1•I1111111

1

Sikes Disposal PitsCrosby,Texas

Work Plan - Volume IVQuality Assurance Plan

Submitted to:

Texas Department

Water Resources

LOCKWOOD. ANDREWS &NEWNAM, INC.

In Association with:

ENVIRONMENTAL SCIENCE ANDENGINEERING, INC.

HARDING LAWSON ASSOCIATES

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983695

WORK PLAN FOR

SIKES SITE

VOLUME IV

QUALITY ASSURANCE PLAN

Prepared in Cooperation

with the

Texas Department of Water Resources

and the

U.S. Environmental Protection Agency

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This is Volume IV of a 4-volurne work p lan presented to the Texas Department

of Water Resources in partial fulfillment of contract requirements on the

Sikes -S i te Studies. . The four volumes are as fo l lows:

I. Project Act iv i ty and Sampl ing Plan

II. Project Safety Plan

III. Data Management and Chain-of-Custody Plan

IV. Quali ty Assurance Plan

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VOLUME IVTABLE OF CONTENTS

Section Page

1.0 PROJECT DESCRIPTION 1-1

2.0 PROJECT ORGANIZATION AND RESPONSIBILITIES 2-1

3.0 QA OBJECTIVES FOR MEASUREMENT DATA 3-1

3.1 PRECISION, ACCURACY, AND COMPLETENESS 3-13.2 ROUTINE LABORATORY AND ANALYST CERTIFICATION 3-3

3.2.1 ROUTINE LABORATORY CERTIFICATION 3-33.2.2 ANALYST CERTIFICATION 3-3

4.0 SAMPLING PROCEDURES 4-1

5.0 SAMPLE CUSTODY 5-1

5.1 FIELD-DOCUMENTATION 5-15.2 ANALYTICAL DOCUMENTATION 5-45.3 DOCUMENT CONTROL AND REVIEW 5-6

6.0 CALIBRATION CONTROLS AND FREQUENCY 6-1

6.1 GENERAL CALIBRATION PROCEDURES 6-16.2 GAS CHROMATOGRAPHY (GC) 6-26.3 GC/MASS SPECTROMETRY (GC/MS) 6-36.4 INDUCTIVELY COUPLED ARGON PLASMA SPECTROMETRY

(ICAPj 6-4

7.0 ANALYTICAL PROCEDURES . 7-1

8.0 DATA REDUCTION, VALIDATION, AflD REPORTING . 3-1

8.1 OUTLIERS 8-58.2 DATA VALIDATION 8-5

9.0 INTERNAL QC CHECKS ' 9-1

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VOLUME IVTABLE OF CONTENTS

[Continued, Page 2 of 2]

Section Paae

10.0

11.0

12.0

13.0

- 14.0

PERFORMANCE AND SYSTEM A U D I T S

P R E V E N T I V E M A I N T E N A N C E

11.1 GAS CHROMA TOGRAPHS11.2 GC/MS11.3 TOC A N A L Y Z E R S11.4 ICAP11.5 TOX A N A L Y Z E R11.6 SPECTROPHOTOMETERS11.7 A N A L Y T I C A L BALANCE

P R O C E D U R E S U S E D TO ACCESS DATA P R E C I S I O N , A C C U R A C Y ,AND COMPLETENESS

CORRECTIVE ACTION

13.1 P R O B L E M I D E N T I F I C A T I O N13.2 F O L L O W U P P R O C E D U R E S

QA REPORTS TO .MANAGEMENT

14.1 R E G U L A R R E P O R T I N G14.2 N O N R E G U L A R R E P O R T I N G

10-1

11-1

11-111-211-211-211-311-311-4

12-1

13-1

13-113-2

14-1

14-114-1

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VOLUME IVLIST OF FIGURES

Page

Organization Chart, French Limited/Sikes.Pit SiteInvestigations 2-2

5-1 Sample Labels 5-2

5-2 Field Chain-of-Custody Logsheet • 5-3

5-3 Flow Chart of Interactive Sample Analysis andRecording System (ISARS) 5-5

5-4 Project Filing System. 5-7

8-1 DATA Input Form 3-2

13-1 Quality Assurance Corrective Action Request andRouting Form 13-4

14-1 Quality Assurance Corrective Action Status Form 14-2

LIST OF TABLES

.Table . Page

3-1 Summary of Precision, Accuracy, and CompletenessObjectives of Standard EPA Methods 3-2

1.0 -PROJECT DESCRIPTION

The overall goals and objectives of these investigations are to

characterize the Sikes site with respect to the presence of hazardous

wastes, characterize the wastes onsite, determine the extent of waste

migration from the site, evaluate target receptors, and determine site

geology and hydrogeology.

The site, which is currently owned by Mrs. Sikes, is a 25-acre tract

near Crosby, Texas. Several unlined disposal pits are located on the site.

These pits were used until 1967 to dispose of industrial wastes from nearby

petrochemical industries. An undetermined number of drums containing

unknown wastes are also onsite.

. Flooding of the site by the nearby San Jacinto River has occurred in

the recent past. As a result, contaminated materials were released into

the immediate surrounding area. Federal, state, and local sampling teams

have determined that the waters and sediments in the pits are contaminated

with inorganic and organic waste materials. No known remedial actions have

been accomplished to date to mitigate contaminant migration from the site.

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2-1

2.0 PROJECT ORGANIZATION A.NO RESPONSIBILITIES

An o rgan iza t i on chart for the project is presented in F i g u r e 2-1. The

duties of the key i n d i v i d u a l s in r e l a t i o n s h i p to Q u a l i t y Assu rance ( Q A ) are

as fo l lows .

The Project QA Supervisor is designated by the QA Manager . The

supervisor provides specif ic QA support to project management and ensures

that primary technical operat ions are e f f i c i e n t l y coord ina ted for a

spec i f i c project. As a member of the project management team, the Project

QA Supervisor is responsible to the Project Director for the f o l l o w i n g :

1. Development of a specific Project QA P l a n which def ines the QA

objectives of the project d isc ip l ine area and integrates these

in to a u n i f i e d program;

2. Implementation of system and performance audi ts d u r i n g project

operat ion to assure that the def ined opera t ions are proper ly

performed;

3. In t roduct ion of performance e v a l u a t i o n samples i n t o the a n a l y t i c a l

f l o w scheme as needed;

4. Prompt n o t i f i c a t i o n of the Project Manager of any q u a l i t y cont ro l

( Q C ) de f i c i enc i e s ;

5. P rov i s ion of gu idance and coord ina t ion to r a p i d l y resolve any

QA/QC problems;

6. M a i n t e n a n c e of all project QA records and assemoly of project QA

data for inspect ion by project management ; and

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LOCKWOOD, ANDREWS,& NEWNAM

Jim Tremblay, Project Manager

ESE PROJECT MANAGER

0. Mizell

QUALITY ASSURANCE

ESE PROJECT DIRECTOR

R. G. Aldetler. Ph.D.

INDUSTRIAL HYGIENE/SAFETY

J. Mousa. Ph.D.

FIELD SAMPLING

R. Fotkemer

C. Haury

CHEMISTRY

K. Hatfield

DATA MANAGEMENT

T. Gillesoie

Figure 2-1ORGANIZATION CHART

FRENCH LIMITED/SIKES PIT SITE INVESTIGATIONS

2-3 oo

7. Provision for independent review to assure the quality of all

deliverables or outputs from the project team to Texas Department

of Water Resources (TDWR), including all progress reports,

technical memoranda, and interim and final report components.

The Project Manager is responsible for effective day-to-day management

of the total project staff as well as direct communication and liaison with

the client. His responsibility specific to QA is.to approve all QA/QC

procedures to be used in the conduct of the project, to provide additional

authority when required to support the Project QA Supervisor, and to

approve of any revisions to the Project QA Plan.

Discipline Managers are responsible for provision of accurate field or

laboratory data produced by analysts and sampling personnel under their

supervision. They are responsible to the Project QA Supervisor and Project

Manager to ensure that all QC procedures are followed and documentation is

provided.

It is the responsibility of analysts and field team members to perform

the required QC procedures and to document all observations in logbooks in

permanent ink. It is the responsibility of analysts to perform preliminary

QC check's to ensure that each batch of data being generated meets all

analytical criteria. Field team members or analysts must also bring any

unusual field or analytical observation or problem to the immediate

attention of his/her Team Leader and the Discipline Manager.

O3-1 E:

3.0 QA OBJECTIVES FOR MEASUREMENT DATA

3.1 PRECISION, ACCURACY, AND COMPLETENESS

Clearly defined objectives for precision, accuracy, and completeness

of the data are necessary to ensure the generation of reliable and

reproducible data of known quality. The maximum QA objectives for each

measurement parameter in terms of precision, accuracy, and completeness are

summarized in Table 3-1 and are based on EPA method acceptance criteria.

The precision of the method will be the percent deviation of the

replicate analyses and/or samples spiked at a known level. The accuracy of

the method will be the average percent recovery of the spikes at a known

concentration level. The percent recovery is calculated by subtracting the

background concentration from each found concentration and dividing by the

spiked concentration times 100 percent.

Where available, EPA precision and accuracy criteria will be used to

assess the acceptability of data as outlined in Table 3-1. In cases where

EPA precision and accuracy criteria are not available for certain methods,

historical ESE criteria will be used.

Data that do not meet the precision and accuracy criteria by the

proper analytical method will be identified by the Project QA Supervisor to

the Project Manager. At this point, any necessary corrective actions will

be initiated.

Table 3-1. Summary of Precision, Accuracy, and Completeness Objectives for Standard EPA Methods

Parameter

Total OryanicExtractables

Total Organic Carbon

Total Organic Hal ide

Phenol

Silver

Arsenic

Ueryl 1 JIIIM

Reference

EPA Method 413.2

EPA Method 739

EPA Method 415.1

Modified EPAMethod 415.1

Interim EPAMethod 450.1

Modified EPAMethod 450.1

EPA Method 420.1EPA Method 417

Federal RegisterMonday, Dec. 3,l'J/9

Federal RegisterMonday, Dec. 3,1979

Federal RegisterMonday, Dec. 3,

Test Condition

Distilled water spiked withn-hexadecane, Isooctane, andchlorobenzeneStandard soil spiked with n-hexadecane, isooctane, andchlorobenzene

Water spiked with oxidizableorganic compoundsSoil spiked with oxidizableorganic compounds

Water spiked with 2,4, 6-tri-chlorophenol

Soil spiked with 2,4,6-tri-chlorophenol

Water spiked with phenolSoil spiked with phenol

Water spiked with silverSoil spiked with silver

Water spiked with arsenicSoil spiked with arsenic

Water spiked with berylliumSoil spiked with beryllium

PrecisionStandardDeviation

(*)

V(

9.4

6.1

5

15

15

7.67.6

14.510

15.815

5.110

AccuracyAverageBias (%)

-10

-2

+8.2

-5

-15

-15

-1.6-1.6

-2.9-10

-1.4-15

-1.5-10

Com-pleteness(percent)

90

90

90

90

90

90

9090

9090

9090

90 ,'.90

000791

Table 3-1. Summary of Precision, Accuracy, and Completeness Objectives for Standard EPA Methods(Continued, Cage 2 of 6)

Parameter

Cadmium

Cliromi urn

Copper-

Mercury

Nickel

lead

Selenium

Ant imony

Reference

FederalMonday1979

FederalMonday1979

FederalMonday1979

FederalMonday1979

FederalMonday1979

FederalMonday1979

FederalMonday19/9

FederalMonday

Register, Dec. 3,

Register, Dec. 3,

Register, Dec. 3,

Register, Dec. 3,

Register, Oec. 3,

Register-, Dec. 3,

Register, Oec. 3,

Register, Dec. 3,

Test Condition

Water spiked with cadmiumSoil spiked with cadmium

Water spiked with chromiumSoil spiked with chromium

Water spiked with copperSoil spiked with copper

Water spiked with mercurySoil spiked with mercury

Water spiked with nickelSoil spiked with nickel

Water spiked with leadSoil spiked with lead

Water spiked with seleniumSoil spiked with selenium

Water spiked with antimonySoil spiked with antimony

PrecisionStandardDeviation

14.710

8.415

17.710

8.710

10.315

20.715

24.115

515

AccuracyAverageBias (%)

+ 1.6-10

-0.23-20

-3.4-10

-2.0-20

-5.7-15

-7.4-15

-H>,7-15

0.0-15

Com-pleteness(percent)

9090

9090

9090

9090

9090

9090

9090

9090

L.J1Ul

19/9

000792

Table 3-1. Summary of Precis ion, Accuracy, and Completeness Object ives for Standard EPA Methods(Continued, Page 3 of 6)

Parameter

Thai 1 ium

Z inc

Reference

Federal RegisterMonday, Dec. 3,19/9

Federal RegisterMonday, Dec. 3,

Test Condition

Water spiked with thalliumSoil spiked with thallium

Water spiked with zincSoil spiked with zinc

PrecisionStandardDeviation

(%)

14.515

2010

AccuracyAverageBias (%)

-2.9-15

+5.3-10

Com-pleteness(percent)

9090

9090

Pest ic ides/PCBs

BenzeneUrumodichlorome thaneiiroiiiofonii

1979

EPA Method 608

Interim EPA* Method,Revised October1980

EPA Method 624

Carbon tetrachlorideChlorobenzeneChloroethane2-Chloroi;thyl vinyl etherClil orof oniiClil oromethaneI) i hromochl oromethane1 ,2-Oiclilorohenzene1 ,3-(J ichlorohenzene1 ,4-Diclilorobenzene

EPA Method!November 1901

Water spiked with lindane, 5 -15aldrin, endrin, DDT,Arochlor 1254Soil spiked with lindane, 5 -15aldrin, endrin. DDT,Arochlor 1254

Water spiked with the 11.1 -10surrogate compounds: bromo-fluorobenzene, pentafluoro-benzene, and 1,4-difluoro-benzene

Soil spiked with the 19.0 -30surrogate compounds: bromo-fluorobenzene, pentafluoro-beozcne, and 1,4-difluoro-benzene

90

90

90

90

000793

Table 3-1. Summary of Precision, Accuracy, and Completeness Objectives for Standard tPA Methods(Continued, Page 4 of 6)

PrecisionStandardDeviation

Parameter Reference Test Condition

AccuracyAverageBias (%)

Com-pleteness(percent)

i (Continued)1,1-Oichloroethane1 ,2-Oichloroethane1 , l-Uicliloroethenetrans-1,2-Oichloroethene1 ,2-l)ichloropropanec i s-1,3-1) jcliloroproperietrans-1,3-Oichloropropenetthyl benzeneMe thy lent; chloride1,1,2,2-TetrachloroethaneTetrachloroethtMieToluene1,1,1-Trichloroethane1,1,2-lrich)oroelhaneTrichloroetheiieT r i ch1 oro f 1 uoroiiie thaneVinyl chlor ide

Acjd Lxtrac_tahles^-Cfiloro-3-mctriyTphenol2-Chlorophenol2 ,4-l)ichloro|)heriol2 ,4-nimuthylphenol2 , 4 - l ) i i i i l r o p h e n o l2-Methyl-4,6-dinitrophenol2-Nitrophenol4-Nitropheno)Pentachloro|)henolPhenol2,4,6-Trichlorophenol

EPA Method 625

EPA Methodt,November 19151

Water spiked with the 20.0 -25surrogate compounds: dg-phenol, peritaf luorophenol,and 2-fluorophenol

Soil spiked with the 23.1 -35surrogate compounds: d(>-phenol, pentafluorophenol,and 2-fluorophenol

90

90

L.)

Ol

000794

Tdhle 3-1. Summary of Precision, Accuracy, and Completeness Objectives for Standard EPA Methods(Continued, Page b of 6)

Parameter Reference

PrecisionStandardDeviation

Test Condition (%)

AccuracyAverageBias (%)

Com-pleteness(percent)

Uase/Neutral ExtractablesATenapfitheneAceiia|ihtliyleneAnthraceneUenzo(a)anthraceneBenzo(b) f luorantherieUenzo(k)fluorantheneBenzo(a)pyreneBenzo(ghi )peryleneBenzyl butyl phthalateBi s(2-chloroethyl)etherBis(2-cliloroethoxy)methaneBis(2-elhylhexyl)phthalateBis(2-ethylhexyl)phthalateBis(2-chloroiso|)ropyl )ether4-Broinophenyl pliunyl etherChlordane2-Chloronaphthalene4-Chlorophenyl phenyl etherI) i bL*nzo( a ,h) antliraceneDi-n-l)iitylphLluildte1 ,3-DichlurobenzeiiuI ,2-l)ichlorc)l)L'iizoiu!1 ,4-l).icliloroberiZL'iie3,3' -IHchlorohenzidineDiethyl phi h.ihil et) iiiu.'lhyl |iht hal.iU:2 .4-Diri i lrotoluene2 ,(>-!) in t trotolueneI) i-ri-uct.ylphl.ha Idle

EPA Method 625

EPA MethodtNovember 1981

Water spiked with thesurrogate compounds: d5-nitrobenzene, 2-fluoro-blphenyl, 1-fluoronaphtha-lene, and decafluorobiphenyl

Soil spiked with thesurrogate compounds: d5-nitrobenzene, 2-fluoro-biphenyl, 1-fluoronaphtha-lene, and decafluorobiphenyl

26.2 +63 90(for d5-nitrobenzene)

16.7 -20 90(for all others)

28.4 t35 90(for d5-nitrobenzene)

23.1 -35 90(for al1 others)

000795

I'ablu 3-1. Summary of Precision, Accuracy, and Completeness Objectives for Standard EPA Methods(Continued, Page 6 of 6)

PrecisionStandardDeviation

Parameter Reference Test Condition

AccuracyAverageBias (X)

Com-pleteness(percent)

Uase/Neutral Extractables (Continued)FluorantlteneIluorenellexachlorohcnzenellcxach I orohu tad i enellexacliloroethane1ndeno(1 ,2,3-cd)pyreneI sophoroneNaphthaleneNitrobenzeneN-Ni trosodi-n-propylamineIMienanlhrenePyreneI ,2,4-rriclilorobenzene

* Interim Method for the Sampling and Analysis of Priority Pollutants in Sediment and Fish Tissue, EPA, LMSL,Cincinnati, Ohio, 1977.

1 Extraction and Analysis of Priority Pollutants in Sediment and Soil, EPA, Athens, Georgia, November 1981.

Source: ESE, l'J83.

000796

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3-8 2

3.2 ROUTINE LABORATORY AND ANALYST CERTIFICATION

3.2.1 ROUTINE LABORATORY CERTIFICATION

The project analytical laboratory is certified for drinking water

analysis by the Florida Department of Health and Rehabi l i tat ive Services

according to the regulations set forth under the Florida Safe Drinking

Water Act (Chapter 403.863, F.S.). The laboratory is also certified by the

National Institute for Occupational Safety and Health (NIOSH) through their

NIOSH Proficiency Analyt ical Testing (PAT) Program.

The analytical laboratory participates in a round-robin testing

program run by the Florida Department of Environmental Regulation (DER) for

water and wastewater analysis for various inorganic and organic parameters.

3.2.2 ANALYST CERTIFICATION

Accurate and precise analyses can be conducted only by well-trained

analysts who can correctly operate instruments, thoroughly understand the

analytical methods they use, use good analytical technique, and understand

and practice necessary QC procedures. While the necessary training may

initially be obtained from courses, experience, or on-the-job training, it

is imperative that the analyst's capabilities be verified prior to

conducting analyses and reviewed periodically thereafter. A list of

qualified personnel for each analytical task w i l l be provided by the

approoriate group leaders to the Project QA Supervisor. At regular

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3-9

intervals, each group leader will review the capabilities of each analyst

and recoimend whether certification should be continued.

For any analytical method, analysts will be considered certified if

they have been involved in developing the precision and accuracy needed for

the analytical methods. The precison and accuracy of data generated by

analysts during the analysis of samples during the project will be audited

by the Analytical Team Leader and the Project QA Supervisor to ensure

compliance with precision and accuracy criteria.

New analysts performing project analyses will be considered

conditionally certified until the first set of accuracy and precision data

is generated. If these data meet the criteria of precision and accuracy

established for the analytical method, the analysts will be considered to

be certified. Any data which do not meet the criteria may be rejected and

corrective action taken.

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4.0 SAMPLING P R O C E D U R E SI '

The techniques and g u i d e l i n e s used to select the s a m p l i n g sites w i l l

I f o l l o w acceptable EPA procedures. The site selection protocol w i l l be

audited and approved by the Project QA Supervisor.

1

All procedures required for col lec t ing f ie ld samples , i n c l u d i n g the

use of appropr ia te s a m p l i n g procedures, prepared containers , preservat ion

techniques , chain-of-custody procedures,"-and documenta t ion pract ices , w i l l

f o l l o w acceptable EPA procedures. Preparation of an approved f i e l d

I s a m p l i n g p l a n and a sample site b r i e f ing package is required pr ior to

l e a v i n g on a f i e l d trip.

I

Prior to f ina l approval of the Work P l a n , the Project QA Superv i so r

w i l l perform a system audi t of the S a m p l i n g and A n a l y s i s P l a n , i n c l u d i n g

methods appendices for compliance with the study object ives. D u r i n g the

f i e l d effort, the Project QA Supervisor w i l l moni tor sample c o l l e c t i o n ,

| • check f i e l d notebooks and logsheets, and report any incons i s tenc ies and /o r

o m i s s i o n s to the F i e l d Team Leader.

I

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5.0 SAMPLE CUSTODY

The primary objec t ive of sample custody for th i s project is to create

an accurate writ ten ver i f ied record, which can be used to trace the

possession and h a n d l i n g of the samples from "the moment of c o l l e c t i o n

through data analyses and reporting. Adequate sample custody wi l l be

ach ieved by means of approved f ie ld and analy t ica l documenta t ion and

document control and review.

5.1 FIELD DOCUMENTATION

Sample col lec t ion for this project w i l l f o l l o w approved EPA

procedures. Sample labels (Figure 5-1) are prepared by the computerized

ESE data management system prior to f i e ld s a m p l i n g t r ips . All samples

collected in the f i e ld a r e - c o m p l e t e l y documented by the F i e l d Team Leader

u s i n g the sample custody logsheet shown in F igure 5-2.

F i e l d notebooks and copies of all logsheets w i l l be turned in for

r ev i ew by the Assis tant Project Manager for F i e l d I n v e s t i g a t i o n s at the

c o n c l u s i o n of each f i e l d t r ip . The F ie ld - 'Team Leader is respons ib le for

r e v i e w i n g and s i g n i n g al l f i e l d notes for completeness prior to l e a v i n g the

f i e l d . The Project QA Supervisor audi ts and counters igns al l f i e l d notes.

The F i e l d Team L e a d e r ' s log w i l l c o n t a i n a l l o f the i n f o r m a t i o n needed

to docurne.it when , where , and how the s a m p l i n g program was conducted .

5-2E.S.E, »79313400NORANDrt

SAMP* STAID.30100 SU-2

FRACT* CSAMPLESSAMP.DATE HRFGL- PRENTICE

30100 SU-2

10/10/7?

FLD.GPNQRA4

M

NORA4105-1PFS

E.S.E. >79313400MORANDA

SAMP* STAID.30100 SU-2

FRACT» CFSAMPLERSAMP.DATE HRFCL= PRENTICE

3-0100 SU-2

10/10/79

FLU.GPNORA4

MORA4105-1PFS

E.S.E. *79313400NORANDA

SAMP* STAID.30100 SU-2

FRACT- SSAMPLERSAMP.DATE HRFGL» PRENTICE

30100 SU-2

10/10/79

FLD.GP,MORA4

NORA4105-lfFS

E.S.E. *79313400- 10/10/79NQRANDA

SAMP* - STAID. FLD.GP30100 SU-2 HQRA4

FRACT= NSAMPLERSAMP.DATE HR MFGL» PRENTICE

30100 SU-2 NORA4103-1PFS

Figure 5-1SAMPLE LABELS

I At S i l l Ml ' f t 6 IM I K l U C .cmi.il c I N u r i i l H : •.•-r<yvi» s

I Gl U » H I 1,11 I I SI ItS A M . 1 » P f

> I A . i' ill I t

• Kin i re Mien rrr. t" i E X A M PN A M f : Q A A P P R A I f A L

Cl O( B A t ' l ' . ICA l L I ' C A I I O N UllhlN PHOJfCI A R I A < « « i :S l d F I I HAP • 110 OUT ( l A U : 7 / 2 W 8 J

S A H l ' . l Y I ' l S A M P . I V P f S A M P . I V P fS I A . ? M 20803

S « M P . I V H

INS C IJ ! f N ' C N f

11.11 ll.-l lAU II HI l,Alf IIMI OAU IIMf!

« ...,' S •)

y, • .

M A . ' ?f,e , ' MA . * ?cKh r ? A . * 0 ? r t t » ' ' IA.S 2 0 B C Br ti s c r s . r N r r w s

OAU IIMI I:AH IIMI t»'t MMI UAII IIMI

l1 I. n

2 ') hVI

s i A . f zinc ?.,HH z j e i z zoa isc n i t u •. c N ; r N s

UAH t in DAU IIK< ot ic \ \ t \ OAU linti ,

111 :?'/9

'J1

OIISI H V A 1 IONS e i S A H P L I R I H C C H A R i :

S A M i i t o (IT: c l ( i i v l f ) B Y : UAU/ I IM I :O R G A N I C Al IOK : C«G AKI / A 1 1 OK' :

HI 1 1 MIDI SHI II ll>: K f C M V C b till O A l f / I I M f :( i H G A N i ^ A i ION: O R G A N I / A I ION:

HI 1 INUL'ISHI U 1: > : H M I I V t f l FOR I ADIIR A I (IN Y I' Y : OAI f / l l ' < f :O M G A N I {* 1 ION: nRG A N I 7 A I ION :

C II S

U A T I K \ f fF CPh SUU.O.PRI) MC/l

CONO UMMO/CH

c IA.b ittfl *>

C H S

OAU IIMI

UAIIR IfMP CPh SUD.O.PRH MC/lrONii uMHo/cn

?'»MC M S

DAU IIMlUAII R IfMP CPH SUII. 0. PUB MC/LCONO UMHO/CH

HI I I K I U 01 M l l I ' M I Nl :

Figure 5-2FIELD CHAIN OF CUSTODY LOGSHEET

CM

I

000802

GC

At a minimum, the Field Team Leader's log will contain:

1. Sampling instructions;

2. Site name and location;

3. Names of field team members assisting in the Campling effort;

4. Sample numbers;

5. Collection dates and times;

6. Descriptions of sample fractions and preservation;

7. Date, time, and method of sample shipment;

8. Sketches and descriptions of all sample points; and

9. All field team sampling notes and calculations.

5.2 ANALYTICAL DOCUMENTATION

Sample analyses for, this project will be performed in the certified

analytical laboratory. Sample custody procedures for sample analysis will

follow the approved EPA procedures.

The computerized laboratory data management system is an integral part

of the sample custody procedure for all sample analyses performed at. the.

analytical laboratory. Figure 5-3 summarizes the role of the data

management system for ensuring sample analysis integrity.

The Project QA Supervisor will frequently monitor samole log-in; check

pertinent logsheets, tracking- forms, and data input- computer forms; and

report any sample custody inconsistencies to the Project Manager.

5-5

o

Field TripPreparation

Sample Log-In

Information onAnalysis Neededto be Performed

TAssign Analysis

Input AnalysisResults

IncersampleQuality Control

ACTIVITIES

Define parameters for. analysis.Assign temporary station codes.Define sample fractions.Produce sample labels and logsheets.

Set permanent station codes.Specify samples which vere actually collected,Store collection time and date.Store holding time notifications.Activate samples in system.

Comprehensive list of all parametersrequested for analysis and a list ofsamples available for each parameter

Reserve "batch" of sample numbers foran analysis.Set status for the sample-parametercombination to "in the lab".

Generate calibration curve.Perform quality control checksCalculate sample results.Store final data.

Check for data inconsistencies

ReportingFinal Data

Produce a data report listing concentrations,.status, and optionally the batch controlnumber.

Figure 5-3FLOW CHART OF INTERACTIVE SAMPLE ANALYSIS

AND RECORDING SYSTEM (ISARS)

5'6 £DC

5.3 DOCUMENT CONTROL AND REVIEW .3

The tern document control includes the maintenance of project fi les.

All project files will be maintained by the Project Manager and Ass is tan t

Project Managers. All project documents will be kept in project f i les.

Project personnel may keep their own files; however, all official and

original documents will be placed in the official project fi le according to

the fil ing system shown in Figure 5-4.

The Project QA Supervisor will review the project file periodically to

ensure that it is complete and that the chain of custody is documented

completely from the moment of collection through analysis and final

disposit ion of samples.

The Project QA Supervisor will independently maintain a QA file for

this project. At the end of the project, the QA project fi le will be

turned over to the Project Manager. The fol lowing documents will be placed

in the QA project file:

1. QA records maintained throughout the invest igat ion;

2. Documentation of QA system and performance audits;

3. Documentation of all unusual findings or observat ions;

4. Documentation of all QA corrective actions;

5. All official QA correspondence received or issued relat ing to

the invest igat ion, including records of teleonone c a l l s ;

5. One copy of all QA del iverable review sheets; and

7. Any other QA documents related to the project or fol lowuo

act iv i t ies related to the investigation.

5-7X

1.0 PROPOSAL

2.0

1.11.21.31.41.51.6

RFPRFP APPENDICESPROPOSALAPPENDICES TO PROPOSALSPROPOSAL APPROACHNEGOTIATIONS

PROJECT ADMINISTRATION2.12.22.32.42.52.62.7

CONTRACTPROJECT INITIATION DATASUBPROJECT BUDGETSESE PURCHASE ORDERSESE INVOICESPROJECT PROJECTIONSCOMPUTER PRINTOUTS

2.7.1 JAN 83 COST REPORTS2.7.2 FEB 83 COST REPORTS2.7.3 MAR 83 COST REPORTS2.7.4 APR 83 COST REPORTS2.7.5 MAY 83 COST REPORTS2.7.6 JUN 83 COST REPORTS2.7.7 JUL 83 COST REPORTS2.7.8 AUG 83 COST REPORTS2.7.9 SEP 83 COST REPORTS

3.0 CORRESPONDENCE

3.13.23.3 .3.43.5

TO LAN/HLATO ESESTATE LETTERSOTHERSMONTHLY STATUS

3.5.1 JAN 833.5.2 FEB 833.5.3 MAR 833.5.4 APR 833.5.5 MAY 333.5.5 JUN 333 .5 .7 JUL 833.5.3 AUG 333.5.9 SE? 83

REPORTS-

STATUSSTATUSSTATUSSTATUSSTATUSSTATUSSTATUSSTATUSSTATUS

4.0. IN-HOUSE MEMOS

'4.1 MEMOS4.2 TELEPHONE CALLS

5.0 GRANTS AND REGULATIONS

5.1 TDWR GRANTAPPLICATION

5.2 TEXAS WATER QUALITYREGULATIONS

5.3 FEDERAL WATER QUALITYREGULATIONS•

5.4 CERCLA NOTES

6.0 FIELD AND ANALYTICAL DATA

6.1 MICROFICHE6.2 WELL INVENTORY DATA-

LAN6.3 FIELD TRI? NOTEBOOKS6.4 WELL LOGS—HLA6.5 CHEMISTRY DATA6.6 DATA I N T E R P R E T A T I O N

7.0 ESE REPORTS

7.1 SAMPLING AND ANALYSISPLANS

7.2 DATA MANAGEMENT =LANS7.3 QUALITY ASSURANCE

PLANS7.4 SAFETY PLANS7.5 DRAFT REPORT7.5 FINAL REPORT

8.0 MAPS AND PHOTOGRAPHS

8.1 MAPS8.2 PHOTOGRAPHS

Figure 5-4. PROJECT FILING SYSTEM

5-1 §

6.0 CALIBRATION CONTROLS AND FREQUENCY

Calibration controls will be required for analytical operations of

this project. Each instrument will be calibrated in a manner consistent

with EPA calibration protocols where specified for the individual methods.

Calibration will be documented in the instrument logbook and/or parameter

notebook. The Project QA Supervisor will verify the calibration curves,

identify any problems with the calibration procedure, and initiate the

proper corrective action, as needed.

6.1 GENERAL CALIBRATION PROCEDURES

For all methods, a minimum of three calibration standards at different

concentration levels for each parameter of interest will be prepared by

adding volumes of one or more stock standards to a volumetric flask and

diluting to volume with the appropriate solvent. The stock standard

solutions are prepared by dissolving precise amounts of standard materials

of known purity in an appropriate solvent. Standard EPA reference

materials will be used as the primary standard whenever possible. The

concentrations of the calibration standards will correspond to the expected

concentration range of the analyte in the samples and will bracket the

sample concentration range.

A calibration curve will be prepared from the results of tabulated

peak heights or area responses against the concentration. Alternately, if

the ratio of response to amount injected (response factor) is a constant

oo

CO

6-2 8

over the working range [<10-percent relative standard deviat ion (RSD) ] , the

average response factor can be used in place of a calibration curve.

Analytical balances are calibrated on a routine basis with a set of

certified weights. Records of analytical balance calibration are kept in

the balance logbook.

6.2 GAS CHROMATOGRAPHY (GC)

A fresh calibration curve will be prepared daily. If a response

factor is used, its value will be established and verified on a daily

basis. For GC analyses, the working calibration curve or response factor.

will be verified each working day by running one check calibration standard

periodically during a run, but no less than once every 15 samples. If the

response or response factor for any analyte of the check calibration

standard varies from the expected value by more than +20 percent, the test

must be repeated using a fresh calibration standard. Continued variation

by more than +_20 percent requires that a new calibration curve be prepared

or a new response factor determined.

Calibration of GC gas flow rates will be conducted periodically during

the course of the analytical runs, but at a minimum must be checked when

the instruments are initially set up for a specific analysis. Gas flow

rates are measured using a soap bubble flowmeter.

6-3

6.3 GC/MASS SPECTROMETRY (GC/MS)

The calibrati-on procedure for GC/MS determinations is s imi lar to the

general cal ibration procedure, except that relative response factors (RF)

for the individual compounds will always be used where:

RF . Vc •

where: A = Integrated area taken from the extracted ion current

profile,

Q =» Quantity of material,

c » Compound, and

s = Standard.

A minimum of three compound levels, covering a significant portion of

the linear range of the instrumental determination, will be employed to

determine the instrument sensitivity, i.e., response per unit quantity of

compound. The resultant slope from the least squares of the cal ibrat ion

data will be employed to calculate the relative response factor as:

R = ( s l o p e ) / ( A s / Q s )

A 1- point calibration will be employed daily for all subsequent work

to maintain the instrument response within 30 percent of the original

ca l ib ra t ion.

ooe

6-4

Daily GC/MS instrument control will be practiced to ensure that the

instrument is calibrated and in proper working -condition. The GC/MS will

be tuned daily with perfluorotributyl amine (these outputs are contained in

the instrument tuning log), and it- performance will be monitored with a

reference compound such as decafluorotriphenylpnosphine and/or with a

composite mixture of compounds representative of the samples being

analyzed. An instrument tuning log is maintained to flag any deterioration

of instrument performance.

The specific compounds will be monitored to confirm that their

fragmentation patterns remain consistent, and to ensure uniform sensitivity

specific ions representing the mass range to be scanned will be selected

from these compounds and quantitated by integrating the peak area of their

respective extracted ion current profiles. The applicable internal

standards will be added to this mixture and will serve as the standard for

quantification.

Each fraction to be analyzed on the GC/MS will be spiked with internal

standards at a concentration consistent with the particular fraction. For

most extracts, the concentration is expected to range from 50 to

100 nanograms.

5.4 INDUCTIVELY COUPLED ARGON PLASMA SPECTROMETRY (ICAP)

A fresh 2-point standardization will be performed daily at a minimum

on the spectrometer to correct for fluctuations. The standardization will

6-5 —

DC

be verified each working day by running one check reference standard

periodically during the run, but no less than once every 20 samples. If

the check reference calibration standard concentration varies from the

expected value by more than +5 percent, a fresh standardization must be

initiated and verified.

rl

7-1

7.0 ANALYTICAL PROCEDURES

The analytical procedures used for this project are presented in

Table 3-1. Within the flow of the project scheme, the Project QA

Supervisor will monitor sample log-in, proper dispensing of samples, and

batching the samples into analytical runs to ensure that the proper

analytical methods are being used.

Any diff icult ies encountered in adhering .to the approved analytical

procedures will be reported by the appropriate Subproject Manager to the

Project QA Supervisor and the proper' corrective action implemented.

JO

8-1 O

8.0 DATA REDUCTION, VALIDATION, AND REPORTING

Data transfer and reduction are essential functions in summarizing

information to support conclusions. It is essential that these processes

are performed accurately and, in the case of data reduction, accepted

statistical techniques are used.

At a minimum, example calculations must be included with the

summarized data to facil i tate review. The entry of input data and

calculations should be checked and the signature/initials of the data

technician and reviewer(s) accompany all data transfers with and without

reduction.

An example data sheet (Figure 8-1) for this project will involve

reporting standard curves, QC data, and sample data. All data must be

final approved by the Project QA Supervisor before releasing the data to

the client.

Sample response data information will be sent to the Laboratory Data

Assistant for computer entry. The Laboratory Data Ass is tant will enter the

information from the batch form into the computer, which will calculate:

1. Quadratic regression line for standards,

2. Coefficient of variat ion for replicates,

3. Spiked recoveries,

4. Reference sample concentrations, and

5. Sample concentrations.

3-2BATCH t 10014 ANALYST NAME- BARBARA WEEKS

CO

ANALYSIS DATE SETUP DATE" 01/27/83ANALYSIS TYPE • 1 0-CURVE+EXTRACT 1-CURVE*«ATER 2-MANUAL WATER 3"MANUAL EXTRACTPROJECT NTJKSE2. 8ZMZWJO STARTS WITH SAKPLE * 20900

1. 72000 CYANIDE ( H C / L ) NO SPOCE DILUTION E3TECTAVERAGE RECOVERY- 100.00 » OR - 15.00 PRECISION CRITERIA- 13.200: * OR - DET.UMT.

CALIBRATION DATA

QUALITY CONTROL

#SP!XES REQUIRED- 1 ^REPLICATES REQUIRED-

SPIKE QCSPITE COCZTAIL CONCEHTRAT10SS

72000. _SAMPLE t SAMPLE PORTION SPIKE PORTION

SAMPLE SAMPLE PORTION SPIKE PORTION

QC SAMPLE RESPONSES

72000QC SAMPLE* 4 TYPE CYANIDE (MG/L)

1.

REFERENCE SAMPLE # DILUTION RESPONSE

If A BATCH # AND CONCENTRATION ARE PRINTED IN THE ENTRY SPACETHEN THE VALUE HAS ALREADY Btifl RtbiSVED FOR YSZ 3ATC3 # INDICATED

72000CYANIDE (MC/U

1. 20900

Figure 8-1DATA INPUT FORM

8-3

The following quadratic equation will be used to calculate final data in

the laboratory for analysis requiring a calibration curve:

Concentration = Intercept + M * Response + M2 * Response**2

The following equations will be used to calculate a quadratic

regression:

Denominator = N*(AB2*AB4-AB3**2)+2*AB*AB2*AB3-AB2**3-(AB**2)*AB4

Intercept = (CQ*(AB2*AB4-AB3**2)+COAB*(AB2*AB3-AB*AB4}+

AB2CO*(AB*AB3-AB2**2))/Denominator

M = (N*(AB4*COAB-AB3*AB2CO)-AB*AB4*CO+AB2*(AB*AB2CO+AB3*CO-

AB2*COAB))/Denominator

M2 = (N*(AB2*AB2CO-AB3*COAB)+AB*(AB2*COAB+AB3*CO-AB*AB2CO)-

(AB2**2)*CO)/Denomi nator

Correlat ionCoefficient = (M*(N*COAB-AB*CO)+M2*(N*AB2CO-AB2*CO))/(N*C02-CO**2)

where:

M - Coefficient,

-M2 a Coefficient,

AB = Sum(absorbances),

AB2 = Sum(absorb. **2),

3-4ooC

AB3 = Sum(absorb. **3),

ABA = Sum(absorb. **4),

CO = Sum(concentration),

C02 = Sum(conc. **2),

COAB = Sum(conc. *absorb.),

AB2CO = Sum(absorb. **2 * cone.), and

N s Number of standards.

Precision and accuracy criteria for acceptance of data will be derived

from EPA precision and accuracy data for standard EPA methods and from the

data presented in Table 3-1. The QC criteria will be stored in the

' computer data management files for each STORE! number and different method

used for a STORET number.

After the computer calculates the QC checks, the Laboratory Data

| Assistant will route the completed batch information to the Chemistry

Discipline Manager and Project QA Supervisor for final approval.

IThe completed batch forms will be stored in files arranged numerically

' by batch number. Strip charts, copies of parameter notebooks, -and QC

i charts will be stored for each parameter in a project notebook.

When the data are complete for an experiment, the computer will

organize the information in the field group. The conclusions for the final

report will depend on the information from the data.

8.1 OUTLIERS

O u t l i e r s in the f i e l d laboratory and m a i n labora tory generated data

w i l l be determined u s i n g the D i x o n Cr i t e r i a as described in the

EPA-qAMS-005 document and in "Processing Data for O u t l i e r s , " by W . J . D i x o n ,

Biomet r ics , V o l . 9, No. 1, 1953.

8.2 DATA V A L I D A T I O N

The Project QA Supervisor w i l l randomly select 10 percent of the data

generated in the f ield and m a i n laboratory for v a l i d a t i o n pr ior to

repor t ing the data. The v a l i d a t i o n process w i l l i n v o l v e t r ac ing a data

p o i n t back through the c a l c u l a t i o n s , chromatograms and/or str ip charts,

laboratory notebooks, extract ion. logs, sample checkin , and f i e l d s a m p l i n g

logs. The. f i n d i n g of suspect data in the samples selected w i l l necessitate

a more thorough e v a l u a t i o n of the data by the QA Supervisor to ensure that

o n l y v a l i d data are reported.

9-1

9.0 INTERNAL QC CHECKS

Responsibility for internal QC checks rests with the Analyt ical Team

leader at the analytical laboratory. 'The Project QA Supervisor will

monitor the performance of the analysts 'and-the Analytical Team Leader for

implementation of proper QC checks and to final approve all data.

For analysis conducted in the analytical laboratory, the fol lowing QC

checks will apply:

1. At least three standards for standard curve,

I 2. Correlation coefficient for curve is greater than 0.995,

3. Percent recovery for spikes is within criteria,

* 4. Samples are within range of standards,

S. At least 10 percent of the samples are replicates, and

I 6. At least 5 percent of the samples are spiked.

For data generated in the analytical laboratory, the acceptance

1 criteria for precision and accuracy are determined as fo l lows:

* =• V ± 3p

i where:l

TT a Average percent recovery from spiked sample data during the

run,

7T' = Average percent recovery for the particular anaiyte as obtained

from Table 3-1, and

p = Standard deviation (expressed as percent) for the part icular

anaiyte as obtained from Table 3-1.

oc

oc

oc10-1 O

10.0 PERFORMANCE AND SYSTEM AUDITS

Two types of audit procedures will be used by QA to assess and

document performance of project staff—system audits and performance

audits. Thase are performed at frequent intervals under the direction of

the Project QA Supervisor. These audits form one of the bases for

corrective action requirements and constitute a permanent record of the

conformance of measurement systems to QA requirements.

System audits are inspections of training status, records, QC data,

calibrations, and conformance to standard operating procedures (SOPs)

without the analysis of check samples. System audits will be performed

periodically on laboratory, and office operations or on field operations.

The development and approval of the Work Plan constitutes the initial

system audit for this study.

The systems audit protocol is summarized as follows:

1. Field Operations—The Project QA Supervisor will check:

a. Field notebooks, logsheets, and tracking forms, and report

any inconsistencies and/or omissions;

b. Field sampling plans; and

c. Sample site briefing package.

2. Laboratory Operations — The Project QA Supervisor will check:

a. Parameter and/or laboratory notebooks;

b. Instrument logbooks;

c. Sample log-in, dispensing, and label ing for analys is; and

10-2oricc

d. Final approval of data from each sample lot.

In addition, the Project QA Supervisor will monitor all

experiments to assure complete adherence to the approved

analytical methods as detailed in Table 3-1.

3. Final Reports—The Project QA Supervisor will review all final

reports and deliverables to the client.

Performance audits will include evaluation and analysis of two types

of check samples. A performance evaluation sample from EPA will be

analyzed periodically along with the regular samples.

In addition, ESE routinely participates in performance test sample

programs administered by:

1. EPA, Environmental Monitoring Support Laboratory (EMSL)-Cincinnat i

(d);

2. EPA, EMSL-Research Triangle Park (RTP) ;

3. EPA, Region IV;

4. Florida Department of Environmental Regulat ion ( D E R ) ;

5. Florida Department of Health and Rehabi l i tat ive Serv ices;

6. Alabama Department of Health;

7. U.S. Army Corps of Engineers, South At lant ic D i v i s i on ; and

3. American Industrial Hygiene Assoc ia t ion (AIHA) (ESE is an AIHA-

accredited laboratory).

The results of these inter!aboratory studies will be periodically

evaluated by the Project QA Supervisor during the project as part of the

performance audits.

Peer review of all deliverable reports and data supporting this

project will be performed by the Discipl ine Managers, Project Manager,

Assistant Project Manager(s), Project QA Supervisor, and by selected

members of the Technical Review Committee. Proper protocol for peer review

within each discipline or technology area specifies review and/or approval

of a draft deliverable or portions of a deliverable by the Discip l ine

Manager. The Project QA Supervisor, with or without review, approves each

document, based on an audit of the discipline review. If the document is

not approved, -it is returned to the author for revisions, and then

resubmitted. After Project QA Supervisor approval, the document is reviewed

or audited by the Assistant Project Managers and the Project Manager.

After approval, the document may be released.

Clri

11-1

11.0 PREVENTIVE MAINTENANCE

To minimize the occurrence of instrument failure and other system

malfunction, a preventive maintenance program will be implemented. The

mpjor analytical instruments used in this study will be spectrophotometers,

total organic carbon (TOG) analyzers, total organic halogen (TOX)

analyzers, GC, GC/MS, and ICAP. In addition, analytical balances will c-e

employed to provide accurate standard weights. The preventive maintenance

performed for each is as follows.

11.1 GAS CHROMATOGRAPHS

GC septa w i l l be replaced on a weekly basis or more frequently as

needed when symptoms of septum deter iora t ion are noted. Frequent

in jec t ions w i l l require replacement on a d a i l y basis . Carr ier and detector

gases w i l l be changed, when the supp ly of gas in the cy l inders f a l ' l s below

100 pounds per square inch ( p s i ) , to prevent contaminants from reach ing the

detector or columns. M o l e c u l a r sieves and oxygen traps used in the gas

l i n e s w i l l be replaced on a regular basis. GC detectors w i l l be

p e r i o d i c a l l y removed and c leaned to remove a c c u m u l a t i o n s , w h i c h can affect

ins t rument performance. Instrument c a l i b r a t i o n curves w i l l be mon i to red

and compared to h is tor ica l performance cr i ter ia . . E x c e s s i v e n o i s e , low

response, and poor p rec i s ion are indica tors of a di r ty detector and may

cause more frequent detector c l e a n i n g . Spare co lumns , pack ing m a t e r i a l s ,

i n s t r u m e n t c a b l e s , and PC boards w i l l be a v a i l a b l e in case of b r eakage or

m a l f u n c t i o n t o m i n i m i z e ins t rument down t ime .

11-2

11.2 GC/MS

All routine preventive maintenance performed for gas chromatographs

also will be performed for the GC/MS equipment. In addition, the ionizing

source will be periodically dismantled, thoroughly cleaned, and reassembled

to prevent serious sensitivity problems. Calibration with selected mass

standards will be performed on a daily basis to ensure that instrument

performance has not deteriorated. The failure to achieve calibration will

require source cleaning procedures to be implemented. Spare parts and

equipment will be available for the system components most likely to

experience failure. Routine maintenance by the manufacturers'

representatives will also be performed on an annual basis.

11.3 TOC ANALYZERS

The sensitivity of the TOC analyzer will be monitored to assure

compliance with historical performance. Combustion tubes will be replaced

on a regular basis, the frequency depending on the extent of instrument

use. Spare parts will be available for the inlet ports, combustion tubes,

packings, and IR source.

11.4 ICAP

Routine maintenance on the Jerri l l-Ash ICAP system by the

manufacturer 's representatives is performed on -an annual bas is . ' In

addit ion, a quarterly serv ice contract is maintained on the minicomputer.

11-3

Periodically, the analyst will dismantle, clean, and reassemble the

torch and nebulizer to prevent serious sensitivity problems. Calibration

with selected standards will be performed daily to ensure that the

instrument performance has not deteriorated. The failure to achieve

standardization could require cleaning, including changing the tubing of

the sample delivery system. Spare parts are available for the system

components most likely to experience failure.

11.5 TOX. ANALYZER

Proper maintenance of the adsorption module and the microcoulometric

analyzer is essential. Reservoirs, switching valves and plumbing, granular

activated carbon (GAC) columns, and column housings will be cleaned

routinely and/or replaced as needed. The inlet tubes and POX sparger

may need cleaning on a weekly basis if usage is frequent. Spare parts such

as 0-rings, tubing, septa, and GAC columns will be available for the system

components most likely to experience failure.

11.6 SPECTROPHOTOMETERS

The sensitivity of the spectrophotometers will be monitored to ensure

compliance with historical performance. The sampling system and air

filters will be checked regularly and cleaned and/or replaced as needed.

Spare parts and equipment will be available for the system components most

l i k e l y to experience failure.

<Nooo

11-4

11.7 A N A L Y T I C A L BALANCE

A n a l y t i c a l ba lances w i l l be cleaned and c a l i b r a t e d on a yearly bas i s

by m a n u f a c t u r e r s ' representatives. M o n t h l y , the accuracy of a n a l y t i c a l

balances w i l l be compared to standard weights.

12-1

12.0 PROCEDURES USED TO ASSESS DATA PRECISION, ACCURACY, AND COMPLETENESS

Data accuracy and precision will be assessed for each measurement

system and each sample lot using a known EPA reference sample analyzed

periodically and/or samples spiked at a known level. The percent recovery

(R) will be calculated as:

100*(Spike Sample Cone. ) (Sample+Spike Vo l . )R = _ -(Sample .Vol .) (Sample Cone.) _

(Spike Conc . ) (Sp i ke Vo lume)

The following equation is an example of how this would be calculated:

1 ml of spike with concentration of 100 ppb10 ml of sample with concentration of 10 ppbspiked sample concentration of 20 ppb

. „». ( " " ' 1 0 ' • 100. • 120 percent

The recovery of the sample will then be compared to the method

accuracy and precision acceptance criteria, as determined from the data in

Table 3-1. If the recovery does not fall within the control l imits for

method performance:

Upper Control Limit (UCL) = R + 3S

Lower Control Limit (LCL) = R - 3S

Where S is the standard deviation of the percent recovery

n n ?I R/ - ( 2 R.) /

__lfi_

12-2 jso

then the results reported in all samples processed as part of the same set

must be qualified and the analytical method and data carefully evaluated.

Sample analyses may need to be repeated.

The Project QA Supervisor will final approve and validate all data

before submitting the final data to the client.

GOr)

13-1 22

13.0 CORRECTIVE ACTION

R a p i d , e f fec t ive , and thorough means of imp lenient ing the correct ion of

QA problems and for noncomply ing items, as well as f o l l o w u p reports, are

essential to the implementa t ion of a m e a n i n g f u l QA program. The two major

types of corrective actions, immediate and long-term, both require

appropriate documentation. Problems requir ing immediate r e so lu t ion such as

ins t rument m a l f u n c t i o n or unexpected f ie ld condi t ions are documented f u l l y

in f i e l d data books or instrument logs and are covered under normal

operat ing procedures for all d i s c ip l ines .

Corrective action may also be req-uired to correct noncomply ing items

or systematic errors. Management must apply a systematic corrective act ion

to e l iminate such long-term problems. The Project QA Supervisor w i l l

assist the Project Manager in imp lemen t ing the process of s c h e d u l i n g ,

pe r fo rming , documenting, and ensur ing the effectiveness of the ac t ion . Such

ac t ion may consist of personnel r e t r a i n i n g or removal from a project ,

r e a n a l y s i s of ques t ionable data, instrument replacement, or improved

s a m p l i n g procedures. The Project QA Superv isor , af ter c o n s u l t a t i o n w i th

the Project Manager and Project Director , has "stop work" au tho r i t y for

project ac t iv i t i e s wh ich -a r e judged out of control and can require

r e s a m p l i n g or a n a l y s i s to br ing data items into c o m p l i a n c e .

12.1 P R O B L E M I D E N T I F I C A T I O N

U p o n n o t i f i c a t i o n of a problem or when a po ten t i a l p rob lem is

i d e n t i f i e d th rough any a u d i t i n g procedure, the Project QA Supe rv i so r then

00

13-2 ' X

n o t i f i e s the Project Manager and Project Director . Together, the Project

Manager and QA Supervisor perform a br ief , but . thorough, i nves t iga t ion of

the reported problem immediately to determine if a corrective ac t i on

request is required and should be f i l e d .

R e v i e w of the F i e l d Trip P l a n , for example, may iden t i fy a po t en t i a l

problem to which an immediate so lu t ion may be a p p l i e d , thereby a l l e v i a t i n g

the necessity for a formal corrective action request.

Corrective actions may be ini t ia ted for each measurement system

( i n d i v i d u a l d i s c i p l i n e s ) by the D i s c i p l i n e Managers. The Project QA

Supervisor, a l o n g with the Project Manager, w i l l be responsible for

app rov ing the corrective action in the same fash ion as if it had been

in i t i a t ed as a project QA function.

13.2 FOLLOWUP PROCEDURES

Adequate fo l lowup procedures are provided for ei ther type of

corrective action since these actions are not considered complete u n t i l the

problem has been effect ively and permanently solved.

A corrective action request form is used to document all long-term

corrective actions taken. The form may be i n i t i a t e d by any i n d i v i d u a l who

observes a p rob lem on a speci f ic n o n c o m p l y i n g item; each form is l i m i t e d to

a s i n g l e problem. If more than one problem is i n v o l v e d , each prob lem

s h o u l d be documented on a separate corrective act ion request form. Cop ie s

13-3

of the form are given to the Discipline Manager and the QA Supervisor. The

Project Manager, Project QA Supervisor, and Discipline Manager discuss tne

problem jointly to:

1. Determine that specific corrective action is needed to elimi-

nate the problem and assign responsibility for investigating,

implementing, and documenting the situation;

2. Determine when the system became out of control;

3. Set a time schedule for determining the required action;

4. Assign responsibility and time schedule to implement the

required action;

5. Establish desired effectiveness of the corrective action and

implement the correction; and

6. Verify and document that the corrective action has eliminated

the problem.

The Project QA Supervisor has the authority to require measurements

that are compromised to be discontinued or limited until corrective action

is complete and data quality is no longer questionable. The QA Supervisor

also may order the re-analysis of samples or measurements occurring since

the documented evidence that the system was in control. Figure 13-1 shows

the project corrective action form.

For this project, project-specific corrective actions will be

documented to the Project Manager. The Project QA Supervisor will assist

13-4 _rO00

QUALITY ASSURANCE CORRECTIVE ACTION RZQUTSTAMD ROUT INC FORM

1. Identif ication of a Proble

N«tUt« Of V f f i t t t m m -

CA* .

2. Determination of Required Action:

R«ipoo<ibi l icy Aaiigncd "*•

t" >•'""•

Ou* D«ce:.

3. laplementicion of Required Action:

Responsibility Aj«ign«d "••

A. Aouriag Ef fcctivenes* of Action:

Responsibili ty Ajsigned tn-

Procedure to Ajiure

Due Date:

Due Date:

Figure 13-1QUALITY ASSURANCE CORRECTIVE ACTION

REQUEST AND ROUTING FORM

oc13-5 O

the Project Manager to define responsibilities for scheduling, performing,

documenting, and ensuring the effectiveness of-the required actions.

Ultimate disposition of any corrective action will be by formal

notification to the project management staff and will become a part of the

permanent project records file.

QA may issue a corrective action for circumstances other than audit

nonconformances. If, in the opinion of the QA staff, for example, members

of the project team other than the individual disciplines (i.e., project

management) have been negligent and/or nonresponsive to information need

requests, a need for corrective action may result. As in the case of audit

nonconformance, the corrective action is not complete until.a satisfactory

resolution is achieved.

S3

14.0 QA REPORTS TO MANAGEMENT

This Project QA Plan provides a documentable mechanism for the

assurance of quality work products. This section provides for periodic

reporting to management at all levels on the performance of measurement

systems and data quality. The Project QA Supervisor will be responsible

for this reporting activity.

14.1 REGULAR REPORTING

The Project QA Supervisor will report the QA activities of each month.

This reporting will normally consist of a regular assessment of measurement

data accuracy, precision, and completeness as well as the formal status of

any performance and system audits conducted during the intervening period.

Significant problems identified and their solution status wi.ll be

reported, and the project QA Corrective Action Status Form (Figure 14-1)

will be updated.

14.2 NONREGULAR REPORTING

Potential problems which arise between regular project meetings may be

identified to management on a nonregular basis. Notation of the problem

will be in a memorandum, and investigation of the problem wil l commence

immediately. This action is in addition to any formal actions taken and

reported under regular reporting.

aa of (Date):

CJJ Brief Deacription

OriginatorInitial*and Date

Pe termination and ImplementationInitials Due Date Initial* Due Date [to Date "Poke" Date

Effectiveness

Figure 14-1QUALITY ASSURANCE CORRECTIVE ACTION

STATUS FORM

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