanks

- Contamination levels detected in method blanks

- Response factors of all organic analytes.

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There may be the need to monitor (chart) certain parameters other

than percent recovery or relative percent difference which can

offer the analyst insight as to the stability or suitability ofthe measurement system. The analyst is encouraged to recognize

those aspects of the analytical measurement system which, ifmonitored, may aid in determining the stability of the system.

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Section 5: Training and Effective Date: 7/90Standardization Superceded Date: NEW

5.0 Training and Standardization

It is the BCM Lab's objective that the quality and consistencyof data generated by laboratory staff be independent of theperson performing the work. Conformance to standardizingoperating procedures for all laboratory activities, a thoroughprogram of training, and periodic proficiency reviews ensure

achieving this objective. All laboratory personnel complete atraining program consisting of at least the followingactivities before being permitted to perform an analyticalmethod independantly:

Instruction by the department supervisor on all aspectsof the method(s) and supporting SOPs;

- Chemical reactions taking place during analysis

- Physical processes taking place during analysis

Analytical manipulation

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Section 5: Training and Effective Date: 7/90Standardization Superceded Date: NEW

- Data recording and reporting requirements

Data interpretation

Real time QC decision making tools

- Troubleshooting

Observation of the trainee by an experienced analyst;

Review of performance by the supervisor, throughinspection at the bench, review of performance with

single blind quality control samples, and review oflaboratory data following the analyses;

iPeriodic audit of procedures and performance by lab QApersonnel; and

Participation in in-house seminars on proceduralchanges and on laboratory safety.

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BCM Laboratory QA Program Plan Page 1 of 9Section 6: Quality Assurance Audits Effective Date: 7/90


6.0 Quality Assurance Audits

6.1 Introduction

Quality assurance audits play an important role in BCM Lab'soverall QA/QC program. This section describes the role of the QA

auditor and the nature of quality assurance audits.

6.2 Purpose

The purpose of a quality assurance audit is to provide anobjective, independent assessment of a measurement effort. Thequality assurance audit ensures that the laboratory's datagenerating, data gathering, and measurement activities produce

reliable and valid results. Cases can occur in whichinadequacies are identified in the above operations. In suchinstances, audits provide the mechanism for implementingcorrective action.

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6.3 Quality Assurance Auditors

The QA auditors are people who design and/or perform QAperformance and system audits. Since QA audits represent, by

definition, independent assessments of a measurement system andassociated data quality, the auditor must be functionally

independent of the measurement effort to ensure objectivity. Theauditor must fully understand the objectives, principles,and procedures of the measurement efforts to be able to perform athorough and effective evaluation of the system.

The auditor must be able to identify components of the systemthat are critical to overall data quality. For this reason, theaudit focuses heavily upon those elements. The auditor's

technical background and experience provide the basis for

appropriate audit standard selection, audit design, and datainterpretation.

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BCM Lab's organizational structure, described in Section 2,

ensures the independence of the QA function. The laboratory QAmanager is given the responsibility for the administration andexecution of audit activities at the laboratory facility. The QA

staff assists the manager in designing and performing systemaudits. These are internal audits which are conducted by the BCMlaboratory's quality assurance personnel.

6.2 External Audits

External audits are those conducted by an independentorganization such as EPA, AIHA, PADER, NJDEP and the BCM

corporate Quality Assurance department. The purpose these auditsis twofold:

l.To assure senior laboratory management that thelaboratory's QA department is effective and that theobjectives of this quality assurance program plan are met.

uBCM Laboratory QA Program Plan Page 4 of 9Section 6: Quality Assurance Audits Effective Date: 7/90


2.To provide BCM clients both existing and prospective, with

the assurance that a quality service is being provided atthe laboratory.

The BCM Laboratory's QA department performs three generaltypes of audits (technical systems, performance evaluation,and data quality) which are described in the followingsubsections.

6.3 Technical Systems Audits

A technical systems audit is an on-site, qualitative review ofthe various aspects of a total sampling and/or analyticalsystem. The technical systems audit is an assessment of overalleffectiveness, and represents an objective evaluation of a set ofinteractive systems with respect to strengths, deficiencies, and

potential areas of concern. Typically, the audit consists ofobservations and documentation of all aspects of sample analyses.

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These audits review the following technical components:

- Calibration procedures and documentation

- Completeness of data forms, notebooks, and other reportingrequirements

- Data review and validation procedures

- Data storage, filing, and recordkeeping procedures

- Sample custody procedures

- Quality control procedures and documentation

- Operating conditions of facilities and equipment

- Documentation of maintenance activities

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The laboratory's QA department prepares detailed systems auditchecklists prior to each audit. These delineate the critical

aspects of each methodology and measurement system. Checklistsare used by the BCM management as audit guidelines and byauditor(s) to document all observations.

Technical Systems Audits do not address the following:

measurements; policies regarding the role of Quality Assurance;and concerns involving assessments of the data quality indicators(i.e. accuracy, precision).

6.4 Performance Evaluation Audits

The purpose of performance evaluation audits is to quantitatively

assess the measurement data quality. These audits provide adirect evaluation of the various measurement systems'capabilities to generate quality data. This evaluation isaccomplished by challenging the measurement system with acceptedreference standards (i.e. EMSL standards) which are generally

single blind in nature.

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Performance evaluation audits address the following:

- Accuracy and precision of the measurement system.

- The quality control data as compared to the actual datacollected.

- The measurement system as a function of established controllimits.

- Significant deviations of precision and accuracey over time.

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6.5 Audits for Data Quality

Audits for data quality provide information required to validate

the quality of data by adressing the following:

- Adequacy of data recording

- Precision and accuracy of resultant data

- Adequacy of data calculation, generation, and processing

- Documentation of procedures

- Identification of method limitations to aid users in the

evaluation and application of data

Audits of data quality will establish whether the data collectionprocedures need modifications, and whether the documentation ofquality control protocols is adequate.

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uBCM Laboratory QA Program Plan Page 9 of 9Section 6: Quality Assurance Audits Effective Date: 7/90


Audits for data quality are performed when reviewing final

reports and data package deliverables. These audits are performed

with the 'end data users' requirements in mind. It is the BCMLaboratory's objective to present data in a concise,understandable format.

6.6 Post-Audit Debriefing

Following each audit, a post-audit debriefing session isconducted. The purpose of this session is to discuss preliminaryaudit results with the audit participants. The debriefingsession is followed by a detailed audit report that identifies

areas of concern and recommendations for corrective actions.

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BCM Laboratory QA Program Plan Page 1 of 5Section 7: Standard Operating Effective Date: 7/90

Procedures Superceded Date: NEW

7.0 PURPOSE

Standard operating procedures (SOPs) play an integral role in a

laboratory's QA/QC program. Well-defined procedures detailing allphases of the analytical process are important in producing

comparable, reliable, repeatable results.

SOPs are developed at the BCM laboratory for every routine or

repetitive analytical and/or non-analytical task.

7.1 SOP CONTENTS

The basic requirements for SOP generation are well defined at BCM

laboratories. To maintain consistency, BCM has established (at aminimum) the following 13 sections for its technical SOPs:

- Application- Sample handling and Preservation- Interferences

- Method Summary- Apparatus- Reagents

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- Standard Preparation- Quality Control- Procedure- Calculations- Data Documentation

- Strip Charts/Chromatograms/printouts- Computer Setup (optional)

The format for non-technical SOPs contains, at a minimum, thefollowing six sections:

- Purpose- Application- Safety- Procedure- Quality Control- Documentation



7.2 SOP GENERATION

SOPs are initially drafted by a senior member (preferrably) of

the department in which the SOP is required. It is then submittedto the laboratory's Quality Assurance department for review,editing, formatting and to enter the SOP into the document

control system.

Once this is established, the document is circulated for review.The review process is as follows:

- Originator- Department supervisor- Department manager- Department Director- Technical Director- Laboratory Director

Having gone through this approval/editing process the document isthen signed, a document control number is assigned, and it is

then distributed to the appropriate department(s).

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7.3 SOP NECESSITY

The EPA defines an SOPs as documents detailing procedures whichare commonly accepted as the method for performing specific

routine or repetitive tasks.

An SOP is needed when any of the following criteria are met:

- The analysis is performed or expected to be performed

on a regular basis.

- The analysis is performed or expected to be performedby more than one analyst.

There are times at BCM laboratory when analyses are requested tobe performed on "one-time" basis. SOPs are not applicable inthese instances.

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Section 7: Standard Operating Effective Date: 7/90Procedures Superceded Date: NEW

7.4 SOP MODIFICATION

SOPs are considered "living" documents and will require updatesin order to stay current. In the event that new method

publications/addendums are published by the EPA or otheragencies, QA notifies the department. The department plans andimplements the revised procedure. The old SOP is annotated to

reflect the change. The SOP is then revised to incorporate thenew procedure. It is then submitted for the usual editing and

document control procedures. The document revision is givenhighest priority, and it is then returned to the analyst asquickly as possible.

AR3QIS27

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BCM Laboratory QA Program Plan Page 1 of 4Section 8: Document Control Effective Date: 7/90


8.0 DOCUMENT CONTROL

8.1 INTRODUCTION

A laboratory such as BCM must have an effective system for tracking,archiving and updating those documents which are generated (e.g. data

packages) and those which govern and document the laboratory's dailyoperations (e.g. SOPs, notebooks).

8.2 STANDARD OPERATING PROCEDURES

These documents are developed, written, edited and assigned adocument control number by the laboratory Quality Assurancedepartment. These documents contain the following information on

every page:

- an effective date

- the superceded date (if applicable)- the document name- the page number (in the form 'page _ of _')

ftR30l5-29

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Hard copies of these documents are maintained in the laboratory's

quality assurance office. Copies are made and distributed to all

applicable laboratory personnel. Revisions are effected by the

laboratory QA department, a superceded date is documented, and therevised SOP is then distributed to lab personnel. Copies of SOPs are

stored on magnetic discs in two separate locations (Lab QA andCorporate QA).

8.3 LABORATORY NOTEBOOKS

Laboratory notebooks are bound books which are assigned by a membeof the laboratory quality assurance department to an individualanalyst. The notebooks are assigned a volume number, pagedesignations for each volume are also recorded this aids in data

retrival. New notebooks are assigned at the beginning of each year in

order to further aid in data retrival.

8.4 COMPUTER GENERATED DATA

All data which is generated by an automated data acquisition systemis to be magnetically stored for a period not less than .five years.Data acquired by the GC/MS systems will be archived on eight track

magnetic tape. Data acquired by the GC data acquisition system will

£8301530



be archived on 'CS-80 ' data cartridges. Data generated on PCs will

be archived to floppy diskettes. Once archived, the laboratory must

keep these records for no less than five years.

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Section 8: Document Control Effective Date: 7/90Superceded Date: NEW

8.5 Data Packages

The collation of analytical data packages is performed by the

Documents Department at the laboratory. Once the data is reviewed and

released the package is copied. The original is sent to the client

and an exact duplicate is kept at the laboratory for two years. The

data packages are then transported to off-site storage for an

additional three years. They are then disposed.

8.6 Client Reports/ Invoices

Analytical reports and invoices are generated by the laboratory's

administrative staff. Once released, the original reports and

invoices are sent to the client. Copies are then microfiched and

maintained at the laboratory for five years.

ftR30!532

SPa5-CO

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BCM Laboratory QA Program Plan Page 1 of 11Section 9: Sample Custody, Sampling, Effective Date: 7/90

and Sample Tracking Superceded Date: NEW

9.0 Sample Custody, Sampling, and Sample Tracking

9.1 Sample Custody

A stringent chain-of-custody system is vitally important inensuring the validity of collected data. There must be adocumented, traceable link between any given measurement and the

sample and parameter that it is reported to represent. Thechain-of-custody must represent a legally acceptable record thatcovers all aspects of the pre-sampling preparation, samplecollection, post-sampling handling, storage, and analysisprocess. This record originates with the preparation of allsample containers that are used and indicates "who did what andwhen" until final disposition of the sample. The custodyprocedures used are also to ensure that the integrity of the

sample is maintained throughout the course of the collection,handling, and analysis process (i.e., that there is noopportunity for inadvertent contamination).

SR30153**

D



The EPA National Enforcement Investigations Center (NEIC) defines

a sample to be under custody if:

o it is in an individual's possession

o it is in the individual's view after being in theirpossession

o it was in the individual's possession and was locked up

o it is placed in a designated secure area

Refer to Figure 4.1 for a sample of a chain-of-custody form

9.2 Sampling

Field sampling is outside the scope of laboratory operations;however, sampling packages are provided by the laboratory for

field sampling projects. Sampling packages are designed tosimplify the task of collecting environmental samples andshipping them to the BCM Laboratory for analysis. Sampling

packages contain the following:

&R30I535



o Sample containers, pre-cleaned by BCM Laboratory, in

accordance with EPA protocol;

o Sample Chain-of-Custody forms;

o Sample labels, see Figure 4.2;

o Chemical ice packs (where applicable);

o Foam inserts;

o Absorbent packing material; and

o Summary of sample containers, preservation techniques

and holding times, see Table 4.1.

9.3 Laboratory Sample Control and Sample Tracking

Sample control and tracking is organized by a Laboratory

Information Management System (LIMS).

A830I536



All sample information, including the date for sample disposal or

return, is stored in the LIMS computer system. Samples receivedat BCM are delivered immediately to the Login Department. Allshipping containers are inspected for physical damage or evidence

of tampering.

The samples are unpacked by the Sample Custodian. Shipping

containers, condition of samples, the number of samples percontainer, and accompanying documentation are noted in a bound,

volume-numbered log notebook. Sample identification is verifiedagainst the chain-of-custody form. Any peculiarities are broughtto the attention of the Technical Client Services Representative.

A sticker providing a BCM sample number is affixed to eachindividual sample bottle. The samples and corresponding IDnumber(s) are logged into the log notebook and the LIMS computer

system. Analytical requirements and pertinent informationwritten on the accompanying chain-of-custody are also documented

AR'30i537



in the log notebook and computer entered.

Following sample log-in, the samples are placed in the designatedstorage area. The analyst removes the samples from the cold

storage area and obtains custody of the samples by the use of abarcode system. After analysis, the sample is returned to thedesignated storage location in the Login Department. The sample

is stored until the assigned time or written permission is givento either properly dispose of or return the sample to the

client. All sample documentation is maintained in filecabinets.

9.4 Sample Storage/Sample Check-out

The sample storage area is controlled by the Sample Custodian.Access to the sample is only permitted through the samplecheck-out procedure. This procedure requires the analyst to log

onto the LIMS system using his/her password. A sophisticatedbarcoding system allows the following information to be recorded:

1. Sample ID (a six character alphanumeric field)

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3. Date samples were logged in/out

4. Time samples were logged in/out

5. Name of individual who assumed/relinquished custody ofsamples

Once having the above information stored in the computer a reportcan then be issued which details the history of the sample(s)through the laboratory. This report is then attached to the finalreport.

AR30I539



BCMPROJ NO.

CHAIN OP CUSTODY RECORDPROJECT NAUI

•AMPtERS. ftfawctaroJ

STA.NO. OATf TIUE iu

Smetloalapatoha* by:

R*u**w4aa*«' aysfJMffffafvraJ

RoHnouiah**1 by:ffff«at«r*j

E0

STATION LOCATION

Oat*/Tlm«

Oat*/Tlm*

Oat* 'Tim*

NO.OPCON-TAIN-ERS

Roe*iv*a by:(S/ffMfBT*)

Roootvod by:(Sliu»tfr+J

R**«W*« tor (Slttttmr*Laboratory ay.

//////

/SAUPUE TTMT KtV

S-S*4MA-Atr

/ / / ////,./ tAMWUNQ REMARKS

/ / / / / / / V

fS/f*«i»r«7

R»MnoM»i««0 by:fSJM*laro>

at*/ m*

•flHP

.

'Oat* Tim* R*a*rv*« »yt

'•" ~ ?,w*%rSMevMf rRM*r*tn*> Remark*

Distribution Ortotaal Aoo*«a»ai**a SMo*n*«*t, Copy to Coordinator BiWc c'v jfcM A

Figure 9.1. Chain-of-custody Form


and Sample Tracking superceded Date: NEW

BCM ENVIRONMENTAL ANALYTICAL LABORATORY SERVICESSAMPLED SY:SHIP TO". BCM

PLANT:

LABi860 Gravtrs RoiO Nomstown. PA 19401

DATE: 1 TIME:SENT BY:Blllino/PreMct No.

LOCATION:

SAMPLE IDENTIFICATION- OupUeat*ftima

• YwQNoO• YM O Ma n

a ACIDITY zcoo 3 ODOR asoaoincconotmanot- M ana/or O P AIMiimty ~ CHLORIDE ~ OIL I GREASE Q SULFATE3 BOO : COLOR 3pH aSULFIDE3 BROMIDE 3 CYANIDE 3 PHENOLS Q SULFITCC CALCIUM. M C«CO<] r FtUOWOE ~ PHOSPHOROUS, onno aSUFRACTANTCMSA*)= CARBON, oravic ~ HARDNESS 2 PHOSPHOROUS, total D TURBIDITY_; CARSON, toiw - M«gn«»ium •» CaCOj ~ SILICA Q WATER ASSAYBACTERIOLOGICAL. -fvsvCaMom ~T0t»i Coiitorm Z Ftc*i Slnjp, STout Pitta Count OPotabiaWtttrNITROGEN: 3Ammonit 3Nllrit»SOLIDS. 3 Tom 7VOHIH* Tot«!

3Nltntt 3 Organic 3Total<*|«Wah«30lssc;.M 3Vol.OiM.. CSu*Pwwo0 QVoi.Suw. OSWIMM*

METALSISoacitW

OTHER:

BCM M R«» Utl

ENVVWNMENTAL LABORATORY SERVICES

SHIP TO: BCM LAB1850 Gftvart Road « Norrmtown. PA 18401

SAMPLE FROM: " ———

SAMPLE LO.9ciito*9 F*o<nt of W0fltrtylnQ MflfM) or I>xno<« Q«»f __ Tlm»: CoiMetM By

SAMPLE ANALYSIS

Figure 9.2 BCM Lab Sample Labels



Table 9.1. Parameter, Preservation Techniques and Holding Times40 CFR Part 136 Clean Water Act

rt*lM«l

OlMrtMlMI

t

HIM ttr

WaWMHi VOlOtOf ttaWV

Itettrttl l«u:ftctl itrwwncct '. S Cwl, <*C, o.OOB Mti»Oj5*I ttoil *trwtw4BCt '• * Cwl, 4*t, 0.008 atjijOji4' iVOX Iwttiteltltr . '. Cwl, 4*C 14 Mr*Altlllttty '. Cwl, 4*C 14 Mr*MWI« '. Cwi. 4*c, KjUi u UK: . 21 Mr*

ltlBIWK«> Mr*** WMM. CITMMCWWt ',CMCtCII

f.Ut»l «M MM4DU U '.

.*> '•4M (ryot* iltrvwB P.

«• VI J..__-r ",lltriti '.lltrttt '•fit mt ram t

f',

Itlrwftttl) 0ttt*l '.

ttt*l ' •.. .... fllttrwlt '.M*M«*. Miiinitrwlt (US) '.IMI4M, itttl*44)l* '•Iniwi, mUttlt '.Slltct '

Cwl, 4*C 4» ICwl. 4*C. »?», U HtO 21 <MM rtwlrt« 21 Mr*MM rtwir<4 toiCwl. 4»C U _...Cwl. 4*C, |«OH t«,pN>U, t.tf 14 My*nctr*«C K«>

MM rtwlrwMO) U HKJ, KfW U *Kt « MMM- - - - - - , totirttr««i

l, 4*C,Cwl, 4*C, Nt»4 U |WOCwl, 4«C 24 IMM) u **<z n Mn

U KKJ t iCwl. 4*C 4( Icwi, 4*t, HI»( t* «H<I n iCwl. 4*C M ICwl. 4*C, H»»» U ttKt 21 Mr*Cwl, 4*C, MCI «r tMO« »• «MO a Mnrnttr M««tMiir. cwi, <*t n MOT

It It •* tw MM r*«lrM Mtlrit «lilt M tw Mi •• tin MM *t*rt »• Mrt I MOT'7 Cwl, 4*C, H>»4 U *t<I 21 My*

Cwl. 4»C 41 I ..Cwl. 4°C. MjM< tt t«Kt 21 Mr*Cwl. 4*C J Mr*Cwl, 4*C 41 MOTcwi, 4*e ) MT*Cwl, 4*t 41 kwrtCwl. 4*t 7 My*cwi, 4«c a Mr*cwi. 4*e it Mr*Cwi, 4*e a Mr*Cwl, 4°c <«M IIM Kttitt tin 7 My*twiw »nr«ml4M U IMM

MM rtwlrr*Cwl, 4*CNOHO FWM?OV PAtiiyttCwl, 4K

talttt** ""' '"•tailiw '.taintt '•S»<4Ct«M* '•

:<7» 'H*l4CtrMI* «, TtUl4«-llM< Cwl, 4»C, 0.0043 HtfM)]{*) 14 Mr*

6, Itlflw-IIDW Cwl, 4*C, O.OOB NtaMhi*' 14 My*HC1 (4) (HI '*'

t, Ttlflwllm* Cwl, 4*C. O.OOB HfiMhH) 14 MrtMjwtt IN tt 4.{ (*>

U, TiUlwltM* Cwl, 4»C. O.OOB MtifOi 7 Mr* Mtll titrtcttaititrtettw

IwiltlM* «. J«lflt*-llM« Cwl, 4«t, O.OOB MtifO] 7 Mr* tWII wtrtettwr*u«utt t*ttr* «. itinwitM* cwi, 4*c 7 Mr* «MII tttrwtiM40 Mjr* *f ttr

i* 001 t, TtlfiwtlMtt Cwl. 4<t, *MT« l« Mrt, O.OQB 7 My* "Hll titrtcttantitrtctlw

KM 4eryl«wltrtl« t, ItUlw-Mw* Cwl, 4*C 7 My* wtll tmtrtiirantat



Table 9.1. Parameter, Preservation Techniques and40 CFR

rwwvttr No./nMM

Mttroiroaittct 4nd tioonoront

Polyngcltir *roa«tlC hydroctroom

lUlottlttrs

Chlortntttd tiydroctrooa*

TCOO

Mtttctdn Tin::rtSltcIM*

Part 136 Clean Water Act (cont.

ConUintrU) Prtmtitton'2'

G, T«tf lon-tintd Cool, 4<>C, O.OOB M SjOjt*) .ttort tn d*rk

i, Itldon.lintO Cool, 4'C, O.OOW HtjSjOjl4),itort In d4rt

G, TtUlon.lintd Cool, 4«C, O.OOU NljSjOji4),

G, ItHlon.ltntd Cool, 4°C

5, !«lf lon-llntd Cool, 4'C, O.OOK MjSjOjM),

-a, Tclflon.hntd Cool, 4'C, pH S*l (u>

Holding Times

1«.,- -,.,„ ,,-HI

7 dty* wit II titrtcttt*40 otyt Ifttrtitrtetton

7 d«yt until tstrKttM40 diy* *fttrt strict Ion

7 dirt until titricttt*40 ««yt «rttrtitrKtloa

7 diy* until txtrtcttt*40 d«yt «fttrtitrKtlaa

7 dty* until titrtctlM40 d«yt <(t4)TtxtrKttto

7 «tyi until titrKtlan40 4t*y« aUirtitrKtlaa

t«»u:MpM, »tt« tM rictlHB f. 6 HMOj to PH<2 t Matin



Footnotes forTable 9.1. Parameter, Preservation Techniques and Holding Times

1 Polyethylene (P) or Glass (G).

2 Sample preservation should be performed immediately upon simple collec-tion. For composite chemical samples, each aliquot should be preserved at thetime of collection. When use of an automated sampler makes U Impossible topreserve each aliquot, then cnemical samples may be preserved by maintainingat 40C until compositing ana sample splitting Is completed.

3 Samples should be analyzed as soon as possible after collection. The timeslisted are the maximum times that samples may be held before analysis andstill be consioereo valid. Samples may be held for longer periods only if thepermittee, or monitoring laboratory, has data on file to show that the speci-fic types of samples unoer study are stable for the longer time, and hasreceived a variance from the Regional. Administrator under § 136.3(e). Somtsamples may not be stable for the maximum time period given in the table. Apermittee, or monitoring laboratory, is obligated to hold the sample for ashorter time if knowledge exists to show that this 1s necessary to maintainsample stability. See $ 136.3(e) for details.

* Should -only be used in the presence of residual chlorine.

5 Maximum holding time is 24 hours when sulfide is present. Optionally illsamples may be tested with lead acetate paper before pH adjustments in orderto determine 1* sulfide is present. If sulfide is present, it can be removedby the aodUion of caomium nitrate powder until a negative spot test 1sobtained. The sample is filtered and then NiOH is added to pH 12.

6 Samples should be filtered immediately on-site before adding preservativefor dissolved metals.

7 Guidance applies to samples to be analyzed by GC, 1C, or GC/HS for specificcompounds.

8 Sample receiving no PH adjustment must be analyzed within seven days ofstapling.

9 The pH adjustment is not required If acrolein will not be measured.Samples for acrolein receiving no pH adjustment must be analyzed within 3 daysof sampling.

10 For the analysis of diphenylnltrosamlne, add 0.008X NajSjOs andadjust pH to 7-10 with NaOH within .24 hours of sampling.

U The oH adjustment may be performed upon receipt at the laboratory and anybe omitted 1f the samples are extracted within 72 hours of collection. Forthe analysis of aldrin, add 0.008X

COaS'

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Section 10: Using Quality Control Effective Date: 7/90

In the Laboratory Superceded Date: NEW

10.0 Using Quality Control in the Laboratory

10.1 The Purpose of Quality Control

The use of Quality Control in the lab generates information to

perform the following:

Evaluate precision and accuracy data in order to qualify(validate) field sample data.

Indicate the need for corrective action measures when QC

data indicates trends or needs for system modifications.

Determine the effect of the corrective action.

10.2 Definitions

To understand a quality control program and quality control data,

a clear description of its components is essential.

BCM Laboratory QA Program Plan Page 2 of 9Section 10: Using Quality Control Effective Date: 7/90


ACCURACY: The proximiy of a result or the mean (X) of a set ofresults to the true value. Accuracy is expressed as a

percent recovery (%R).

PRECISION: The measure of agreement of a set of replicate results

without any prior knowledge of the true value.Precision is expressed as relative percent difference(RPD).

ANALYTICAL

BATCH Samples of similar composition (matrix) which areanalyzed together with the same method and sequence ofevents. The same lots of reagents and in the same time

period or in continuous sequential time periods.

STANDARD

CURVE The graphical representation of an analyteconcentration versus its corresponding instrument

response.

u


Section 10: Using Quality Control Effective Date: 7/90In the Laboratory Superceded Date: NEW

METHOD

BLANK An artificial sample used to monitor the introductionof contamination into the analytical process. The blankis treated exactly as the sample and is analyzed within

an analytical batch.

CALIBRATION

CHECK

SAMPLE A blank which has been spiked with the analyte(s) ofinterest from an independant source to monitior theexecution of the analytical method.

ENVIRONMENTAL

SAMPLES A representative sample of any material collected from

any source for analysis. The BCM Laboratory categorizesenvironmental samples as follows:

GroundwaterWastewaterDrinking Water

Hazardous WasteAir

ftR3-OI5li8



SURROGATES Organic compounds which are similar to analytes ofinterest,but not normally found in environmental

samples.These compounds are then spiked into all blanks

standards and samples prior to analysis. Percentrecoveries are calculated for each surrogate; thisrecovery indicates the efficacy and efficiency of themethod on a given environmental matrix.

MATRIX SPIKE/

MATRIX SPIKE

DUPLICATES In matrix spike/matrix spike duplicate samples a knownquantity of sample of certain analytes are added to a

sample matrix prior to sample extraction, distillation

or digestion. Soil and wastes samples are homogenizedand split into duplicates, spiked and analyzed. Percent

recoveries are then calculated along with the relativepercent difference between the samples.

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Section 10: Using Quality Control Effective Date: 7/90In the Laboratory Superceded Date: NEW

FIELD

RINSATE

BLANKS Reagent water used in the field to rinse sampling

equipment. This is used for the determination of crosscontamination from one sampling source to another.

TRIP BLANK Reagent water is transported to the sampling site in 40

ml VOA vials. The trip blank is unopened but analyzed

with the associated samples to determine potentialtransmigration of volatile organics to other samples.

METHOD

DETECTION

LIMITS Method detection limits (MDLs) studies are performed todetermine the minimum concentration of an analyte thatcan be measured and reported with 99% confidence that

the analyte concentration is greater than zero and isdetermined from analysis of a sample in a given matrix

containing the analyte. The procedure used for MDL

determination is found in 40 CFR 136 Ap. A.

88301550



10.2 Applying Quality Control

When performing analyses in the laboratory it is manadatory thatthe analyst has a copy of the analytical SOP and that it isfollowed implicitly. All quality control procedures are detailedin these SOPs.

All analytical procedures contain much of the same basic elements

and their impact on the data will be dicussed:

A) Calibration standards (all)B) Check standard (all)C) Method blank (all)D) Spiked method blanks (all)

E) Surrogate recovery (organics)F) Matrix spike/duplicate samples (all)

G) Control Charting (all)



A) Calibration Standards must be generated at a minimum of

three concentration levels. The correlation or linearity of

these calibration standards must meet those spcified in theindividual method. The acceptability of these standards is

critical for the analysis of the environmental samples.Should these samples not conform to the requirementsspecified, they must be prepared and reanalyzed.

B) Check Standards are standards which are prepared from asecondary source at a specified concentration so as to checkthe validity of the calibration of the measurement systex Bas well as a check to ensure that the measurement system isperforming optimally. Should the check standard fall outsidethe established criteria, the analyst must stop the analysis

and try to ascertain the cause. Refer to the individual SOP.

for details regarding preparation and acceptable limits.

C) Method Blanks are used in most analyses. These blanksgenerally constitute the primary analytical solvent being

used in the method. The method blanks are run per analytical

batch and are used as indicators of potential samplecontamination as well as background laboratory

S83Q1552

u



contamination. Contamination greater than the regulatoryquantitation limit allowed can compromise sample data.

D) Spiked Method Blanks are solvent blanks spiked with aspecific analyte at a predetermined concentration. Spikedmethod blanks are used on a per batch basis in order toascertain method efficiency independent of matrixinterferences. Should recoveries be poor the analyst must

assume that the analytical measurement system is notfunctioning optimally.

E) Surrogates are compounds which are not expected to befound in the environment. These compounds are spiked into

every sample, standard, blank, matrix spike and matrix spike

duplicate; they are used to evaluate analytical efficiencyby measuring percent recovery. Surrogates are used for

organic analysis.

F) Matrix Spike/ Matrix Spike Duplicate Samples are matrix

samples which are spiked with known quantities of specificcompounds in order to determine the appropriateness of the

method to the matrix in question.

HMOI553

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This spike is performed in duplicate so as to ascertain the

precision of the method to the matrix in question.

G) Control Charting is used by the analyst to graphicallytrack percent recovery and relative percent difference ofthe quality control data generated in order to recognizetrends within an analytical process..

RR30i55i»

&R301555

CO

*._

¥**«*•,**-

J

BCM Laboratory QA Program Plan Page 1 of 7Section 11: Data Quality Calculations Effective Date: 7/90


11.0 Data Quality Calculations

11.1 Introduction

Precision and accuracy are the two most important indicators ofdata quality. Precision is a measure of variability for

replicate measurements of the same parameter. Accuracy measuresthe degree to which a measured value agrees with the true valuefor a given parameter. This section provides instructions for

calculating data quality in terms of precision and accuracy.Other calculations are included at the end of this section.

Precision and accuracy (spikes and duplicates) are used tovalidate sample data and monitor the performance of themeasurement system (i.e. instrument, analyst, and method).

11.2 Precision

The precision of analytical laboratory data is evaluated using(1) standard deviation, (2) range, (3) coefficient of variation,also known as the relative standard deviation, and (4) relative

percent difference.

AR30I55S



11.2.1 Standard Deviation

The standard deviation is an expression of the precision of

data. One standard deviation is a limit within which 68% ofthe data within a specified data set can be found. The formulais as follows:

n-1 W n-1In these equations, n = population size

X = i'th observation in the sample,iX = sample mean

11.2.2 Range

The range is the largest observation in a data set minus thesmallest observation in the data set, often denoted as R.

R = X - Xmax min

J


Section 11: Data Quality Calculations Effective Date: 7/90Superceded Date: NEW

11.2.3 Coefficient of Variation

The coefficient of variation (CV), or relative standard

deviation, is a commonly used measure of variability that is

adjusted for the magnitude of the values in the sample:

CV - Standard Deviation x 100

Mean

The coefficient of variation is used most often when the si

of the standard deviation changes with the size of the mean.

When individual measurements of CV or standard deviation arecombined (pooled) to obtain an overall measure of variability

for a given type of analysis for measurement, the followingtechnique may be used:

Pooled CY - 2 Xj OF1

n2 OF,

i - 1

ftR30i558



In this equation, X = CV of data seti

DF = degrees of freedom for data set i(k( - 1)

n = total number of data sets (e.g.,

total number of duplicate pairs)k = number of data points in set ii

(e.g., k=2 for duplicates)i = data set 1, 2, 3 .... n

11.2.4 Relative Percent Difference

Relative Percent Difference (RPD) is another commonly usedmeasure of variability that is adjusted for the magnitude of

the measured values. It is used only when the sample containsonly two observations and is given by:

RPD - IX - Xl x 100[(X + X )/2]

where X and X are duplicate sample measurement results.1 2

RPD is directly related to CV for duplicate results by:

RPO CY.



11.3 Accuracy

11.3.1 Relative Error

The accuracy of analytical laboratory data is usuallypresented in terms of (1) relative error, and (2) confidence

intervals at the 95% level.

Percent Relative Error = Measured Value - Actual Value x 100Actual Value

95% Confidence Interval - X * t fQ. n-nL

In this equation, X = sample means = sample standard deviationa - risk level (0.025 for the 95% confidence

interval)t(a,n-l) - value of the tabulated student's "t"

distribution for n-1 degrees of freedom and

risk level, a


Section 11: Data Quality Calculations Effective Date: 7/90Superceded Date: NEW

11.3.2 Percent Recovery

Accuracy may also be expressed as percent recovery, given by:

% Recovery = Measured Value x 100Actual Value

In this instance, percent recovery is used with a knownconcentration standard reference material.

Percent recovery is related to percent relative error by:

Recovery = % Relative Error + 100

Spike recovery is commonly used to determine the performanceof a method:

% Spike Recovery = Spike Smpl Cone.(mg/1) - Sample Cone (mg/1) x 100Spike Amount (mg/1)

R830I561

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Section 11: Data Quality Calculations Effective Date: 7/90


11.3.3 Instrument Linearity Checks

Acceptance criteria for instrument response linearity checksare based upon the correlation coefficient, r, of the best fit

line for the calibration data points. The correlation

coefficient reflects the linear of response to the calibrationstandards and is calculated as:

n(V[n(2x2) - (2x)2] [n(2y2} - (2y)2]

In this equation, x - concentration of standard

y = instrument response (peak area)

n = number of calibration points (x, y, datapairs)

The general acceptable criteria for the correlationcoefficient is that it must be > 0.995.

ftR30I562

ro

RR301563

u


Section 12: Data Reduction & Reporting Effective Date: 7/90Superceded Date: NEW

12.0 Data Reduction & Reporting

In the BCM Laboratory, the reduction of raw data is theresponsibility of the analyst. Calculation of sampleconcentrations proceeds in accordance with individual analyticalStandard Operating Procedures (SOPs) given to each analyst.

After properly recording data, the analyst signs and dates eachpage attesting to the validity and completeness of the data. Thecomputed results, the analyst's initials who performed theanalysis, and the notebook page(s) where the raw data isdocumented are entered into the LIMS computer system by the

analyst. This information constitutes a preliminary and/or afinal report which is also generated by the LIMS computer system.On a regular basis, notebooks are checked for errors (i.e.

calculation or transcription) by another analyst, who cosigns anddates pages which have been reviewed attesting that the

information on that specific sheet is valid and understood.

After this review, the department supervisor performs a review ofnotebook. This ensures that all sample documentation and quality

control data (i.e. spikes and duplicates) were

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BCM Laboratory QA Program Plan Page 2 of 4Section 12: Data Reduction & Reporting Effective Date:'7/90


correctly calculated according to the respective analytical SOP

followed.

Identification of systems which are out of control and subsequentoutliers is an integral part of the review of data. Underlyingproblems can be realized and trends can be recognized by controlcharting the routine daily performance of the instrument/analyst.These trends can be used to circumvent problems which wouldotherwise develop unobserved.

A review of the preliminary report, a facsimile of the finalreport, is then performed by the Laboratory Manager. Any

incomplete analyses or questions regarding the validity of the

data found in the preliminary report are brought to the attentionof the department supervisor in which the problem is suspected tohave originated. After all problems have been rectified a finalreport is generated. This report is checked for consistency andcontinuity before it is signed and released by the Laboratory

Manager and forwarded.

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BCM Laboratory QA Program Plan Page 3 of 4Section 12: Data Reduction & Reporting Effective Date: 7/90


A compilation of raw data supporting a final report is called adata package. This package is required only for regulatoryprojects (i.e. DER, RCRA, etc.) or upon client request. TheDocumentation Department, which is under the direction of theTechnical Client Services Representative, collate and audit apercentage of data contained in the data package. The datapackage along with the final report is given to appropriate

personnel (i.e. project managers or engineers) for use in

formulating project action plans.

12.2 Precision & Accuracy Reporting

Matrix precision and accuracy data are reported with every samplebatch or every 20 samples. These are reported as percent recovery

(%R) and relative percent difference (RPD) (see Chapter 11 fordefinitions and calculations). These data inform the user as tothe applicability of the analytical method to the sample matrixbeing analyzed.


Section 12: Data Reduction & Reporting Effective Date: 7/90Superceded Date: NEW

12.2 Method Detection Limits

Prior to the laboratory employing a method for routine analysisof samples, method detection limits along with precision and

accuracy data must be generated and meet requirements set forthby the governing agency. The procedure for method detection limit

determination is found in 40 CFR 136 Appendix A.

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BCM Laboratory QA Program Plan Page 1 of 4Section 13: Preventive Maintenance Effective Date: 7/90


13.0 Preventive Maintenance

13.1 Introduction

The primary objective of a preventive maintenance program is tohelp ensure timely and effective completion of sample analyses.In implementing this program, efforts are focused in threeprimary areas:

- Establishment of maintenance responsibilities

- Establishment of maintenance schedules for major and/or

critical instrumentation and apparatus

- Establishment of an adequate inventory of critical

spare parts and equipment

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13.2 Maintenance Responsibilities

Maintenance responsibilities for permanently assigned equipmentare delegated to the respective Laboratory Supervisors. Thelaboratory supervisors then establish maintenance procedures andschedules for each major equipment item. The maintenanceprocedures and schedules are kept with each piece of equipment.Responsibilities for specific items may be delegated tolaboratory personnel, although the Laboratory Supervisors retain

responsibility for ensuring adherence to prescribed protocol.

13.3 Maintenance Schedules

The effectiveness of any maintenance program depends to a large

extent on adherence to specific maintenance schedules for eachmajor equipment item. A specific schedule is established for allroutine maintenance activities. Other maintenance activities may

also be identified as requiring attention on a as-needed basis.

1570



Manufacturers' recommendations provide the basis for theestablished maintenance schedules, and manufacturers' service

contracts provide primary maintenance for many major instruments(e.g., GC instruments, mass spectrometers, atomic absorption

spectrometers, analytical balances, etc.) All aspects of routine

and nonroutine instrument maintenance are recorded in logbooks bythe respective laboratory personnel.

Along with a schedule for maintenance activities, an adequateinventory of spare parts is required to minimize equipment

downtime. This inventory emphasizes those parts (and supplies)which:

o are subject to frequent failure;

o have limited useful lifetimes; oro cannot be obtained in a timely manner should failure

occur.

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13.4 Spare Parts

Laboratory Supervisors are responsible for maintaining anadequate inventory of necessary spare parts.

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BCM Laboratory QA Program Plan Page 1 of 1Section 14: Corrective Action Effective Date: 7/90


14.0 Corrective Action

The QA/QC program used by BCM for its analytical servicesplaces the following responsibilities on the laboratoryworkers, supervisors, group leaders, QA officers, laboratorymanagement, and technical staff management:

- All measurement procedures must be followed as specified

by the relevant SOPs- Measurement data must meet the prescribed acceptance

criteria described in the relevant SOPs

When a problem arises, action to correct the problem must betaken promptly. For example, Laboratory Supervisors will

initiate corrective action when QC results fail to meetacceptability limits. In such cases, the analyst executes the

corrective action by reanalysis of the analyte in question.Corrective action is also initiated upon identification of someother problem. The Quality Assurance Group may initiate

corrective action on the basis of QC data or audit results.After corrective action has been initiated, the appropriatepersonnel are informed of the steps that were taken to correct

the problem. Management will evaluate the changes made and are-audit will be done.

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BCM Laboratory QA Program Plan Page 1 of 6Section 15: SOP/ EPA Method Reference Effective Date: 7/90

Listing Superceded Date: NEW

15.0 SOP/ EPA Method Reference Listing

Wet ChemistryTest Parameter SOP Document Control Number EPA Method Reference

Color 600-110.2 EPA # 110.2

Specific Cond. 600-120.1 EPA # 120.1Tot. Hardness 600-130.2 EPA # 130.2

Ca Hardness 600-311C SM 16 311C

Odor 600-140.1 EPA # 140.1

pH 600-150.1 EPA # 150.1

Tot. Dis. Solids 600-160.1 EPA # 160.1

Tot. SUS. Solids 600-160.2 EPA # 160.2

Tot. Vol & Fixed

Solids 600-160.4 EPA # 160.4

% Total Solids 600-160.41 EPA # 160.41

Tot. VolatileSolids 600-160.43 EPA # 160.43

Settleable Matter 600-160.5 EPA # 160.5Turbidity 600-180.1 EPA f 180.1

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Section 15: SOP/ EPA Method Reference Effective Date: 7/90Listing Superceded Date: NEW

Wet ChemistryTest Parameter SOP Document Control Number EPA Method Reference

Langlier Index 600-203 SM 16 203Specific Gravity 600-213E, SM 16 203E

Acidity 600-305.1 EPA ft 305.iAlkalinity 600-310.1 EPA ft 310.1

Group Alkalinity 600-310.11 EPA ft 310.11Chloride 600-325.3 EPA ft 325.3

Cyanide Amenable

to Chlorination 600-335.1 EPA ft 335.1Total Cyanide 650-412B SM 16 412B

(distillation)Total Cyanide 600-335.3 EPA ft 335.3Fluoride 600-340.2 EPA # 340.2

Ammonia N 650-350.2 EPA ft 350.2

(distillation)Ammonia N 600-350.3 EPA ft 350.3Total KjeldahiNitrogen 600-351.2 EPA # 351.2Nitrate as N 600-353.2 EPA # 353.2

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Wet Chemistry

Test Parameter SOP Document Control Number EPA Method Reference

Ortho Phosphate 600-365.2 EPA ft 365.2Total Phosphorus 600-365.4 EPA ft 365.4

Sulfate 600-375.4 EPA # 375.4

Sulfide 600-376.1 EPA ft 376.1

Sulfite 600-377.1 EPA ft 377.1

COD 600-410.4 EPA ft 410.4

Oil & Grease(gravimetric) 600-413.1 EPA ft 413.1

Oil & Grease(IR) 600-413.2 EPA ft 413.2

Total Petroleum

Hydrocarbons 600-418.1 EPA # 418.1Phenols

(distillation) 650-420.2 EPA ft 420.2Phenols (4,AAP) 600-420.2 EPA ft 420.2

MBAS 600-425.1 EPA ft 425.1

TOX 600-9020 EPA ft 9020

BOX 600-APP.D EPA ft APP.D

Ignitability 600-FLPT EPA ft 173.150Reactivity 650-335.3, 650-376.1 EPAft335.3, 376.1

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Metals SOP Document

Test Parameters Control Number EPA Method Reference

Aqueous Sample Prep.

ICP/AAFlame 450-3010FICP EPA ft 3010

Solid,Semisolid sample

prep ICP/AAFlame 450-3050FICP EPA ft 3050

Solis,Semisolid sample

Mercury Analysis 400-245.5 EPA # 245.5

Aqueous sample

Mercury Analysis 400-245.1 EPA # 245.1

Graphite FurnaceAtomic Absorption 400-GFAA CLP SOW 7/88

Graphite Furnace w/Zeeman Correction 400-GFAAZC CLP SOW 7/88

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Metals SOP DocumentTest Parameters Control Number EPA Method Reference

ICP Analysis for trace EPA ft 200.7Metals in Water & Wastes 400-200.7 CLP SOW 7/88

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Organic SOP DocumentTest Parameters Control Number EPA Method Reference

Extraction forSemivolatiles 250-SVCLP CLP SOW 2/88

Extraction forPesticides 250-PEST/PCB CLP CLP SOW 2/88

Pesticide/PCBAnalysis 200-PPCLP CLP SOW 2/88

CLP Volatile

Analysis 500-VCLP CLP SOW 2/88

CLP SemivolatileAnalysis 500-SVCLP CLP SOW 2/88

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BCM Laboratory QA Program Plan Page l of 1Section 16: References Effective Date: 7/90


1. 40CFR/10-84 = "Guidelines Establishing Test Procedures for the

Analysis of Pollutants Under the Clean Water Act", 40CFR, Part

136, Federal Register 49 (209), October 26, 1984.

2. SW846 3rd ed. = "Test Methods for Evaluating Solid Waste",

SW846 Third Edition, Office of Solid Waste, U.S. EnvironmentalProtection Agency, Document Control No. 995-001-00000-1, 1986.

3. EPA-600/4-79/020 = "Methods for Chemical Analysis of Water and

Wastes", EPA-600/4-79/020, EMSL, Cincinnati, OH, 1983.

4. EPA-600/4-79/019 - "Handbook for Analytical Quality Control in

Water and Wastewater Laboratories", EPA-600/4-79/019, EMSL,

Cincinnati, OH 1979.

5. Statement of Work, Organic, 2/88 Rev., US EPA ContractLaboratory Program.

6. statement of Work, Inorganic, 7/88 Rev., US EPA ContractLaboratory Program.

7. Interim Guidelines and Specifications for preparing Quality

Assurance Project Plans, QAMS-005/80, 12/29/86.FIN

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