sdms docid 2009027 bbi - united states environmental

SDMS DocID 2009027

BBIBLASLAND. BOUCK & LEE, INC.e n g i n e e r s & scientists

Transmitted Via U.S. Mail

December 5, 2002

Mr. Matthew MellonU.S. Environmental Protection AgencyHazardous Site Cleanup Division (3H S23)1650 Arch StreetPhiladelphia, PA 19103-2029

Re: Former Koppers Company. Inc.Newport. Delaware SiteBBL Project #: 388.27.005

Dear Mr. Mellon:

In a November 25. 2002 email, the United States Environmental Protection Agency (U.S. EPA) requestedtwo copies of both the January 1994 Quality Assurance Project Plan (QAPP) and the October 2002Sampling and Analysis Plan Addendum, for the Site. The requested documents are enclosed.

Please call with any questions.

Sincerely.

BLASLAND. BOUCK & LEE. INC.

Stuart D. MesSurVice President

KJ/dmn

Enclosures

cc: Jane Patarcity, Beazer (without enclosure)Maryann Nicholson, DuPont (without enclosure)

59221550.doc A R 3 I 1 3 0 7

REVISION NO. 1

NEWP Odfez,•*-

QUALITY ASSURANCE PROJECT PLANREMEDIAL INVESTIGATION/FEASIBILITY STUDYFORMER KOPPERS COMPANY, INCNEWPORT SITE

January 31, 1994

For:

U.S. Environmental Protection AgencyRegion 3841 Chestnut StreetPhiladelphia, Pennsylvania 19107

Prepared for:

Beazer East, Inc.436 Seventh AvenuePittsburgh, Pennsylvania 15219

and

Du Pont ChemicalsRoom 122281007 Market StreetWilmington, Delaware 19898

Woodward-Clyde 4r

Prepared by:

Woodward-Clyde Consultants5120 Butler PikePlymouth Meeting, Pennsylvania 19462

Project No. 91C2628-3X2

1 1 5 0 0 K-TRPT-0002259

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A R 3 I 1 3 0 9

Woodward-Clyde FEB04t«flConsultants 4

Engineering & sciences applied to the earth t. its environment

January 31, 199491C2628-1

Mr. S. Andrew SochanskiU.S. Environmental Protection AgencyRegion III841 Chestnut BuildingPhiladelphia, Pennsylvania 19107

Re: RWP, FSP, QAPjP, and HASPFormer Koppers Company, Inc., Newport SiteNewport, Delaware

Dear Mr. Sochanski:

On behalf of Beazer East, Inc. (Beazer) and E. I. DuPont de Nemours and Company,Inc. (DuPont), Woodward-Clyde Consultants (WCC) are submitting 8 copies of theRevised Work Plan (RWP), Field Sampling Plan (FSP), Quality Assurance Project Plan(QAPjP), and Health and Safety Plan (HASP). In addition, two copies are being sentdirectly to the Delaware Department of Natural Resources and Cpnservation (DNREC).These plans have been revised due to comments presented by the U. S. EnvironmentalProtection Agency (EPA) in the August 24, 1993 comments letter. Beazer and DuPonthave addressed the issues presented in the referenced letter, as resolved at theDecember 15,1994 meeting and summarized in the January 3, 1994 letter from the EPA_The RWP, FSP, and HASP are complete copies. However, as agreed at theDecember 15, 1993 meeting, only two complete copies of the QAPjP have been sent toyou; all other copies of the QAPjP exclude sections of the plan that were not revised(Appendices A, B, C, E, and F). We request that the recipients of incomplete copiesof the QAPjP replace the former sections in the plan binders with the enclosed revisedsections, and discard the supplanted sections.

A summary table has been supplied with each of the plans to guide the reader to thesection and page where revisions have been made relative to the EPA comment. Pleasenote that some revisions were made based on discussions at the meeting that were notpresented in the January 3, 1994 summary letter. These have been noted on the table.To further facilitate your review of the plans one copy of the text of each of the planshas been marked to show deletions of former text (cross-outs) and insertions of new text(underlines), and is included with this submittal. In addition, in response to a commentmade on the QAPjP, a recent performance evaluation conducted on Wadsworth/AlertLaboratories, of Pittsburgh, Pennsylvania, has been submitted to you with these plans.

91C2628-I/PLANCOV.LTR/KPR4 01-31-94

5120 Butler Pike • Plymouth Meeting, Pennsylvania 19462215-825-3000 • Fax 215-834-0234

A R 3 I I 3 I O

Woodward-ClydeConsultants

Mr. S. Andrew SochanskiU.S. Environmental Protection AgencyJanuary 31, 1994Page 2

Regarding wetland delineation, the Revised Work Plan (June 23, 1993) provided thatBeazer and DuPont would utilize the Corps of Engineers Wetlands Delineation Manual(U.S. Army Corps of Engineers, Technical Report Y-87-1) ("1987 Manual"), which theJanuary 1993 Corps of Engineers - EPA Memorandum of Agreement requires to be usedfor wetlands delineation. In its August 24, 1993, comments on the Revised Work Planletter, EPA stated that the "Federal Manual for Identification and Delineation ofJurisdictional Wetlands" (Federal Interagency Committee for Wetlands Delineation,1989) ("1989 Manual") must be used for wetlands delineation for risk assessment. Atour December 15 meeting, Beazer an DuPont proposed performing wetlandsdelineations using both manuals. In its January 3, 1993 letter, the Agency advised thatboth manuals may be used but that EPA would use the 1989 manual to delineatewetlands for risk assessment. It is Beazer's and DuPont's understanding that thedelineation based upon the 1989 Manual will not be used for any other purpose,including, but not limited to, Jurisdictional delineation, and that the delineation basedupon the 1987 Manual will be used for such purposes. We reserve our right to invokedispute resolution with respect to the use of delineation based on the 1989 manual forany purpose, including, but not limited to risk assessment.

We look forward to progressing with this program. If you have any questions that willfacilitate your review, please do not hesitate to call.

Sincerely,

Ji~->r James P. Buczala Robert G. Ehlenberger

Project Geologist Project Manager

Enclosurescc: Walter Graham, EPA

Peter Ludzia, EPASamantha Philips-Fairchild, EPA (w/o enclosures)Margie Zhang, DNREC (2 copies)Jane Patarcity, BeazerBrandt Butler, DuPontJoel Karmazyn, DuPontT. Faye, Esq., Beazer (w/o enclosures)Michele Gutman, Esq. BCCZ (w/o enclosures)Norm Griffiths, Esq. DuPont (w/o enclosures)Ceil Mancini, WCCJohn Flaherty, Wadsworth/Alert (QAPjP only)Shelly Eyraud, Enseco (QAPjP only)Brad Ayars, Lancaster Labs (QAPjP only)

9IC262S-1/PLANCOV.LTR/KPR4 01-31-94

A R 3 I 1 3 1 1

SUMMARY OF PLAN REVISIONS

FORMER KOPPERS COMPANY. INC. NEWPORT SITENEWPORT, DELAWARE

EPA Comment NumberWP

1234

5

91 11221222426293739464956

57

58

61FSP

646566676871

727375

Sub/act of Revision

StatisticsStatisticsStatisticsAcceptance of RS15 as control station

Sediment grain-size relative to macroinvertebrate samplingInclusion of field notes, preliminary data reduction, etc.Inclusion of field notes, preliminary data reduction, etc.Report SQLsFate and transport analysis added to Rl reportDefine "HHE" and "EE"Insert word "upland" in section titleAnalysis of NAPL samplesReference Figures 8 and 1 1Number and location of PCDD/PCDF samplesAdd term "first flush"East drainage area dataDelete term "best attainable"Use of either water or sed data to determ contam areasCriteria to determine when groundwater purging is complete

Wetland delineation

GPS

Delete the word "conceptual"

Use of PIDs and FIDsHandling of decon waste waterRecording of precipitation dataChange "sediment" to "macroinvertebrate"Preservation of benthic samplesStainless steel sediment sampling tools

Licensed surveyorReference PTG-1 in text, re: ambient air surveyUse organic-free water

Basis of Response

January 3,1994 LetterJanuary 3,1994 LetterJanuary 3,1994 LetterJanuary 3,1994 Letter

December 15, 1993 Meeting

January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter/No Actionlin part)January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter

January 3, 1994 Letter



January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterResponse accepted (No Action)January 3, 1994 Letter

January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter

Location of ResPlan

WPWPWPWPWPWPWPWPWPWPWPWPWPWPFSPWPWPWPWPWPFSP

WPFSP

WPFSP

WP

FSPFSPFSPFSP

FSP

FSPFSPFSP

Section

4.6.34.6.34.6.34.6.2.74.6.34.6.1.34.6.4.34.6.4.34.7.34.16.24.54.5.44.7.34.5.2.22.18.14.6.14.6.2.14.6.2.74.6.34.7.3PTG-9

4.8.22.16PTG-1 44,8.22.16PTG-1 55.7.2.1

PTG-1PTG-3PTG-1 2PTG-1 3

2.14.1PTG-102.52.62.8.2

ponsePage

4.374.374.374.344.374.25, 4.394. 404. 404.474.614.124.194.474.162.364.234.274.324.344.47A. 9-2A. 9-54.50-4.522.28 to 2. 29A. 14-34.532. 30

5.8

A. 1-1A. 3-4, A. 3-5A. 12-2A. 13.1

2.23A. 10-12.32,42.8CO

COPage 1 of 4 1 /31 /94

SUMMARY OF PLAN REVISIONSFORMER KOPPERS COMPANY, INC. NEWPORT SITE

NEWPORT, DELAWARE

EPA Comment Number

76777980838487888990

91939495969798

QAPJP100

14II 2

III 10

III 13

III 14IV 1&2

IV4&6V 3 c

VI 1bVI 2eVI 2j

VI 2n

VI 2p

Subject of Revision

Sample designations on boring logRationale for surface soil sample locations (ref WP Sec 4.5)Rain fall criteria for first flush samplingCriteria for a major rain eventCorrect editorial error, re: use ethanol for benthic: pres.Identification of organisms to genus levelTransectsSeasonal variations, re: ecological evaluationNumber and location of PCDD/PCDF samplesNumber and location of PCDD/PCDF samples

Equipment listSample labels, re: include samp initials and bottle lotShip VOA sediment samples in inverted positionFootnote revision, re: number of bottles requiredNo glass bottleware for aqueous metals samplesCalibration checks of field instrumentsPosition of RS15

Document control formatDistribution listRationale for wells to be sampled for PCDDs/PCDFs

Filtering procedures

Grab or composite samplesID key personnel

Organization chartPrecision objectives for field duplicate samplesMechanism for planning and approving site activitiesGrab or composite samplesLow velocity positive displacement pumps

Holding times

Sample handling and shipping procedures

Basis of Response

January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter

Response accepted (No Action)January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterResponse accepted (No Action)

January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter


January 3, 1994 LettlrJanuary 3, 1994 Letter

January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter



Location of ResPlan

FSPWPFSPFSPFSPFSPFSPFSPFSPFSPFSPFSP

FSPFSPFSPFSPFSP

QAPjPQAPJPFSPWPQAPJPFSPFSPQAPjP

QAPjPQAPJPFSPFSPFSPWPQAPjP

FSPFSP

SectionPTG-34.132.9.12.9.22.142.14.22.152.152.17.12.17.32.18.12.18.12.18.5

3.33.6Table 6Table 6Table 9

TOC2.18.54.7.35.2.4PTG-92.3Table 1aFigure 5Figure 53.3.21 .02.3PTG-94.7.35.2.5Table 1 1Table 63.6

ponsePage

A. 3-2, A. 3-34.572 .102 .102.212.252.282.282.312.352.36, 2.372.36, 2.372.38

3.63.7

12.384.465.79.62.1

3.61.12.19.64.485.7

3.7CO

CO

COPage 2 of 4 1131 /94

SUMMARY OF PLAN REVISIONSFORMER KOPPERS COMPANY, INC. NEWPORT SITE

NEWPORT. DELAWARE

CO

EPA Comment NumberVI 2r

VI 2s

VI 2uVII 2aVII 3a

VIII 2e

VIII 2gX red, 1X red, 6X rep, 3X rep, 5XI 1&3

XII 1b

XII 3aXII 3b

XII 4XII 6XII 7

XIII 2XIII 3

XVI 2aXVI 2eXVI 3a

101102

HASP104105106107108109

Subject of RevisionFrequency of field and trip blanks

Filtering procedures

Coordination with the laboratoryDocument source of reagents or suppliesID sample custodiansCalibration documentation requirements

All analytes included for calibration standards?UnitsProcedures for handling blank resultsID key individuals who handle/report dataAdd to list of Level III reporting requirementsState objectives for field duplicate precisionSpecify that the lab must be audited for parameters for

which it does not have a CLP contractProvide field audit check listDescribe lab audit protocolPresent acceptance criteria for auditsSchedule of auditsSubmit recent PE for laboratorySpare parts listSource of spare partsStatus of projectChanges to QAPjPFinal storage and security of data filesCompleteness goalCalibration procedures

Replace "constituents" with "contaminants"Restructure HASPUpgrade respiratory protectionSite security - sign postingDetailed exposure pathways/health effectsList key personnel and response authorities

Basis of ResponseJanuary 3, 1994 Letter


January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter

January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter

January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter

Location of ResPlan

QAPJPQAPJPFSPWPWPQAPjPFSP

QAPJPQAPJPQAPJPQAPjP

QAPJPQAPJPQAPJPQAPJPQAPjPQAPjPQAPjPQAPjPQAPjPQAPjPQAPjPQAPjP

Section3.2.1Table 2Table 54.13Table 55.2.4PTG-9PTG-114.35.1Table 16.2.2APP G6.28.28.1Table 1a8.2.13.3.22.17.1APPH10.210.3.410.2

Submitted with QAPjPQAPjPQAPjPQAPjPQAPjPQAPjPQAPjPQAPjPHASP

HASPHASPHASPHASPHASPHASP

11.111.114 .014 .014 .03.3.36.1ATT 6

>onsePage

3.2

4.56

5.79.611.24.15.2

6.5

6.48.38.2

8.33.62.17.1

10.210.410.2

11.111.114.114.214.13.66.3

throughout planlimited restructuring8.19.16

8.29.9

Table 4a and 4b2.1 2,1

CO Page 3 of 4 1/31/94

SUMMARY OF PLAN REVISIONSFORMER KOPPERS COMPANY/INC. NEWPORT SITE

NEWPORT, DELAWARE

EPA Comment Number110111112

114115116117118119120121122123124

125126127128129130131132133134135136

Subject of RevisionHeavy equipment decontaminationImproved safetyChanges to hazard assessment / inhalation of particulates

First aid • snake bitesTick bitesBee stings / allergic reactionsPhysical hazardsExplanation of probe selection - HNuMonitoring instrument limitationsInstrument calibrationsReference errorClarification of consistently elevatedRationale for assignment of Action LevelsExposure Levels for pentachlorophenol

Methane discussionPPE selection based upon taskDiscuss level A & B PPEModify discussion of respirator cartridge changeDiscuss fit testingEstablishment of exclusion zonesDecontamination padHazard risk analysisOn-site emergenciesResponse to incidentsAddition of missing sectionsHASP approvals moved to front of plan

Basis of ResponseJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter

January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter

January 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 LetterJanuary 3, 1994 Letter

Location of ResPlan

HASPHASPHASP

HASPHASPHASPHASPHASPHASPHASPHASPHASPHASPHASP

HASPHASPHASPHASPHASPHASPHASPHASPHASPHASPHASPHASP

Section10.1Table 4b7.1

ponsePage

10.2

7.1Tables 3, 4, 57.27.27.2Table 57.5.17.5.17.5.37.67.67.67.3Table 37.5.2Table 4b8.19.6.1Att 119.1410.27.611.39.3

1 .0

7.17.17.2

7.87.87.97 .107. 107, 107.3

7.9

8.29.4

9.810.17. 1011.39.2

1

I*3OCO

CO

en

Page 4 of 4 1/31/94

REVISION NO. 1

QUALITY ASSURANCE PROJECT PLANREMEDIAL INVESTIGATION/FEASIBILITY STUDYFORMER KOPPERS COMPANY, INC.NEWPORT SITE

January 31, 1994

For:

U.S. Environmental Protection AgencyRegion 3841 Chestnut StreetPhiladelphia, Pennsylvania 19107

Prepared for:

Beazer East, Inc.436 Seventh AvenuePittsburgh, Pennsylvania 15219

and

Du Pont ChemicalsRoom 122281007 Market StreetWilmington, Delaware 19898

Prepared by.

Woodward-Clyde Consultants5120 Butler PikePlymouth Meeting, Pennsylvania 19462

Project No. 91C2628-3X2

A R 3 I 1 3 1 6


TABLE OF CONTENTS

Section Page Number

DISTRIBUTION LIST 11.0 PROJECT DESCRIPTION AND OBJECTIVES 1-1

1.1 PURPOSE AND SCOPE 1-11.2 SITE BACKGROUND 1-21.3 PROJECT SCHEDULE 1-21.4 SAMPLING PROGRAM 1-21.5 DEFINITION OF OBJECTIVES 1-31.6 DATA QUALITY OBJECTIVES 1-41.7 PROJECT DEFINITIONS 1-8

2.0 PROJECT ORGANIZATION AND RESPONSIBILITY 2-1

2.1 RESPONSIBILITIES OF KEY PERSONNEL 2-1

2.1.1 Project Managers 2-22.1.2 Project QA/QC Officer 2-22.1.3 Task Leaders 2-32.1.4 Project Staff 2-32.1.5 Site Health and Safety Officer 2-3

2.2 QUALIFICATIONS OF PERSONNEL 2-3

3.0 QUALITY ASSURANCE OBJECTIVES FORMEASUREMENT OF DATA 3-1

3.1 GENERAL 3-13.2 LEVEL OF QA EFFORT 3-1

3.2.1 Field QC Samples 3-1

3.3 DATA QUALITY INDICATORS 3-4

3.3.1 Accuracy 3-53.3.2 Precision 3-63.3.3 Completeness 3-63.3.4 Representativeness 3-73.3.5 Comparability 3-7

91C262S-I/QAPJP-KN.RPTYKPR4 i 01-31-94

f l R 3 l 1 3 1 7


TABLE OF CONTENTS (continued)

Section Page Number

3.4 SENsrnvrrY OF ANALYSIS 3-8

4.0 SAMPLING AND FIELD PROCEDURES 4-1

4.1 SCOPE OF WORK 4-14.2 QUALIFICATIONS OF SAMPLING PERSONNEL 4-14.3 HELD INVESTIGATION 4-1

5.0 SAMPLE AND DOCUMENT CUSTODY PROCEDURES 5-1

5.1 FIELD DOCUMENTATION " 5-15.2 SAMPLE IDENTIFICATION 5-2

5.2.1 Sample Location Numbers 5-35.2.2 Sample Labels 5-65.2.3 Sample Containers 5-75.2.4 Sample Preservation 5-75.2.5 Sample Handling and Shipping 5-7

5.3 CHAIN-OF-CUSTODY PROTOCOL 5-8

5.3.1 Field 5-85.3.2 Laboratory Custody Procedures 5-10

5.4 PROJECT FILE 5-10

6.0 CALIBRATION PROCEDURES AND FREQUENCY 6-1

6.1 FIELD INSTRUMENTS AND EQUIPMENT 6-16.2 LABORATORY INSTRUMENTATION 6-3

6.2.1 Standard/Reagent Preparation 6-46.2.2 Documentation 6-5

7.0 ANALYTICAL PROCEDURES 7-1

7.1 LABORATORY PROCEDURES 7-1

91C262S-I/QAPJP-KN.RFT/KPR4 H 01-31-94

R R 3 I 1 3 1 8



Section Page Number

8.0 DATA REDUCTION, REPORTING AND VALIDATION 8-1

8.1 DATA REDUCTION 8-18.2 REPORTING DEUVERABLES 8-2

8.2.1 Non CLP Deliverables (Level 3) 8-38.2.2 CLP Deliverables 8-4

8.3 VALIDATION/REVIEW 8-58.4 REQUIREMENTS FOR LAB DATA

RESULTS ON DISKETTES 8-6

9.0 INTERNAL QUALITY CONTROL CHECKS 9-1

9.1 FIELD QC CHECKS 9-19.2 LABORATORY QC CHECKS 9-1

9.2.1 Matrix Spike Sample 9-39.2.2 Matrix Spike Duplicate Sample 9-49.2 3 Method Blank Sample 9-49.2.4 Laboratory Control Samples (LCS) 9-49.2.5 Surrogate Compounds, Internal

Standards and Cleanup Standards 9-5

9.3 QUALITY CONTROL OF BENTHICLABORATORY ANALYSES 9-6

9.4 GEOTECHNICAL ANALYSES 9-6

10.0 PERFORMANCE AND SYSTEMS AUDITS 10-1

10.1 PERFORMANCE AUDITS 10-110.2 SYSTEMS AUDITS 10-210.3 AUDIT PROCEDURE 10-2

10.3.1 Audit Notification 10-210.3.2 Pre-Audit Conference 10-210.3.3 Audit 10-310.3.4 Acceptance Criteria 10-310.3.5 Post-Audit Conference 10-3

91C262S-1/QAPJP-KN.RPT/KPR4 Hi 01-31-94

f l R 3 l 1 3 1 9



Section

10.3.6 Audit Report

10.4 AUDIT RESPONSE10.5 FOLLOW-UP ACTION10.6 AUDIT RECORDS

11.0 PREVENTIVE MAINTENANCE

11.1 FIELD INSTRUMENTS11.2 LABORATORY INSTRUMENTS

12.0 DATA MEASUREMENT ASSESSMENT PROCEDURES

12.1 ACCURACY12.2 PRECISION12.3 COMPLETENESS

13.0 CORRECTIVE ACTION

Page Number

10-3

10-410-410-5

11-1

11-111-2

12-1

12-212-312-3

13-1

13.! FIELD CORRECTIVE ACTION 13-113.2 LABORATORY CORRECTIVE ACTION 13-213.3 CORRECTIVE ACTIONS FOLLOWING DATA ASSESSMENT 13-4

14.0 QUALITY ASSURANCE REPORTS TO MANAGEMENT

15.0 REFERENCES

14-1

15-1

91C2628-1/QAPJP-KN.RFT/KPR4 IV 01-31-94

A R 3 I 1 3 2 0

Woodward-CtydeConsultants


LIST OF TABLES

TABLE la

TABLE 1

TABLE 2

TABLE 3

TABLE 4

TABLES

TABLE 6

TABLE 7

TABLES

TABLE 9

TABLE 10

TABLE 11

LIST OF PROJECT PERSONNEL

QC LEVEL OF EFFORT FOR ANALYTICAL TESTING

SUMMARY OF QC SAMPLING AND ANALYSIS PLAN

QUALITY CONTROL METHOD CRITERIA FOR ACCURACY(SURROGATE SPIKE RECOVERIES) FOR ORGANICPARAMETERS (WATER AND SOIL SAMPLES)

QUALITY CONTROL METHOD CRITERIA FOR ACCURACY(MATRIX SPIKE RECOVERIES) AND PRECISION(RELATIVE PERCENT DIFFERENCE) FORORGANIC PARAMETERS (WATER AND SOIL SAMPLES)

QUALITY CONTROL METHOD CRITERIA FOR ACCURACY(MATRIX SPIKE RECOVERIES) AND PRECISION(RELATIVE PERCENT DIFFERENCE) FOR METALSAND INORGANICS (WATER AND SOIL SAMPLES)

QUANTITATION LIMITS FOR VOLATILE ORGANICS

QUANTITATION LIMITS FOR SEMI-VOLATILE ORGANICS

QUANTITATION LIMITS FOR ORGANOCHLORINEPESTICIDES AND PCBs

QUANTITATION LIMITS FOR INORGANIC PARAMETERS

QUANTITATION LIMITS FOR PCDDs/PCDFs

SAMPLE CONTAINERS, PRESERVATION ANDHOLDING TIME REQUIREMENTS

91C262&-l/QAPIP-KN.RFTflCPR4

A R 3 I 1 3 2 101-31-94

woodward-ClydeConsultants


LIST OF TABLES (concluded)

TABLE 12 SUMMARY OF ANALYTICAL METHODS

TABLE 12a SUMMARY OF GEOTECHNICAL SAMPLES AND METHODS

TABLE 13 FIELD EQUIPMENT CALIBRATION AND MAINTENANCEREQUIREMENTS

LIST OF FIGURES

FIGURE 1 REGIONAL LOCATION PLAN

FIGURE 2 HISTORICAL FACILITY OPERATION MAP

FIGURE 3 POTENTIAL AREAS OF INTEREST

FIGURE 4 SAMPLE LOCATION MAP

FIGURE 5 PROJECT ORGANIZATIONAL STRUCTURE

LIST OF APPENDICES

APPENDIX A WADSWORTH/ALERT QUALITY ASSURANCE PLAN

APPENDIX B LANCASTER LABORATORIES QUALITY ASSURANCE PLAN

APPENDIX C ENSECO QUALITY ASSURANCE PLAN

APPENDIX D RESUMES OF KEY WCC PERSONNEL

91C262M/QAPJP KN.RPT/KPR4 VI 01-31-94

A R 3 I 1 3 2 2


TABLE OF CONTENTS (concluded)

LIST OF APPENDICES (concluded)

APPENDIX E LOW LEVEL METHOD DETECTION LIMITS

APPENDIX F GEOTECHNICAL ANALYSES, QUALITYASSURANCE/QUALITY CONTROL & STANDARDOPERATING PROCEDURES

APPENDIX G CALIBRATION DOCUMENTATION REQUIREMENTS

APPENDIX H FIELD AUDIT CHECK LIST

91C262S-1/QAPJP-KN.RPT/KPR4 VU 01-31-94

A R 3 I 1 3 2 3


DISTRIBUTION LISTQUALITY ASSURANCE PROJECT PLAN

FORMER KOPPERS COMPANY, INC. NEWPORT SITENEWPORT, DELAWARE

NAME

Walter Graham

Peter Ludzia

S. Andrew Sochanski

Samatha Philips-Fairchild

Marge Zhang

Jane Patarcity

Brandt Butler

Joel Karmazyn

Robert Ehlenberger

James Buczala

Ceil Mancini

John Flaherty

Shelly Eyraud

Brad Ayars

AFFILLIATION

EPA

EPA

EPA

EPA

DNREC

Beazer

DuPont

DuPont

WCC

WCC

WCC

Wadsworth/AlertLaboratories

Enseco

Lancaster Laboratories

91C2628-1/QAPJP-KN.RPT/KPR4 01-31-94

A R 3 1 1321*


Section 1.0Revision No. 1

02-01-94Page 1 of 14

1.0

PROJECT DESCRIPTION AND OBJECTIVES

1.1 PURPOSE AND SCOPE

An Administrative Order of Consent (Consent Order) has been executed (effective dateOctober 4, 1991) between Beazer East, Inc., (Beazer), E.I. du Pont de Nemours and

Company, Inc. (Du Pont) and the United States Environmental Protection Agency (U.S.

EPA), Region III to perform a Remedial Investigation (RI) and a Feasibility Study (FS)at the former Koppers Company, Inc. Newport Superfund Site (Site) in Newport,Delaware. The work for the Site will be conducted as a joint effort between Beazer and

Du Pont. This document presents Woodward-Clyde Consultants (WCC) QualityAssurance Project Plan (QAPjP) for work related to the Site. The purpose of thisdocument is to detail methods and procedures for attaining data of known quality whichare scientifically and legally defensible and will meet data quality objectives for the Site.

This QAPjP is to be used in conjunction with the RI/FS Work Plan, Field Sampling Plan(FSP) and the Site Health and Safety Plan (HSP). The QAPjP details the objectives and

planned activities of the current investigations. The QAPjP also presents staffing andother management activities. The QAPjP has been prepared using the following USEPAdocuments as guidance:

1. Interim Guidelines and Specifications for Preparing Quality AssuranceProject Plans QAMS-005/80

2. Preparation Aids for the Development of Category I Quality Assurance

Project Plans (EPA/600-8-91/003)

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SITE BACKGROUND

The former Koppers Company, Inc. Newport Site was a wood preserving (treatment)

facility. The Site is situated on a 317-acre parcel of land located in the northern part

of New Castle County, Delaware (Figure 1) outside of the Town of Newport. White

Clay Creek and the Christina River border the Site to the southwest and southeast,

respectively. Hershey Run, a tributary to White Clay Creek, borders the Site to the

west. Wetlands are associated with each of these three waterways. Figure 2 presents

a historical layout of the Site; and Figure 3 presents delineation of the potential areas

of interest.

Background information, a review of previous studies, and a review of currently available

aerial photographs and topographic maps of the Site are presented in Section 2.0 of the

Work Plan, Remedial Investigation/ Feasibility Study, Koppers Company, Inc. Newport

Site (WP) prepared by WCC and submitted to the U.S. EPA on May 7, 1993.

1J PROJECT SCHEDULE

A detailed discussion of the project schedule is presented in Section 8.0 of the WP. The

beginning date for the scheduled tasks will be determined by the date of approval of the

Work Plan by EPA.

1.4 SAMPLING PROGRAM

The sampling program to be implemented will include collection and analysis of soil,

sediment, groundwater and surface water samples from the Site. Details regarding the

sampling program are provided in the FSP and briefly discussed in Section 4.0. Figure 4

presents the approximate sample locations.

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1.5 DEFINITION OF OBJECTIVES

The main objective of the RI program is to gather data necessary to: perform a Human

Health and Environmental Evaluation (Risk Assessment) for the Site; evaluate the

possible need for Site remediation; and, if needed, to allow for an evaluation of

appropriate remedial action alternatives. In order to best utilize the data generated

during the RI to support the decision making process, a clear definition of the RI

objectives and procedures for data collection is required. The specific objectives of the

RI activities at the Site are to:

• Identify and characterize the nature and extent of potential contaminants

in groundwater, surface water, soils and sediments and identify whether

air is a potential exposure pathway

• Collect data adequate to assess the extent to which the detected

contaminants of interest pose a threat to the public health, welfare, or the

environment

• Define the extent of Jurisdictional wetlands on-site

• Develop a Conceptual Site Model (CSM) and refine the model based on

actual field data, to identify potential sources, to evaluate pathways for

potential constituent migration, and to identify potential human and

environmental receptors

• Produce appropriate, sufficient and defensible data to assess potential

human health and environmental risks, to evaluate the extent of possible

remediation which may be required, and if needed, to support the

development and evaluation of remedial action alternatives

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Characterize cultural and historical resources on-site

In order to accomplish these objectives, a series of tasks will be performed to collect and

evaluate the necessary data on existing Site conditions and characteristics. An integral

part of the process is the definition of Data Quality Objectives (DQOs). DQOs are

described in the following section.

1.6 DATA QUALITY OBJECTIVES

DQOs are presented in this QAPjP in conjunction with the associated Work Plan and

FSP. The purpose of the DQO process is: to ensure that RI task objectives are clearly

defined; to determine what environmental data are necessary to meet these objectives;

and to ensure that information obtained during the RI will be adequate to support

present and future decisions that may rely on these data. It is important that the quality

of data be sufficient to address the immediate project objectives and that they can also

address future issues that are likely to occur. The overall objective of this investigation

is to determine the potential impacts of the Site on area soil, groundwater, wetland

sediments, surface water and air. An important anticipated future objective is to

determine remedial goals, if necessary.

DQOs are defined as qualitative and quantitative statements of the level of uncertainty

decision makers are willing to accept in the outcome of the assessment of Site objectives.

DQOs are established such that the collected data are sufficient and of adequate quality

for their intended use. The DQOs are based on environmental data, including the

specification of a range of true values where decisions can be made, and that any

uncertainty in the decision can be evaluated. DQO development is an iterative process

designed to focus on the decisions which must be made and ensures that the Site

activities are logical and cost-effective.

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The concept of data quality objectives is actually a three-step process. Although thethree stages are briefly discussed below sequentially, they are undertaken in an

interactive and iterative manner whereby all the DQO elements are continually reviewedand re-evaluated. As such, the DQO process is integrated with development of theQAPjP and FSP and may be revised as needed based upon the results of each datacollection activity.

• Stage 1 - Identify Decision Types - Stage 1 of the DQO process definesthe types of decisions which will be made regarding Site remediation, if

necessary, through identifying data uses, evaluating available data,developing a conceptual model of the Site (CSM), and specifyingobjectives for the project. Available information is compiled and analyzedto develop a CSM. This model, presented in Section 4.3 of the Work

Plan, describes potential contaminant sources, potential migrationpathways, and potential receptors. The model facilitates identification ofdecisions which must be made and deficiencies in the existing information.Stage 1 results in the specification of the decision-making process andidentification of why new data are needed.

• Stage 2 - Identify Data Uses/Needs - Stage 2 stipulates criteria fordetermining data adequacy. This stage involves specifying the datanecessary to meet the objectives set in Stage 1. Stage 2 includes selection

of the sampling approaches and the analytical options for the Site,including evaluation of multiple-option approaches to effect more timelyor cost-effective data collection and evaluation. Section 4.0 of the Work

Plan summarizes the data collection components of the RI, in conjunction

with the FSP and the QAPjP, to satisfy the Stage 2 identification of data

needs.

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• Stage 3 - Design Data Collection Program - Stage 3 results in thespecification of the methods by which data of acceptable quality and

quantity will be obtained to make decisions. This information is provided

in documents such as the FSP and this QAPjP. The FSP will providedetails regarding sampling equipment, sampling locations, sample analyses,sampling schedules, and quality control samples. Quantitative limits ofprecision and accuracy are established in this QAPjP for analyticalparameters designed to meet uncertainty goals. Qualitative statements arealso described in this QAPjP concerning the goals of representativeness,

completeness, and comparability, which are important in the overall data

assessment process for making decisions regarding the Site.

Setting priorities for data use helps to determine the highest level of confidence requiredfor each data type. Data use categories include:

• Monitoring during implementation

• Health and safety planning• Site characterization (Site boundary delineation)

• Risk assessment• Evaluating remedial alternatives• Engineering design of remedial alternatives

Based on the Stage 1 efforts in the DQO process, data for the former Koppers

Company, Inc. Newport Site are required for Site characterization, risk assessment, andevaluation of alternatives. Analytical levels for the data uses listed above and the

sampling activities to be conducted during the RI are discussed below.

Level 1 - Field screening or analysis using portable instruments. Results are

often not compound specific and not quantitative, but they are available in real

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time. Examples of Level 1 data that will be collected at the Site during the RIinclude water level measurements, HNU and/or OVA monitoring.

Level 2 - Field analysis using more sophisticated portable analytical instruments.In some cases, the instruments may be set up in a mobile laboratory on-site.

Quality of the data generated depends on the use of suitable calibrationstandards, reference materials, sample preparation equipment, and the training

of the operator. Results are available in real-time or with a time lag of severalhours. An example of Level 2 data that could be collected at the Site, but arenot scheduled, would be soil-gas surveys and certain geophysical surveys.

Level 3 - All analyses performed in an off-site analytical laboratory. Level 3analyses may or may not use Contract Laboratory Program (CLP) procedures, butare required to use EPA-approved methods. They do not usually utilize thedocumentation procedures required of Level 4 analysis. The laboratory may or

may not be a CLP laboratory. Examples of Level 3 data that will be collected atthe Site include geotechnical analyses (i.e., grain size analysis) of the soil,sediment, and select chemical analyses of surface water samples.

Level 4 - CLP routine analytical services (RAS). All analyses are performed inan off-site laboratory following CLP protocols. The laboratory may or may notbe a CLP laboratory. Level 4 is characterized by rigorous QA/QC protocols and

documentation. Level 4 data that will be collected at the Site will include CLPchemical analysis of the soil, sediment, groundwater, and surface water samples.

Level 5 - Analysis by non-standard methods. All analyses are performed in anoff-site analytical laboratory which may or may not be a CLP laboratory. Method

development or method modification may be required for specific constituents or

detection limits. Level 5 analytical methods may be required on residential wells

and selected site monitoring wells as discussed in the Revised Work Plan.

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With the exception of select surface water analyses, geotechnical analyses and

groundwater analyses (in the second and third sampling episodes), all analytical data will

conform to Level 4 requirements. These samples will be analyzed for Target Compound

List (TCL) volatile organics, semi-volatiles (base neutrals/acid extractables), and Target

Analyte List (TAL) metals (total and dissolved for groundwater and surface water

samples) using CLP procedures (see Section 7.0). Twenty percent of the investigative

samples collected will be analyzed for TCL pesticides/PCBs and PCDDs/PCDFs also

using CLP procedures (see Section 7.0). Surface water samples will also be analyzed for

inorganic parameters alkalinity and total suspended solids (TSS). Data for these

analyses will conform to level three requirements.

1.7 PROJECT DEFINITIONS

The following definitions apply to terms commonly used in the text of this document:

Accuracy Nearness of a measurement or the mean of a set of

measurements to the true value. Accuracy is

evaluated using the percent recovery of sample

spikes, analysis of laboratory control samples and

reference materials.

Analytical Batch The basic unit for analytical quality control is the

analytical batch. The analytical batch is defined as

20 or fewer samples which are analyzed together

with the same method sequence, and same lots of

reagents, and within the same time period. Samples

in each batch are of similar matrix (e.g.,

groundwater, surface water, soil, sediment, etc.).

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Calibration Blank

CLP

CLP-SOW

Comparability

Completeness

Duplicate Samples


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Usually an organic or aqueous solution which is asanalyte-free as possible. This sample is preparedwith the same volume of chemical reagents used inpreparing the calibration standards. The calibrationblank is used to give the null reading for the

instrument response versus concentration calibrationcurve.

The U.S. Environmental Protection Agency ContractLaboratory Program.

CLP-Statement of Work

A measure of confidence with which one data set can

be compared with another.

A measure of the amount of valid sample dataobtained from the measurement system compared tothe amount of sample data that are analyzed. Valid

results are those results which meet or exceed qualitycontrol criteria and satisfy quality assurance

objectives. Estimated results are also considered tobe valid.

Duplicate samples for this program are two samples

collected separately at a given time and location.These samples will not be homogenized.

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Environmental Samples(Field Samples)

Field Blank Sample


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Environmental samples (field samples) arerepresentative samples of any materials (aqueous,nonaqueous, or multimedia) collected.

Field blank samples are collected as a check onpotential sample contamination from ambient air

conditions at the site during sampling. A field blanksample is collected in the field by pouring analyte-free water into laboratory glassware for analysis of

VOCs, semi-VOCs, and metals.

FSP

Laboratory CheckSample

Laboratory DuplicateSample (LDS)

Internal Standard

Field Sampling Plan

A laboratory check sample is a sample of knowncomposition which is analyzed concurrently with fieldsamples. It is used to verify analytical system

performance.

A laboratory duplicate sample is a sample that is

divided into two portions, both carried through theanalytical preparation procedure and analyzed as

separate samples. Laboratory duplicate samples are

associated with metals and PCDD/PCDF analyses.

An internal standard is a compound that is notnaturally found and which represents the class ofcompound being tested. They are added to allsamples, blanks and QC samples. Recoveries ofinternal standards are used to compensate for matrix

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Matrix Spike(MS) Sample

Matrix Spike Duplicate(MSD) Sample

Method Blank Sample


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effects in the quantitation process for GC/MSanalyses.

A matrix spike sample is employed to provide ameasure of method accuracy in a given matrix. A

matrix spike sample analysis is performed by adding

a predetermined quantity of stock solutions of certain

analytes that are representative of test constituents,to a sample matrix prior to sampleextraction/digestion and analysis. The concentrationof the spike should be at the regulatory standardlevel, or above the methods quantitation limit.MS samples are associated with organic samples,inorganic samples, and PCDD/PCDF samples.

A matrix spike duplicate (MSD) sample is a secondmatrix spike sample prepared identically to thematrix spike on a duplicate sample of the matrix.

MSD samples are only associated with organic

samples.

A method blank sample is an aliquot of analyte-freewater or solid containing all the reagents used in theprocessing of the samples. The method blank sampleis carried throughout the complete sample

preparation procedure and contains the same reagent

concentrations in the final solution as in the samplesolution used for analysis. The method blank sampleis used to monitor for possible contamination result-

ing from the preparation or processing of the sample.

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Method Detection

Limit (MDL)

PCDDs/PCDFs

Precision

QAPjP

Quantitation Limit

Representativeness


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The method detection limit (MDL) is defined as theminimum concentration of a substance that can be

measured and reported with 99 percent confidencethat the analyte concentration is greater than zeroand is determined from analysis of a sample in agiven matrix containing the analyte.

Dioxins and Chlorinate^! Furans

Precision is the agreement between a set of replicate

measurements without assumption or knowledge ofthe true value. Precision is evaluated as the relativepercent difference (RPD) or percent relativestandard deviation (% RSD) for duplicate or split

samples.

Quality Assurance Project Plan

The quantitation limit is the lowest analyte

concentration which can be reliably achieved withinspecified precision and accuracy limits during routinelaboratory operating conditions as defined in theLaboratory Quality Assurance Plans (LQAPs).

The degree to which a single measurement is

indicative of the characteristics of a larger sample or

area or the degree to which data represents field

conditions.

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Rinsate Blank Sample

Sample Delivery Group

(SDG)


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A rinsate sample is a sample produced in the field byrinsing decontaminated sampling equipment

(including filtering apparatus for filtered samples

where appropriate) with analyte-free water. Thewater is collected for analysis. The volume of watercollected will not exceed twice the volume requiredfor analysis.

For the purposes of this project, an SDG is defined

as each 20 field samples collected, or each 14

calendar day period during which field samples forthis project are received by the laboratory(s)beginning with the receipt of the first sample in theSDG.

Surrogate Spike

Compound

Trip Blank Samples

A surrogate spike is a compound that is not

naturally found which represents the class ofcompounds being tested, spiked to every blank, every

sample and every MS/MSD sample that undergoesorganic analyses excluding PCDDs/PCDFs. Thesecompounds are used to measure analytical efficiency.

Trip blank samples are samples of analyte-free waterprepared in the laboratory. Trip blank samples arekept with the sample bottles from the time they leavethe laboratory until the time they are returned to the

laboratory. Trip blank samples pertain only toaqueous volatile organic compounds (VOC) and,

therefore, the containers must contain no headspace.Trip blank samples serve as a check on sample

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contamination originating from container migration

or from sample transport.

TAL Target Analyte List

TCL Target Compound List

U.S. EPA United States Environmental Protection Agency

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2.0

PROJECT ORGANIZATION AND RESPONSIBILITY

2.1 RESPONSIBILITIES OF KEY PERSONNEL

The organizational structure and responsibility, defined below and in Figure 5, isdesigned to assure adequate project control and proper quality assurance for Siteinvestigative activities at the former Koppers Company, Inc. Newport Site. Further, thenecessary communication and independent review is discussed. The internalorganizational structures for the subcontract laboratories are provided in Appendix A(Wadsworth/Alert), Appendix B (Lancaster), and Appendix C (ENSECO-CAL).

Wadsworth/Alert Laboratories, Inc., of Pittsburgh, Pennsylvania, is the primarysubcontract laboratory; Lancaster is the back-up laboratory; and ENSECO-CAL will besubcontracted to Wadsworth/Alert for PCDD/PCDF analyses. Resumes for key WCCpersonnel are included as Appendix D.

The following key personnel are described below:

• Project Managers• Project QA/QC Officer• Task Leaders• Project Staff• Site Health and Safety Officer

Project organization is presented in Figure 5. Other principal project personnel havebeen identified; however, during the course of the project these personnel may besubject to change without agency notification or approval. A list of other project

personnel is presented in Table la.

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2.1.1 Project Managers

The WCC Project Manager (Project Manager) for the Koppers Company, Inc. NewportSite will be Mr. Robert Ehlenberger. Mr. Ehlenberger has primary responsibility for thecompletion of all activities on the project. He is responsible to Beazer and Du Pont for

the day-to-day control of planning, scheduling, cost control, and implementation of theproject, and for the development of the technical reports and other project documents.The Project Manager monitors all project personnel in planning, coordinating, andcontrolling all technical aspects of the tasks. Project managers for Beazer and Du Pontare Ms. Jane Patarcity and Mr. Joel Karmazyn, respectively. The successful managementof this project will be dependent to a large degree upon the communication between the

project managers.

2.12 Project QA/QC Officer

The Project QA/QC Officer will be Dennis Takade. The QA/QC Officer works directlywith the Project Manager and other project personnel. The QA/QC Officer has theresponsibility to monitor and verify that the work is performed in accordance with this

plan, the SOPs, and other applicable procedures. The QA/QC Officer also has the

responsibility to assess the effectiveness of the QA/QC program and to recommendmodifications to the program when applicable. The QA/QC Officer is responsible forassuring that personnel assigned to the project are trained and indoctrinated relative tothe requirements of the QA/QC Program. He is also responsible for periodic qualityassurance audits. The QA/QC Officer will advise the Project Manager on implemen-tation of the QA/QC program, but the functions of the QA/QC Officer and

representatives are independent of the Project Manager. The QA/QC Officer has theauthority to halt work in case of major problems or nonconformances to the QAPjP or

if any minor problems are not corrected in a timely manner.

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2.1.3 Task Leaders

Each WCC Task Leader is responsible to the Project Manager for planning, scheduling,

cost control, and completion of assigned project tasks. The Task Leader is responsiblefor implementing the QA/QC program related to assigned tasks at the Koppers

Company, Inc. Newport Site. Figure 5 presents the project organization chart and eachtask leader for the RI/FS.

2.1.4 Project Staff

Each member of the WCC project staff is responsible to the Task Leader and/or ProjectManager for completion of assigned project activities. Members of the project staff areresponsible for understanding and implementing the QA/QC program as it applies totheir project activities.

2.1.5 Site Heaith and Safety Officer

The WCC Site Health and Safety Officer (SHSO) will be James Buczala. The WCC SiteHealth and Safety Officer (SHSO) monitors all Site activities and is responsible for the

implementation of and compliance with the Project Health and Safety Plan. The SHSOreports directly to the WCC Project Manager.

22 QUALIFICATIONS OF PERSONNEL

All personnel assigned to the project, including employees and consultants, will be

qualified to perform the task to which they are assigned. Appraisal of the qualifications

of technical personnel assigned to the project will be made by the WCC ProjectManager. The appraisal will include the comparison of the requirements of the jobassignment with the relevant experience and the training of the prospective assignee; itwill also include a determination of whether further training is required and, if required,

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by what method. On-the-job training is acceptable, provided such training is providedby a person qualified to perform the assignment and the results of that training aredocumented. All documents concerning qualification appraisal will be stored in the

project administrative files.

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3.0

QUALITY ASSURANCE OBJECTIVES

FOR MEASUREMENT OF DATA

3.1 GENERAL

The overall QA objective for the investigations at the former Koppers Company, Inc.Newport Site is to develop and implement procedures for sampling, laboratory analyses,

field measurements, and reporting that will provide data having a degree of quality

consistent with its intended use. The sample set, chemical analysis results, and inter-pretations must be based on data that meet or exceed quality assurance objectivesestablished for the project. Quality assurance objectives and procedures for fieldmeasurement systems are also important aspects of these investigations. The followingparagraphs discuss field and laboratory analytical measurements.

Quality assurance objectives are usually expressed in terms of accuracy or bias, precision,

completeness, representativeness, comparability, and sensitivity of analysis. Target

ranges for these objectives are presented for analytical testing and field measurements.Variances from the quality assurance objectives in any stage of the RI/FS will result inthe implementation of appropriate corrective measures and an assessment of the impact

of corrective measures on the usability of the data in the decision-making process.

32 LEVEL OF QA EFFORT

3.2.1 Field QC Samples

To assess the quality of data resulting from the field sampling program, field duplicate

samples, rinsate blank samples, matrix spike/matrix spike duplicate (MS/MSD)

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(organics) and MS/laboratory duplicate samples (inorganics and PCDDs/PCDFs), field

blank samples, and trip blank samples will be collected and submitted, whereappropriate, to the analytical laboratory.

The frequencies of field QC samples to be submitted to the analytical laboratory will beas identified below:

1. Groundwater/Surface Water Samples

• Field duplicate samples will be collected for all subject parameters at a

frequency of one per 20 investigative samples.

• Rinsate blanks will be collected for all subject parameters at a frequency

of one per 20 investigative samples per matrix. Rinsates will includefiltering equipment blanks (filter blanks) for dissolved metals analyses ata rate of one per 20 investigative samples collected for dissolved metalsanalyses.

• Triple sample volume will be supplied by WCC (or as much as sufficient)

to the laboratory to perform MS/MSD (organics) and/or MS/laboratoryduplicate analyses (inorganics, PCDDs/PCDFs). One volume for sampleanalysis and two volumes for MS/MSD or MS/laboratory duplicate

analyses. Other MS/MSD samples will not be collected for samplesanalyzed by low level CLP protocol if the method is required. The lowlevel CLP protocol substitutes laboratory control samples for MS/MSDsamples. For CLP analyses, these QC samples will be collected at a rateof one per twenty investigative samples.

• Trip blank samples (2-40 ml VOC vials filled with laboratory analyte-free

water) will be submitted to the laboratory at a frequency of one per

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shipping container (containing VOC samples) of aqueous samples for

VOC analyses.

• Field blank samples for VOC, semi-VOC and metals will be collected ata rate of 1 per 20 samples collected when field conditions indicate thepossibility of airborne constituents or volatilization of potential

contaminants.

2. Soil/Sediment Samples

• Field duplicate samples will be collected at a frequency of one per 20

investigative samples.

• Rinsate blanks will be collected at a frequency of one per 20 investigative

samples per matrix.

• Sufficient sample volume will be supplied to the laboratory by WCC toperform MS/MSD (organics) or MS/laboratory duplicate analyses(inorganics and PCDDs/PCDFs) at a frequency of one per 20 samples.Submittal of full analytical bottleware to the laboratory should besufficient volume for the primary analysis as well as the MS/MSD

analyses.

• Trip blanks will be submitted to the laboratory at a frequency of one pershipping container (containing VOC samples) for VOC analyses.

• Field blank samples for VOC, semi-VOC and metals will be collected at

a rate of 1 per 20 samples collected when field conditions indicate the

possibility of airborne constituents or volatilization of potential

contaminants.

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Field duplicate samples will be analyzed to check the aggregate sampling precision andanalytical reproducibility. Trip blanks will be analyzed to check for contaminationresulting from sample shipment and/or transport. Field blanks will be analyzed to checkfor contamination from ambient air conditions at the Site. Rinsate blanks will beanalyzed to check for cross-contamination from sampling and/or filtering equipment

decontamination procedures. MS/MSD (organics) samples, MS/laboratory duplicate

samples (inorganics and PCDDs/PCDFs) and/or laboratory control samples (low levelCLP) if required will be analyzed to evaluate analytical accuracy and precision.

The level of QC effort provided by the project laboratory(s) will be equivalent to thelevel of QC effort specified by the respective analytical methods used for analysis. Theoverall level of QC effort is described in the laboratory quality assurance plans (LQAPs)included in Appendices A, B and C. The level of laboratory QC effort required for

specific analytical parameters is summarized in Table 1. The QC sampling and analysisprogram is summarized in Table 2 which lists the specific parameters to be analyzed andthe number and frequency of QC sampling required.

The QC level of effort for the field measurement of pH and Eh consists of pre-measurement calibration and post-measurement verification, using a standard referencesolution each time, as appropriate to the sample pH and Eh. The QC effort for fieldconductivity and dissolved oxygen measurements will include daily calibration of theinstrument, using standard solutions of known conductivity. A detailed discussion of QCprocedures for field instrumentation is included in Section 6.1. The QC for geotechnical

analyses will be in accordance with method protocols which are presented in

Appendix F.

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3.3 DATA QUALITY INDICATORS

The quality of sampling and analysis will be assessed using five data quality indicators:accuracy, precision, completeness, representatives, and comparability. Using the DQOprocess, the data use categories for all samples collected have been established in theRI/FS Work Plan. These categories are: Site characterization; Site boundarydelineation; risk assessment; and evaluation of alternatives. Data quality indicator

objectives (presented in this section) that are not met will be handled as discussed inSection 13.

The definition and specific use of data quality indicators for sampling is different thanfor analysis as discussed in the following sections of this text.

3 J.I Accuracy

Accuracy is the degree of agreement of a measurement to an accepted reference or truevalue. An evaluation of the accuracy of a measurement system provides an estimate ofbias. The accuracy of an analytical method is evaluated by analyzing known referencestandards. The percent recovery achieved by analysis of known reference standards, or

laboratory control samples will be used to define the accuracy for the compounds ofinterest. Reference samples will be analyzed in accordance with the frequencies

prescribed by the methods.

The estimated ranges of accuracy for each measurement parameter are defined withinthe analytical test methods. Acceptable accuracy measures are also dependent on thesample matrix. Tables 3 through 5 provide accuracy and precision objectives for matrix

and surrogate spikes.

The accuracy of field measurements of pH and Eh will be assessed through pre-measurement calibrations and post-measurement verifications, using at least two

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standard buffer solutions. The two measurements must each be within 0.1 standard unit

of buffer solution values. The electrode will be withdrawn, rinsed with deionized water,

and re-immersed between each replicate. The instrument used will be capable of

providing measurement to 0.1 standard unit.

332 Precision

Precision is the measure of variability between individual sample measurements under

prescribed conditions. Precision will be assessed by duplicate analyses of environmental

samples (inorganics and PCDDs/PCDFs) and the analysis of matrix spike/matrix spike

duplicate (MS/MSD) samples (organics). The precision will be expressed in terms of

relative percent difference (RPD). Precision objectives for laboratory QC sample

analyses are provided in Tables 4 and 5. Precision for field duplicate samples will be

evaluated using the QC objective of ± 50 percent in conjunction with review of

laboratory precision (i.e., field duplicate samples will be used to evaluate both laboratory

precision and sample heterogeneity).

3.3.3 Completeness

Completeness is defined as the percentage of the total measurements which are judged

to be valid in accordance with the methods identified in Section 7. The completeness

objective is to generate a sufficient amount of valid data to support each of the data use

categories for the former Koppers Company, Inc. Newport Site investigation objectives.

The data set used to determine completeness includes all QC check analyses verifying

precision and accuracy for the analytical protocol. In addition, all data are reviewed in

terms of stated goals in order to assess the sufficiency of the data base. Completeness

is calculated as the number of usable data points obtained divided by the amount of

sample data analyzed, multiplied by 100. The completeness objective will be 90 percent,

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evaluated on a per analysis basis. The usability of data will be determined dependingupon its intended use, as discussed in Section 8.3.

33.4 Representativeness

Representativeness is the degree to which data accurately and precisely represent acharacteristic of a population, parameter variations at a sampling point, or anenvironmental condition.

Representativeness is a qualitative parameter most concerned with the proper design of

the sampling program. The representativeness criteria may be satisfied by makingcertain the sampling locations are selected properly and that a sufficient number ofsamples are collected to fulfill program objectives. The rationale used to select samplinglocations is described in detail in the Work Plan.

Duplicate samples will be collected and utilized as a means to assess fieldrepresentativeness. By definition, duplicate samples are representative of a given pointin space and time. Representativeness will also be maintained during the sampling effort

by performing all sampling in compliance with the procedures described in detail in the

FSP.

3.3.5 Comparability

Comparability expresses the confidence with which one data set can be compared toanother. Comparability can be related to accuracy and precision as these quantities aremeasures of data reliability. Data are comparable if siting considerations, collectiontechniques, measurement procedures/methods, and reporting are equivalent for the

samples within a sample set. A qualitative assessment of data comparability will be

made of applicable data sets.

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3.4 SENSITIVITY OF ANALYSIS

The fundamental QA objective with respect to the sensitivity of the analytical data is to

achieve quantitation limits (sensitivities) as specified in the analytical protocols. Thesensitivities for the subject analyses are presented in the appropriate method(s).

Sensitivities to be achieved for this program are also presented in Tables 6 through 10.

The presented quantitation limits will be attained, barring any chemical interferences ordilutions required due to matrix interferences.

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4.0

SAMPLING AND FIELD PROCEDURES

4.1 SCOPE OF WORK

The scope of work for the former Koppers Company, Inc. Newport Site is detailed in the

RI/FS Work Plan. Methods for data collection are detailed in the FSP.

42 QUALIFICATIONS OF SAMPLING PERSONNEL

The personnel responsible for sampling and other field activities will have the experience

for sampling the different matrices. They will have read and become familiar with the

appropriate QAPjP and FSP sections. They will be cognizant of the importance and

"level of quality control that must be maintained in order to produce the most

representative samples. Loss of volatiles is always of major concern and, where sampling

for volatiles is required, particular care will be executed. The level of completeness

hinges on the proper taking of samples; therefore, sampling activities will be

appropriately monitored throughout the Site investigative activities at the former

Koppers Company Newport Site by WCC QA/QC personnel.

43 FIELD INVESTIGATION

The field investigation will involve a number of tasks and methods for data collection

at the Site. Communication with the laboratory will be maintained to address the

logistics of analytical bottleware shipments to the Site and sample shipments to the

laboratory. Procedures and methods for the field investigation are detailed in the FSP.

The following is a summary of the general field tasks and what they encompass:

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Site Surveys

• Soil sampling locations

• Wetland boundary delineation

• Location of NPDES outfall

• Location of sites of archaeological and historical significance

• General ambient air quality

• Vegetation survey

• Qualitative habitat survey

• Qualitative wildlife survey

• Terrain conductivity survey of portions of the Site

Drilling and Soil Sampling

• Soil characteristics (grain size, moisture content, permeability)

• Lithology

• Stratigraphy

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Soil quality - field screening (headspace analyses, visual observation, andolfactory evidence)

Soil quality - laboratory analysis

Groundwater Monitoring and Sampling

• Aquifer conditions

• Groundwater quality - field observations

• Groundwater quality - laboratory analysis

• Water levels

Surface Water and Sediment Sampling

• Location of wetlands and drainageway stations

• Field water chemistry measurements (temperature, pH, conductivity)

• Hydrological conditions (tidal stage, flow velocity, water depth)

• Surface water and sediment quality - laboratory analysis

• Sediment characteristics (color, texture, grain size)

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Inorganic and organic substrate components (gravel, sand, sticks, plant

material)

Presence of aquatic vegetation (periphyton, algae, macrophytes)

A number of quality assurance measures are associated with specific tasks and are

detailed in the FSP and the HSP. Details of the following .procedures are included inthe FSP.

Drilling Program

• Utility clearances

• Drilling requirements

• Decontamination protocol

• Water sources

• Protection of water yielding zones

• Backfilling

Sampling Procedures

• Sampling methods

• Sampling equipment

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Decontamination protocol

Field screening (headspace analysis, visual observation, and olfactory

evidence)

Groundwater Monitoring

• Well construction requirements

• Screen and casing requirements

• Location and depth

• Well development

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5.0

SAMPLE AND DOCUMENT CUSTODY PROCEDURES

Verifiable sample custody will be an integral part of all field and laboratory operations

associated with the Koppers Company, Inc. Newport Site investigations. Traceable stepswill be taken in the field and laboratory to document and ensure that all samples havebeen properly acquired, preserved, and identified. The following sections provide thedetails related to carrying out verifiable field and laboratory documentation.

5.1 FIELD DOCUMENTATION

Bound field logbooks will be used to record all pertinent field data collection activities

performed or observations made. Documentation in the field logbook will be sufficientto reconstruct the sampling situation without relying on the memories of the field teammembers. Entries into the field logbook will include, but are not necessarily limited to,the following information:

• Project name• Date and time

• Sample location• Sample number

• Sample depth• Media type• HNU/OVA readings

• Sampling personnel present• Type of health and safety clothing/equipment used

• Analyses requested• Time of sample collection

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• Sample preservation

• Field observations, to include soil description (if relative)

• Weather conditions

• Depth to water

• Soil descriptions

• Other project-specific information, such as documentation of reagent or

supply sources.

In addition, field sketches will be made in the field logbooks when appropriate, with

reference points tied to existing structures in the area (i.e., trees, fence posts, buildings).

Field logbooks will be identified by a project-specific number (i.e., Logbook #1 for

Project Number 91C2628, etc.) and stored in the field project files when not in use. At

the completion of the field activities, the logbooks will be maintained in the central

project file for the CERCLA required time frame.

52 SAMPLE IDENTIFICATION

All samples will be assigned a sample Identification (ID) Number and a Location

Number as the sample is collected. Trie tt> NB. wTll be used to fill out the C-O-C. The

correlation between the ID number and Location Number will be maintained in the field

book and sample tracking forms. The Location Number will be used in data

management in the analysis of sample results. The ID number will be a six digit number

to conform with EPA sample ID number required by CLP SOW formats and to avoid

any sample labeling confusion between WCC and the Lab.

The ID number will consist of a two letter prefix per matrix as follows: SW for surface

water; SOW for groundwater; SD for sediment; and SL for soil and a sequential four

digit number.

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The sampling station, sample type, and sample sequence identifiers (see subsequent

discussion) will be established prior to field activities for each sample to be collected.On-site personnel will obtain assistance in defining any special sampling requirementsfrom the Project Manager.

52.1 Sample Location Numbers

Once the data has been entered into the database, a location number will be used toaccess data. The location numbers will be assigned to each sample collected and aremore descriptive of the sample to allow easy recognition of sample type and sites. Thelocation number is more flexible than the identification number, and although it will beincluded on the COCs in the location space, it will be more of a data management toolthan a tracking device. Location numbers will be given to every sample as it is collected.

Identification numbers will only be assigned to samples submitted to the laboratory foranalysis.

The location number can vary from eight to eleven digits and will describe matrix, site(PAOI or drainageway or basin), location within the site, depth of sample, and type ofQA/QC. An example of a sample location number is as follows:

SB21612R SAMPLE LOCATION NUMBER

• SB 21612R Sample Matrix

The sample matrix is indicated by the first two digits of the location number. Two lettershave been assigned for each matrix on the site.

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Location No. Matrix

SB

SDSW

GWPT

soil boring

sedimentsurface watergroundwater

peat

SB 2 1612R Sample Site

Starting with the third digit in the location number, the site location is represented byeither a single number, as in the case of PAOIs, or a one-to-three-letter designation fordrainageway.

Location No. Site

12

3467

PAOI 1PAOI2

PAOI 3PAOI 4PAOI 6Background

FPSPKP

HR

HRM

WCWCM

Fire PondSouth Pond

Area K Pond

Hershey Run

Hershey Run MarshWest Central DrainagewayWest Central Drainageway Marsh

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Location No.


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Site

ECECMCCRCMMCMDWH

CM

E

East Central Drainageway

East Central Drainageway MarshCentral DrainagewayChristina RiverChurchmans MarshChurchmans DrainagewayWhite Clay Creek

Central Drainageway MarshEast Drainageway

• SB2 16 12R Sequence

The sequence portion of the location number is assigned to the sample or boring in

relation to the sample site. 'These sequences are given on Figure 4 Sample Location

Map.

• SB216 12 R Sample depth

The sample depth portion of the location number indicates the bottom depth of the

sample. In the example, the bottom depth of the sample is twelve feet. Soil boring

sample depth will always be in feet. Sediment sample depth will always be in inches.

SB21612 R QA/QC

Field QA/QC samples, MS/MSD or MS/laboratory duplicate samples will be identified

by the last digit of the location number.

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Location No. QA/AC Type

D Field duplicate

F Field blank

R Rinsate blank

MS MS/MSD or MS/laboratory duplicate

T Trip blank

Duplicate sample will not be identified to the laboratory on the COCs or sample label.

Duplicates will be tracked in the field book and sample tracking sheets.

522 Sample Labels

Sample labels will be filled out as completely as possible by a designated member of the

sampling team prior to beginning field sampling activities each day. The date, time,

sampler's signature, and the last field of the sample identification number will not be

completed until the time of sample collection. All sample labels will be filled out using

waterproof ink. At a minimum, each label will contain the following information:

• Sampler's company affiliation

• Site location

• Sample identification code

• Date and time of sample collection

• Type of Sample (grab or composite)

• Analyses required

• Filtered or Unfiltered (as appropriate)

• Method of preservation (if any) used

• Sample matrix (i.e. soil, groundwater)

• Sampler's signature

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523 Sample Containers

Certified, commercially clean sample containers will be obtained from the analytical lab.

The bottles will be labeled by the lab to indicate the type of sample to be collected.Required preservatives will be prepared and placed in the bottles at the laboratory priorto shipment to the Site. Table 11 lists appropriate sample containers for the specificanalyses required for this project.

5.2.4 Sample Preservation

Sample preservation efforts will commence at the time of sample collection and willcontinue until analyses are performed. Samples will be stored on ice at 4°C in coolersimmediately following collection. Sample preservation requirements are given in Table11. Where appropriate, chemical preservatives will be included in sample containers bythe laboratory. Samples which require filtration will be preserved after the sample hasbeen filtered. Specific procedures for sample filtration are provided in Section 2.2.4 ofPTG 9 presented in Appendix A of the Field Sampling Plan.

5.2.5 Sample Handling and Shipping

The technical holding time is specified as the maximum allowable time between sample

receipt by the laboratory (Level 4) or collection (Level 3) and analysis and/or extraction,based on the analyte of interest and stability factors, and preservative (if any) used.

Allowable technical holding times are listed in Table 11. The holding times presentedrequire samples to be received by the laboratory within two days of collection. Aftercollection, sample labels will be completed and samples stored on ice in an insulated

cooler. Samples will be placed right side up in a cooler with ice for delivery to the

laboratory. Samples will be hand delivered or shipped by overnight express carrier for

delivery to the analytical laboratory. All samples will be received by the project

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laboratory(s) within two days of collection and will be maintained prior to and during

shipment. A chain-of-custody form will accompany each cooler (see Section 5.3).

5.3 CHAIN-OF-CUSTODY PROTOCOL

53.1 Field

Each cooler containing samples sent to the analytical laboratory will be accompanied by

a chain-of-custody (COC) record form. This section describes the procedures for sample

documentation utilizing COC protocol.

The primary purpose of the COC procedures is to document the possession of the

samples from collection through storage and analysis to reporting. COC forms will

become the permanent records of all sample handling and shipment. The Field Task

Leaders or their designees will be responsible to the Project Manager for monitoring

compliance with COC procedures.

The field team members are responsible for the care and custody of the samples

collected until the samples are transferred to another party, dispatched to the laboratory,

or disposed. The field team, under the direction of the Field Task Leader, is responsible

for enforcing COC procedures during fieldwork. The COC procedures are provided as

follows:

• During the day of sample collection, the COC form is completed for the

sample collected. The sample identification number, location number,

sample date and time, type and size of sample container, type of sample

(MS/MSD or MS/laboratory duplicate sample), analysis requested, level

of data quality required, preservative, notation as to whether the sample

was field filtered, and method of shipment is recorded on the form.

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• When the form is completed or when all samples have been collected thatwill fit in a single cooler, the field team members will cross-check the formfor possible errors and sign the COC record. Each cooler will beaccompanied by a separate COC, sealed in a Ziploc*-type bag, and tapedto the inside of the cooler lid.

• After the COC form has been completed and the samples have been

packaged as described above, and prior to a shipment to the laboratory,the cooler will be sealed with a COC seal. The purpose of the COC sealis to indicate whether the cooler has been opened or tampered with duringshipment.

When transferring custody of the samples, the individual relinquishing custody of thesamples will verify sample numbers and condition and will document the sampleacquisition and transfer by signing and dating the COC. This process documents samplecustody transfer from the sampler, usually through an express courier, to the analyticallaboratory. A copy of each COC form is retained by the sampling team for the project

file, and the original is sent with the samples.

In conjunction with data reporting, the analytical laboratory will return the original ora photocopy of the original COC in a Letter of Receipt (LOR) for all shipmentsreceived for purposes of noting problems in sample packaging, COC, or samplepreservation, to the Project Manager for inclusion into the central project file.

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5.3.2 Laboratory Custody Procedures

Laboratory COC, sample storage, and dispersement for analysis and associateddocumentation are found in the LQAPs of Appendices A, B and C of this QAPjP.

5.4 PROJECT FILE

A central project file, containing complete project documentation of all aspects of theactivities associated with the former Koppers Company, Inc. Newport Site investigations,will be maintained by the Project Manager. This file will include:

• Project plans and specifications• Field logbooks and data records

• Maps and drawings• Sample identification documents• COC records• LOR records• The entire analytical data package provided by the laboratory, including

QC documentation

• Data review notes

• Selected references and literature• Report notes and calculations• Progress and technical reports• Correspondence

• Other pertinent information

Project documentation will be checked for completeness to include peer reviews,

checking of calculations, etc., before being included in the file.

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6.0

CALIBRATION PROCEDURES AND FREQUENCY

All field and laboratory instrumentation will be calibrated prior to and during continueduse. The calibration and maintenance history of the project-specific field and laboratory

instrumentation is an important aspect of the project's overall QA/QC program. Assuch, all initial and continuing calibration procedures will be implemented by trained

personnel following the manufacturer's instructions and EPA specifications to ensure the

equipment is functioning within the tolerances established by the manufacturer and the

EPA method-specific analytical requirements.

6.1 FIELD INSTRUMENTS AND EQUIPMENT

The calibration and general maintenance of field instrumentation will be theresponsibility of the Field Task Leaders and the Site Health and Safety Officer. Table13 summarizes the calibration and maintenance requirements for field instrumentation

which may be used during this program. All documentation pertinent to the calibration

and/or maintenance of field equipment will be maintained in an active field logbook.

Entries made into the logbook regarding the status of any field equipment will contain,

but are not necessarily limited to, the following information:

• Date and time of calibration• Name of person conducting calibration

• Type of equipment being serviced and identification number (such as the

serial number)

• Reference standard used for calibration (such as pH of buffer solutions)

• Calibration and/or maintenance procedure used

• Other pertinent information

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Equipment that fails calibration and/or becomes otherwise inoperable during the fieldinvestigation will be removed from service and segregated to prevent inadvertent use.

Such equipment will be properly tagged to indicate that it should not be used until the

nature of the problem can be assessed. Any equipment requiring repair or recalibrationmust be approved for use by the Field Task Leader or Site Health and Safety Officerprior to placement back into service. Equipment that cannot be repaired or recalibratedwill be replaced.

Field instruments will be used to measure pH, Eh, specific conductance and temperaturein both groundwater and surface water samples as described in Project Technical

Guidance No. 9 or the Field Sampling Plan and Remedial Work Plan Section 4.6.4.2,respectively.

The pH meter must be calibrated each day before taking any readings of samples.Calibration and operation of the pH meter will follow the manufacturer's specificinstructions. In general, calibration is done by adjusting the meter with standard buffersthat bracket the expected pH of the field water. Calibration will consist of the followinggeneral procedures:

1. Adjust the reading of the pH meter using the intercept knob with theelectrode placed in the pH 7 buffer by using the calibration knob. Rinse

the electrodes with distilled water between buffer adjustments.

2. With the electrode placed in the pH 4 buffer, adjust the reading of the

meter with the slope knob. Adjust using the temperature knob if themeter has no slope knob.

3. Repeat steps 1 and 2 until the meter gives acceptable readings for all the

buffers used for calibration.

Note: Always used the same electrode for measurements that was used in the calibration.

Recalibrate the meter if the electrode is replaced. Although the temperature setting on

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the pH meter often does not match the sample temperature after calibration, the pH

readings will still be accurate in these cases provided that the response to the buffers iscorrect.

The oxidation/reduction (redox potential) will be measured with the pH meter used asa potentiometer with the probes replaced with combination platinum/reference

electrodes (silver/silver chloride type). The instrument is adjusted to a specific millivolt

potential prior to use using a ferrous-ferric reference solution. The probe should becleaned with distilled water between each sample. Measurements should be made assoon after the sample collection as possible to reduce the exchange of oxygen in thesample with that in the atmosphere.

The conductivity meter must be calibrated each day before taking field measurements.Record time, temperature, and instrument response in the meter notebook. Calibration

is done by noting the response of the meter to several standard conductivity solutionswhich bracket the values expected to be measured in the field. Standards of 100, 1000,and 10,000 /xmhos/cm should be adequate for the samples expected. If the instrumenthas a calibration adjustment, set the response to match the standards. Otherwise, simply

record in the field notebook the instrument response to each standard.

The OVA and HNu screening instruments will be calibrated each day by introducing

known methane (for OVA) and isobutylene (HNu) standards and adjusting theinstruments to the known concentrations. Calibration procedures for monitoringequipment are presented in Attachment 6 to the Health and Safety Plan.

62 LABORATORY INSTRUMENTATION

The calibration procedures that will be used for chemical analyses of the environmentalsamples collected during the RI will be in accordance with the analytical methods

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presented in Section 7.0 and Table 12. As such, all method target analytes will beincluded in calibration standards.

6.2.1 Standard/Reagent Preparation

The generation of quality data is dependent on the purity/quality and traceability of the

standard solutions and reagents used in the analytical operations. To ensure that

standards are of highest purity, all primary reference standards and standard solutionswill be obtained from the National Institute of Standards and Technology (NIST), theEPA Repository, the USAGE, or other reliable commercial sources. The projectlaboratory(s) will enter all standards and standard solutions into a database thatidentifies the supplier, lot number, purity/ concentration, receipt/ preparation date,preparer's name, method of preparation, expiration date, and all other pertinent infor-

mation.

Standard solutions will be validated prior to use. Validation procedures can range froma check for chromatographic purity to verifying of the standard's concentration. Stockand working standards will be checked regularly for signs of deterioration, such asdiscoloration, precipitation, or concentration changes. Care will be exercised in theproper storage and handling of standard solutions, and all containers will be labeled as

to compound, concentration, solvent, expiration date, and preparation data (initials of

preparer/date of preparation). Reagents will be examined for purity by subjecting an

aliquot or subsample to the corresponding analytical method, as well.

Maintenance of essential information on specific standards or reagents will be performedin accordance with the LQAPs (Appendices A, B, and C). Information on reagents andstandards will be used to prevent shelf-life exceedances, note proper storage techniques

to inhibit deterioration and degradation, and to maintain a listing of working standardsolutions prepared from the same stock solution. Management and periodic auditing of

reagents and standards will be performed by the contract laboratory(ies).

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622 Documentation

Documentation of all calibration activities will be maintained by the laboratory and will

also be submitted with the data packages when required or as requested. This

information will become a part of the central project record and could be retrieved as

necessary. Calibration documentation requirements are presented in Appendix G.

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7.0

ANALYTICAL PROCEDURES

7.1 LABORATORY PROCEDURES

The general laboratory procedures or methods planned for investigations at the formerKoppers Company, Inc. Newport Site are summarized in Table 12. TCL, TAL andPCDD/PCDF analyses of all soil, sediment, surface water, and first round monitoringwell groundwater samples will be accomplished using Routine Analytical Service (RAS)CLP protocols. Residential well analyses for TCL parameters will be accomplished usingthe EPA CLP low concentration method and all TAL analyses will follow RAS CLPprocedures. The laboratory will be audited for those CLP parameters for which it doesnot have a CLP contract.

Data from first round monitoring well and residential well sampling will be reviewed todetermine if alternative methods may be employed during remaining sampling rounds

to meet drinking water criteria where applicable. Alternative methods which may beused include EPA methods 524/525, 550.1, or other approved methods. Proposed

alternative methods, along with the first round of non-validated sample results will bepresented to the EPA thirty days prior to the second round of sampling. QA/QCprocedures which may vary due to the use of alternative methods in the second round

of groundwater sampling will be included for EPA review. Method detection limits formethod 524/525, 550.1 are included in Appendix E. Table 2 shows the number ofsamples to be taken for each parameter. The QC review and data validation procedures

are provided in Section 8.0. Specific laboratory practices for the analytical methodsidentified in Table 12, including sample preparation, sample tracking, and documentationcontrols, are provided in the LQAPs (Appendices A, B and C) and are deemed adequate

for this project. The text of this QAPjP supersedes the LQAPs. Wadsworth/Alert

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(primary) and Lancaster (backup) will provide analytical services for this program.

ENSECO-CAL will be subcontracted by Wadsworth/Alert for PCDD/PCDF analysis.Benthic samples will be analyzed by WCC personnel specializing in benthic taxonomy,or an EPA-approved subcontractor. Geotechnical samples will be analyzed byWoodward-Clyde Consultants and Bowser Mourner. A summary of the types of

geotechnical samples and appropriate methods are presented on Table 12a.

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8.0

DATA REDUCTION REPORTING AND VALIDATION

The analytical data generated by the laboratory will be checked for accuracy, precision,and completeness. The data validation process for this project will consist of datageneration, reduction, and two levels of review.

8.1 DATA REDUCTION

The first level of review, which may contain multiple sublevels, will be conducted by theanalytical laboratory's data reviewer who has the initial responsibility for the correctnessand completeness of the data. All data are generated and reduced following protocolsspecified in the LQAPs provided in Appendices A, B and C. The laboratory datareviewer will evaluate the work quality, based on an established set of laboratoryguidelines and this QAPjP. This person will review the data package to ensure that:

• Sample preparation information is correct and complete

• Analysis information is correct and complete• The appropriate SOPs have been followed• Analytical results are correct, and complete and reported with contract-

required units (CLP)

• QC samples and criteria are within established control limits• Blanks are within appropriate QC limits• Special sample preparation and analytical requirements have been met• Documentation is complete (all anomalies in the preparation and analysis

have been documented; out-of-control forms, if required, are complete;

holding times are documented)

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The laboratory will perform the in-house analytical data reduction and QA review under

the direction of the laboratory data review supervisor. The laboratory program

administrator is responsible for assessing data quality and advising the project manager

of any data which were rated "preliminary" or "unacceptable", or other notations whichwould caution the data user of possible unreliability. Data reduction, QA review, andreporting by the laboratory will be conducted as follows:

• Raw data produced by the analyst will be processed and reviewed forattainment of quality control criteria as outlined in this QAPjP and/orestablished EPA methods and for overall quality

• After entry into the laboratory information management system (LIMS),a computerized report will be generated and sent to the laboratory datareviewer

• The laboratory will not subtract blank results from analytical results. Theprocedures for handling blank results are described in the NationalFunctional Guidelines for Organic Data Review (referenced in Section

8.3).

• The data reviewer will decide whether any sample re-analysis is required

• Upon acceptance of the preliminary reports by the data reviewer, final

reports will be generated

Data reduction procedures will be those specified in the USEPA CLP procedures

specified for this project, and those of the project laboratory(s).

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%2 REPORTING DELIVERABLES

Units for the analytes of interest will be reported in micrograms per kilogram (ug/kg)or milligrams per kilogram (mg/kg) for soil and sediment matrices and micrograms perliter (ug/1) for water. Water quality parameters, such as chloride, will be reported in

milligrams per liter (mg/1).

8.2.1 Non-CLP Deliverables (Level 3) - Geotechnical Analyses

The laboratory(s) will prepare and retain analytical and QC documentation. The

laboratory will report the data as a delivery group of 20 samples or less, along with QCsupporting data within 35 calendar days of receipt of the final sample collection in eachSample Delivery Group (SDG). The laboratory(s) will provide the following hard copyinformation (where applicable) in each analytical data package for samples analyzed by

Level 3 protocols:

• Sample results

• QC sample results

• Raw data

• Case narrative

• Date of sample collection

• Date of sample receipt

• Date of sample analysis

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• Method for sample preparation

• Analytical methodology

• Methods of sample cleanup (if used)

• Dates of analyses

• Laboratory control recoveries

• Comparison of all QC data to QC acceptance criteria

• Accompanying sample, calibration, and QC raw data

The case narrative will describe any and all QA/QC problems encountered during

analysis of the samples. For each sample for which QA/QC problems are encountered,the following specific information will be reported in the case narrative:

• WCC sample identification number

• Data with outlying quality control

• Specific analytical problem that occurred

• The corrective action that was taken or attempted to resolve the problem

822 CLP Deliverables (Level 4)

The analytical reports will conform to all reportable and deliverable requirements as

specified in the current USEPA CLP Methodologies specified in Table 12. Laboratories

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will be required to submit two copies of the sample data summary package and one copy

of the sample data package within 35 calendar days of receipt of the final samplecollected in each Sample Delivery Group (SDG). PCDD/PCDF sample data summary

packages (2) and sample data packages (1) must be submitted within 45 calendar daysof receipt of the final sample from each SDG. All data must also be submitted onfloppy disk as discussed in Section 8.4 of this QAPjP.

8.3 VALIDATION/REVIEW

An independent review of the data package will be performed to determine conformancewith each appropriate analytical method identified in Table 12. The guidelinesestablished in this QAPjP and in the following documentation will be used as a basis forthe data validation:

1. Region III Modifications to National Functional Guidelines for OrganicData Review, Multi-Media, Multi-Concentration OLMOl.O-OLMOi.6)June, 1992. USEPA Region III.

2. Region III Modifications for Pesticide/Arochlor Data Review, May 1993.

USEPA Region HI.

3. Region III Modifications to the Laboratory Data Validation FunctionalGuidelines for Evaluating Inorganics Analyses. April 1993, USEPA.Region III

4. Functional Guidelines for Evaluating Data from IFB WAF4-A002

Chemical Analytical Services for 2,3,7,8-Tetrachlorodibenzo-p-dioxin.

USEPA, October, 1985.

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Following validation of the data packages, data assessment with respect to fulfilling

DQOs and usability, will be accomplished by the QA/QC Officer and the ProjectManager. This assessment will include sample collection, sample handling, field data,consideration of rinsate sample, trip blank and field blank samples, and method blankvalues, field duplicate values, and additional flagging or qualifying of data. Exceedanceof a holding time alone does not invalidate a sample result. Based on guidance

documents, holding times are considered guidelines and the validity of the data is leftto the discretion of the reviewer. The usability of the data for each data use categorywill be determined by the QA/AC officer and the Project Manager with input from each

task leader. It is possible that data could be unusable for one data use category butusable for another.

8.4 REQUIREMENTS FOR LAB DATA RESULTS ON DISKETTES

The laboratory shall supply the results of analyses on floppy disks suitable for readingby the DOS operating system Version 3.30 or greater. The floppy disks may be 5-1/4-inch in size formatted to 320 KB double-sided, double density, 1.2 MB double-sided, highdensity or they may be 3-1/2-inch 720 KB double-sided, double density or 1.44 MB

double-sided, high density. The laboratory will clearly label the diskettes with thefilename as defined in the following section and the formatted capacity of the diskette.Also, the laboratory must clearly make distinction between the letter "O" and the number

zero ("0"), and between the letter "I," the letter "L" and the number one ("1") and thenumeral seven ("7") when labelling diskettes and naming files.

For organic analyses, the results of the analyses shall be contained in a single file on afloppy diskette conforming to the EPA CLP Organic Analyses Disk Deliverables Format

A, No duplication of filenames on multiple floppy disks will be permitted. The

laboratory shall conform exactly with the file naming convention specified in the EPA

CLP specification with no deviations permitted. The laboratory shall conform exactly

with the EPA CLP Organic Analyses Disk Deliverables Format A record layout with no

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deviations permitted. In particular, the EPA Sample Number field will remain intact

and will not be corrupted with extraneous information.

For inorganic analyses, the results of the analyses shall be contained in a single file ona floppy diskette conforming to the EPA CLP Inorganic Analyses Disk Deliverables

Format A. The laboratory shall include the results from ALL analyses for a samplegroup in a single file, even if the analyses are performed by different departments. Noduplication of filenames on multiple floppy disks will be permitted. The laboratory shallconform exactly with the file naming convention specified in the EPA CLP specificationwith no deviations permitted. The laboratory shall conform exactly with the EPA CLP

Inorganic Analyses Disk Deliverables Format A record layout with no deviations

permitted. In particular, the EPA Sample Number field will remain intact and will notbe corrupted.

For analyses other than Level 4 performed by the laboratory, the laboratory shallprovide a written description of the format and record layout of the file. The data fileshall be in ASCII format. The laboratory shall not vary the record format during theproject without consultation with the client. The results of the analyses shall be

contained in a single file on a floppy diskette conforming to the laboratories' written

definition of the file record layout with no deviations permitted. The laboratory shallconform to a file naming convention mutually agreed upon by the laboratory and theclient. No duplication of file names on multiple diskettes will be permitted. In

particular, the EPA Sample Number field must be 7 characters long.

To facilitate placing large lab results files on floppy disks, the laboratory will be

permitted to use a data compression program in order to reduce the space requirementsneeded by the file. If data compression programs are used, the laboratory has a choice

of the following: PKZIP Version 1.10 by PKWare, or ARC Version 6.02 by SEA -- withthe preference on PKZIP. The files may be raw archives (*.ZIP or *.ARC files) or they

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may be converted into self-extracting archives (*.EXE) at the discretion of the

laboratory.

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9.0

INTERNAL QUALITY CONTROL CHECKS

9.1 FIELD QC CHECKS

Field quality control checks will include the review and approval of all field docu-mentation by the Field Task Leader or his/her designee. The Field Task Leader willperform random spot checks on the field team(s) daily. Conformance with established

procedures will be checked. Nonconformances will be corrected and reported to theProject Manager orally or by a written memo. Samples identified as nonconforming willbe disposed and new samples obtained. In the event that a serious deficiency(nonconformance) is identified, the sampling team's prior work will also be reviewed.

Quality control of field sampling will involve the collecting and analyzing of QC samplesin accordance with the applicable procedures described in Section 3.0 and in accordancewith the frequencies provided in Section 3.2.1 of this document.

92 LABORATORY QC CHECKS

Two types of quality assurance checks will be utilized to assess the production of

analytical data of known and documented quality. These include:

• Program quality assurance• Analytical method quality control

The stated objectives of the laboratory QA/QC Program are to:

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• Ensure that all procedures are documented, including any changes inadministrative and/or technical procedures

• Ensure that all analytical procedures are conducted according to sound

scientific principles and have been validated

• Monitor the performance of the laboratory by a systematic inspection

program and provide for corrective action as necessary

• Collaborate with other laboratories in establishing quality levels, as

appropriate

• Ensure all data are properly recorded and archived

All laboratory procedures are documented in writing as either standard operatingprocedures (SOPs) or method procedures (MPs), which are edited and controlied.Internal quality control procedures for analytical services will be conducted by thecontracted laboratories in accordance with their Corporate Quality Assurance Plan and

SOPs. These specifications include the types of audits required (matrix spikes, surrogatespikes, reference samples, control samples, blank samples), the frequency of each audit,the compounds to be used for sample spikes and surrogate spikes, and the quality

control acceptance criteria for these audits.

The contracted laboratories will document in each data package provided, that analyticalQC functions have been met. Any samples analyzed in nonconformance with outlying

QC criteria will be carefully reviewed to see if outlying data were due to a matrix effector to laboratory procedures not being in control. The laboratory will re-analyze the

samples if the laboratory procedures were not in control, as assessed by laboratorycontrol samples and other data specific to the analysis, and if sufficient sample volume

is available. It is expected that sufficient volume of samples will be collected for re-

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analysis if required. QC check samples analyzed (method blank sample, rinsate sample,

etc.) will be run concurrently with the sample batch (maximum of 20 environmental

samples) to which they are assigned. The method blank samples will be analyzed at a

rate of 1 in 20. MS/MSDs and MS/laboratory duplicates will be analyzed at frequency

of 1 per 20. These MS/MSD and MS/laboratory duplicate samples will be designated

on the chain-of-custody and extra sample volume will be collected for water samples.

MS/MSD samples will not be analyzed for samples analyzed by low level CLP protocols,

but will be substituted with laboratory control samples in accordance with method

protocol.

The data on the accuracy (matrix spikes) and precision (RPD data) will be used to

evaluate the laboratory performance and matrix effects. The method blank data will be

used to evaluate the background contamination levels.

92.1 Matrix Spike Sample

A matrix spike sample is an environmental sample to which known concentrations of

analytes have been added. The matrix spike is taken through the entire analytical

procedure and the analyte recovery calculated. Results are expressed as percent

recovery of the known amount spiked. The matrix spike is used to evaluate the effect

of the sample matrix on the accuracy of the analysis. Matrix spikes samples and

MS/laboratory duplicates will be analyzed at a frequency of 5 percent, and will be

designated on the chain-of-custody by field sampling personnel. Extra sample volume

will be collected for this purpose, if necessary. A determination will be made in the field

concerning representative matrices. MS samples are not required for the low level CLP

method. Quality control criteria for these analyses are presented in Tables 4 and 5.

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922 Matrix Spike Duplicate Sample

A matrix spike duplicate sample is an environmental sample which is divided into two

separate aliquots, each of which is spiked with known concentrations of organic analytes.The two spiked aliquots are processed separately and the results compared to evaluatethe effects of the matrix on the precision and accuracy of the analysis. Results areexpressed as relative percent differences (RPD) between the percent recoveries. Matrixspike/matrix spike duplicate samples (organics), and matrix spike/laboratory duplicatesamples (inorganics and PCDDs/PCDFs) will be analyzed at a frequency of 5 percent.

MS samples are not required for the low level CLP method. Quality control criteria forthese analyses are presented in Tables 4 and 5.

9.2.3 Method Blank Sample

A method blank sample consists of analyte-free deionized water or solid. Each methodblank is carried through each step of the analytical method. Method blank samples willbe analyzed at a rate of one per batch of 20 environmental samples analyzed for thisproject.

9.2.4 Laboratory Control Samples (LCS)

Laboratory control samples (LCS) are well-characterized, laboratory-generated samples

used to monitor the laboratory's day-to-day performance of analytical methods. LCS will

be used for the CLP method for metals, low level organics analyses and USEPAmethods for TSS and alkalinity. Certain LCS are used to monitor the precision andaccuracy of the analytical process independent of matrix effects. Other LCS are usedto identify any background interference or contamination of the analytical system which

may lead to the reporting of elevated concentration levels or false positive data. One

LCS will be analyzed per analytical batch.

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The results of the LCS are compared to defined laboratory acceptance criteria to

determine whether the laboratory system is "in control". Controlling lab operations with

LCS (as opposed to matrix spike/matrix spike duplicate samples) offers the advantage

of being able to differentiate low recoveries due to procedural errors from those due to

matrix effects. If the LCS results for this project meet acceptance criteria, the method

will be considered in control. Recovery control limits for metals and organics (low level

CLP) are provided in their respective CLP method. Recovery control limits for TSS and

alkalinity are presented in Wadsworth/Alert's LQAP.

92.5 Surrogate Compounds, Internal Standards, and Cleanup Standards

Surrogates are isotopically labeled or halogenated compounds in most cases and are

added to all samples (including laboratory QC samples) submitted for organics analyses

(VOCs, BNAs, and Pesticides/PCBs) prior to sample preparation in extraction in order

to monitor the preparation and/or extraction efficiency. Appropriate surrogate

compounds and acceptable percent recovery control limits which will be used in this

project by the laboratory(s) are presented in Table 3.

Internal standards will be added to samples and blanks after preparation and/or

extraction for VOC, BNA and PCDDs/PCDFs analyses. These compounds are used to

quantitate concentrations of compounds detected in the sample. VOC and BNA internal

standards have acceptable recovery control limits which are presented in the appropriate

method(s). Control limits for PCDD/PCDF internal standards are presented in Table

3, since surrogate compounds are not used for this analysis.

Cleanup standards are added to all samples and blanks analyzed for PCDDs/PCDFs and

are used to monitor the cleanup technique efficiency. Recovery control limits for these

standards are also provided in Table 3.

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93 QUALITY CONTROL OF BENTHIC LABORATORY ANALYSES

Two levels of quality control will be applied to benthic macroinvertebrate laboratoryanalyses. The first level is to provide a quality control check on organism recovery fromthe sample. The second level is to verify the accuracy of taxonomic identification work.

To ensure that all organisms are recovered from each sample, every tenth sorting traywill be resorted. If more than approximately 5 percent of the total number of organismsoriginally recovered from the tray are found while resorting, the previous nine trays willbe resorted also.

Preliminary sorting and identification of benthic samples will be conducted by a stafflevel benthic technician. All taxonomy for all samples will be verified by an experiencedsenior level taxonomist. Representative specimens of all taxa will be maintained in atype specimen collection for the study. Where identification cannot be verified,representative specimens will be sent to a recognized expert in the taxonomy of thespecific group in question.

All benthic analyses will be conducted in accordance with Macroinvertebrate Field andLaboratory Methods for Evaluating the Biological Integrity of Surface Waters (EPA,1990) as detailed in the FSP.

9.4 GEOTECHNICAL ANALYSES

Geotechnical analyses will be conducted in conformance with the quality control planand standard operating procedures which are included in Appendix F.

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10.0

PERFORMANCE AND SYSTEMS AUDITS

Performance and systems audits are conducted to verify documentation on implementa-

tion of the QA program, assess the effectiveness of the QAPjP, identify any nonconfor-

mances, and verify correction of identified deficiencies. The QA/QC Officer will be

responsible for initiating audits, selecting the audit team, and overseeing audit

implementation.

A minimum of one systems audit on fieldwork performance will be conducted by the

QA/QC Officer or his/her designee during the Site investigations. The Field Task

Leader is responsible for supervising and checking that samples are collected and

handled in accordance with the approved project plans and that documentation of work

is adequate and complete. A field audit checklist is included as Appendix K. One

systems audit on laboratory performance may also be conducted by the QA/QC Officer

or his/her designee during the course of the project.

The Project Manager is responsible for overseeing that the project performance satisfies

the QA objectives as set forth in this QAPjP. Reports and technical correspondence will

be peer reviewed by an assigned qualified individual, who is otherwise external to the

project, before being finalized.

10.1 PERFORMANCE AUDITS

The QA/QC Officer will evaluate the need for a performance audit with due consid-

eration given to the recommendations of the Project Manager. Performance audits are

utilized to quantitatively assess the accuracy of data through the use of performance

evaluation and blind check samples. The performance audit will be conducted by the

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QA/QC Officer or his/her designee in accordance with the procedures outlined inSection 10.3.

10.2 SYSTEMS AUDITS

A systems audit will be performed of field operations to review the total data generation

process, which includes on-site review of the field operational system, physical facilitiesfor sampling, and equipment calibrations. The field system audit will be performedduring the field program when analytical samples are being collected. The laboratory

will be audited for those CLP parameters for which it does not have a CLP contract.If a laboratory systems audit is necessary, it will be performed during the time period

when samples collected from the Site are being analyzed. An additional systems auditmay be requested by the QA/QC Officer, if warranted. System audits for both field andlaboratory will follow standard practices.

If a systems audit is necessaiy, WCC has a lab audit and check list progiam lliat isparallel in structure to the USEPA lab audit program that will be used for the audit.The lab audit program consists of the following:

• Inspection of the laboratory's sample receiving and storage facilities

• Inspection of the documentation procedures for sample receipt and routing

• Inspection of the laboratory's analytical facilities, to include checking and

verifying that all equipment, instruments, and devices are consistent withthe laboratory's inventory list.

• Inspection of the laboratory's reagent receiving and handling procedures

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Inspection and auditing of instrument calibration and maintenance logbooks.

etc.

This is usually a two-day procedure.

10.3 AUDIT PROCEDURE

This procedure provides requirements and guidance for performing internal and externalaudits to verify compliance with the elements of the QAPjP.

10J.I Audit Notification

The Project Manager, and, if appropriate, other audited authority (e.g., Field TaskLeader, Laboratoiy Supei visor) will be notified by the QA/QC Officer of an audit at areasonable time before the audit is performed. This notification will be in writing andwill include information such as the general scope and schedule of the audit and thename of the audit team leader.

10.3.2 Pre-Audit Conference

A pre-audit conference will be conducted at the audit site with the appropriate manageror designated representative (e.g., Field Task Leader, Laboratory Supervisor). Thepurpose of the conference will be to confirm the audit scope, present the audit plan,

discuss the audit sequence, and plan for the post-audit conference.

10.3.3 Audit

The audit will then be implemented by the audit team.

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• Checklists prepared by the audit team and approved by the QA/QCOfficer will be sufficiently detailed to document major audit components

• Selected elements of the QAPjP will be audited to the depth necessary toevaluate the effectiveness of implementation

• Conditions requiring immediate corrective action will be reportedimmediately to the QA/QC Officer

10J.4 Acceptance Criteria

Acceptance criteria for field activities will be defined as conformance with the field auditchecklist. Acceptance criteria for laboratory activities will be defined as conformancewith the lab audit checklist.

10.3.5 Post-Audit Conference

At the conclusion of the audit, a post-audit conference will be held with the Field TaskLeader or Laboratory Supervisor, or their designated representative, to present auditfindings and clarify any misunderstandings. Audit findings will be concisely stated by theaudit team leader on a list of findings. The findings will be acknowledged by signatureof the WCC Project Manager or designated representative upon completion of the post-

audit conferences.

10J.6 Audit Report

An audit report will be prepared by the audit team leader and signed by the QA/QC

Officer. The report will include the following:

• Description of the audit scope

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• Identification of the audit team

• Persons contacted during pre-audit, audit, and post-audit activities

• A summary of audit results, including an evaluation statement regarding

the effectiveness of the QAPjP elements which were audited

• Details of findings and program deficiencies

• Recommendations for correcting the findings to the QA/QC Officer, with

a copy to the Project Manager and others as appropriate

10.4 AUDIT RESPONSE

The WCC Project Manager or designated representative will respond to the audit report

within 5 business days of receipt. The response will clearly slaie the corrective aciion

for each finding, including action to prevent recurrence and the date the corrective

action will be completed.

10.5 FOLLOW-UP ACTION

Follow-up action shall be performed by the QA/QC Officer or designated representative

to:

• Evaluate the adequacy of the WCC Project Manager's response

• Assess corrective action is identified and scheduled for each finding

• Confirm corrective action is accomplished as scheduled

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or Follow-up action may be acuutiayifahcd through written communications,

other appropriate means. When all corrective actions have been verified, a memo willbe sent to the WCC Project Manager signifying the satisfactory close-out of the audit.

10.6 AUDIT RECORDS

Original records generated for all audits will be retained within the central project files.Records will include audit reports, written replies, the record of completion of correctiveactions, and documents associated with the conduct of audits which support audit

findings and corrective actions as appropriate.

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11.0

PREVENTIVE MAINTENANCE

To ensure analytical data generated for the former Koppers Company, Inc. Newport Site

investigations are reliable, all equipment and instruments will have a prescribed routine

maintenance schedule in addition to a calibration schedule. Preventive maintenance willbe performed and documented by qualified project personnel.

11.1 FIELD INSTRUMENTS

All field instrumentation, sampling equipment, and accessories will be maintained in

accordance with the manufacturer's recommendations and specifications and establishedfield practice. All maintenance will be performed by qualified project personnel and willbe documented by the appointed equipment manager or his designee under the uiieciionof the equipment manager.

The Field Task Leader and Site Health and Safety Officer will review calibration and

maintenance records on a regular basis to ensure that required maintenance is occurring.These activities will be recorded in the field logbook to document that established

calibration and maintenance procedures have been followed. Field instruments will be

checked and calibrated prior to their use on-site, and batteries will be charged andchecked daily where applicable.

Table 13 presents the field equipment maintenance schedule. Spare parts for field

equipment include extra batteries which will be kept with the sampling crew at all times.

Replacements for damaged instruments or other parts will require only 1 day (within 24

hours) for delivery from the vendor or WCC.

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11.2 LABORATORY INSTRUMENTS

The laboratory is responsible for the maintenance of its laboratory equipment. Pre-ventive maintenance will be provided on a scheduled basis to minimize down time andthe potential interruption of analytical work. All instruments will be maintained in

accordance with manufacturer's recommendations and normal approved laboratorypractice.

Designated laboratory personnel will be trained in routine maintenance procedures forall major instrumentation. When repairs become necessary, they will be performed byeither trained staff or trained service engineers/technicians employed by the instrumentmanufacturer. The laboratory shall have multiple instruments which will serve as backupto minimize the potential for down time. All maintenance will be documented and keptin permanent logs. These logs will be available for review by auditing personnel.

Both scheduled maintenance and unscheduled maintenance required by operationalfailures will be recorded. The designated laboratory operations coordinator will reviewmaintenance records on a regular basis to ensure that required maintenance is occurring.Details of these procedures are provided in the LQAPs provided in Appendices A, Band C.

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12.0

DATA MEASUREMENT ASSESSMENT PROCEDURES

The reliability and credibility of analytical laboratory results are established by theinclusion, as an integral part of any analytical procedure, of a program of randomlyselected replicate or duplicate analyses, analysis of standards or spiked samples, and theutilization of trip blanks, field blanks, and rinsate blanks.

Precision of analytical results may be established as the relative percent difference

(RPD) from true values or from the mean of replicate or duplicate analyses. Accuracyis reported as the percent recovery of a parameter from a sample of known value with

a given analytical procedure and analyst.

Tne procedures described herein are designed to procure precise and accurate data foreach analytical method and analyte. To ensure that reliable data continue to beproduced, systematic checks must show that test results remain reproducible and that themethodology is actually measuring the quantity of analyte in each sample. Quality

assurance must begin with sample collection and not end until the resulting data havebeen reported.

Data assessment and review will be accomplished by the efforts of the Project QA/QC

Officer and his or her designee. The analytical results will be reviewed for compliancewith the established QC criteria as described in Section 8.0. The data assessment by theQA/QC Officer will be based on the criteria that the samples were properly collectedand handled according to the procedures detailed in this QAPjP. Any problems arisingduring sample collection, packing, shipping, or analysis will be taken into consideration.

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The following procedures will be used to evaluate data precision and accuracy for theanalyses conducted.

12.1 ACCURACY

Accuracy will be expressed as percent recovery for laboratory control samples, surrogate

compounds, internal standards (PCDDs/PCDFs), cleanup standards (PCDDs/PCDFs),and recovery standards (PCDDs/PCDFs) as follows:

Percent Recovery = X , 100T

where X = the observed value of measurementT = "true" value

These recoveries will be compared with the laboratory's internal and method controllimits and the outliers will be assessed in conformance with other QC data. Surrogate

compound, internal standard (PCDDs/PCDFs), and cleanup standard (PCDDs/PCDFs)recoveries will also be calculated as above and compared against the limits shown in

Table 3. If the percent recovery limits are exceeded, the data will be assessed inconjunction with other QC data.

In addition, the matrix spike and matrix spike duplicate sample results will be used to

calculate the percent recovery.

Percent Recovery = X-S „ 100(for matrix spikes) T

observed value after spike

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where X = spike sample value

S = sample value

T = amount spiked

These matrix spike and matrix spike duplicate percent recoveries will be compared

against limits shown on Tables 4 and 5 and qualitative conclusions made on the nature

of sample matrix.

122 PRECISION

Precision will be expressed as relative percent difference (RPD) for duplicate

environmental samples as follows:

RPD(%) = |S-D| , 100(S + D)/2

where S = first sample value (original)

D = second sample value (duplicate)

The RPDs will be compared against the limits in Tables 4 and 5.

12.3 COMPLETENESS

Completeness is the measure of the amount of valid sample data obtained from the

measurement system compared to the amount of sample data that are analyzed. Valid

results are those results which meet or exceed quality control criteria and satisfy quality

assurance objectives.

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The equation for completeness will be expressed as follows:



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%C = 100% , VT

Where %C = percent completenessV = number of measurements judged valid

T = total number of measurements

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13.0

CORRECTIVE ACTION

The ultimate responsibility for maintaining quality throughout investigations at the Siterests with the Project Manager. The routine operation of the quality assurance fallsupon the Field Task Leaders, the Project QA/QC Officer, and the Laboratory ProgramAdministrator.

Any and all nonconformances with the established quality control procedures will be

expeditiously identified and controlled. No additional work which is dependent on thenonconforming activity will be performed until the identified nonconformance iscorrected.

I3.I FIELD CORRECTIVE ACTION

The Field Task Leaders will review the procedures being implemented in the field for

consistency with the established protocols. Sample collection, preservation, and labeling,etc., will be checked for completeness. Where procedures are not strictly in compliance

with the established protocol, the deviations will be field documented and reported tothe QA/QC Officer. Corrective actions will be defined by the Field Task Leaders,

Project QA/QC Officer, and Project Manager, and documented as appropriate. Upon

implementation of the corrective action, the Field Team Leader will provide the QA/QCOfficer with a written memo documenting field implementation. The memo will become

part of the Site central project file.

91C2628 1/QAPJP-KN.RPT/KPR4 13-1 _ _ _ 01-31-94



02-01-94Page 2 of 4

13.2 LABORATORY CORRECTIVE ACTION

The laboratory department supervisor will review the data generated to ensure that all

quality control samples have been run as specified in the protocol. Recoveries of matrix

spike samples for consistency with method accuracy and matrix spike duplicate samples

for method precision will be evaluated, using the criteria listed in Tables 4 and 5 and

presented in the applicable method. Laboratory control samples (LCS) data which fall

within the laboratory(s) control limits will be judged to be in control. LCS data which

do not fall within control limits will be considered suspect, and the analysis will be

required to be repeated if sufficient sample volume remains.

If holding times are exceeded or if it is anticipated that they will be exceeded, the

laboratory department supervisor will contact the WCC QA/QC officer as soon as

possible.

Laboratuiy peisomicl will be alerted that collective actions may be necessary if:

• QC data are outside the warning or acceptable windows for precision and

accuracy established for laboratory control samples

• Blanks contain contaminants at concentrations above the levels specified

in the analytical method for any target compound

• Undesirable trends are detected in matrix spike recoveries or relative

percent difference (RPD) between matrix spike duplicates or laboratory

duplicates

• There are unusual changes in detection limits (i.e., if detection limits are

substantially higher or lower than what is expected for given parameter

within a given matrix)

91C2628-1/QAPJP-KN.RPT/KPR4 13-2 • p O | I li fl |~| 01-31-94



02-01-94Page 3 of 4

• Deficiencies are detected by the laboratory QA director during internal or

external audits, or from the results of performance evaluation samples

If any nonconformances in analytical methodologies, quality control sample results, etc.,are identified by the bench analyst, corrective actions will be implemented immediately.Corrective action procedures will be handled initially at the bench level by the analyst,who will review the preparation or extraction procedure for possible errors, check the

instrument calibration, spike and calibration mixes, instrument sensitivity, etc. Theanalyst will immediately notify his/her supervisor as to the problem that is identified andthe investigation which is being conducted. If the problem persists or cannot beidentified, the matter will be referred to the laboratory supervisor and laboratory QADirector for further investigation, and the QA/QC Officer will be notified. Onceresolved, full documentation of the corrective action procedure will be filed by thelaboratory QA Director, and the QA/QC Officer will be provided a corrective action

memo for inclusion into the project file if data are affected.

Corrective action may include, but will not be limited to:

• Reanalyzing suspect samples• Resampling and analyzing new samples• Evaluating and amending sampling and/or analytical procedures• Accepting data with an acknowledged level of uncertainty

• Recalibrating analytical instruments

• Discarding the data

Following the implementation of the required corrective action measures by the

laboratory, WCC will perform QA validation or review and a final determination will be

made by the QA/QC Officer and the Project Manager as to the usability of the datawith respect to the goals of the data use categories. If any data are deemedunacceptable (unusable) by the Project Manager, additional follow-up corrective actions

91C2628 l/QAPJP-KN RPT/KPR4 13-3 • Pk O I I 11 0 I 01-31-94R R 3 I I U O



02-01-94Page 4 of 4

will be explored. Details of laboratory corrective actions are provided in the LQAPs inAppendices A, B and C.

13J CORRECTIVE ACTIONS FOLLOWING DATA ASSESSMENT

The project QA Officer will review the field and laboratory data generated for this

project to ensure that all project quality assurance objectives are met. If anynonconformances are found in the field procedures, sample collection procedures, fielddocumentation procedures, laboratory analytical and documentation procedures, anddata assessment and validation procedures, the impact of those nonconformances on the

overall project QA objectives will be assessed. Appropriate actions, includingresampling, reanalysis, etc., may be recommended so that the project objectives can beaccomplished.

If objectives set for the data quality indicators (Section 3.3) are not achieved, it may be

necessary to implement corrective actions as discussed above. However, failure to meetthe objectives of accuracy, precision, representativeness, and comparability, in and ofthemselves, may not be sufficient to require resampling or reanalysis; only as these data

quality indicators affect the objectives of completeness would there be a need forresampling and reanalysis. Failure to meet completeness objectives may result in thenecessity for resampling and reanalysis as determined by the Project Manager.

91C2628-1/QAPJP-KN.RFT/KPR4 13-4 01-31-94

A R 3 I U02



02-01-94Page 1 of 2

14.0

QUALITY ASSURANCE REPORTS TO MANAGEMENT

The Field Task Leaders will report to the Project Manager or his/her designee on adaily basis regarding progress and status of the fieldwork and quality control issues

associated with the field activities.

The laboratory will maintain detailed procedures for laboratory recordkeeping in order

to support the validity of all analytical work. Each data set report submitted to the

QA/QC Officer will contain the laboratory's written certification that the requestedanalytical method was run and that all QA/QC checks were within the establishedcontrol limits on all samples. The laboratory Program Administrator (PA) will providethe QA/QC Officer or his/her designee with QA reports of their external audits uponrequest (See Section 10.0).

The QA/QC Officer will submit a written summary to the Project Manager following

sampling and analysis which describes the completeness of the field activities being

conducted. After receipt of all the analytical data, a designee of the QA/QC Officer willsubmit a QA report to the QA/QC Officer and Project Manager describing the accuracyand precision of the data collected. Verbal reports will be provided following the receiptof individual data packages. The final report will be based on the data reports and other

information reported orally by the contract laboratory to the QA/QC Officer or his/herdesignee. If any QA problems are encountered, the laboratory PA or QA Director will

issue a written report to the QA/QC Officer, who will immediately report the

problem(s) to the Project Manager.

Data gathered during this program will be stored as stipulated in Section XIV of the

Administrative Order on Consent for this project.

9IC2628-1/QAPJP-KN.RPT/KPR4 14-1 0131-94

A R 3 I 11*03



02-01-94Page 2 of 2

Changes to this QAPjP are subject to EPA approval. Changes may be made by

submitting written revisions to the EPA for review and approval.

91C2628-1/QAPJP-KN.RPT/KPR4 14-2 01-3194

A R 3 1 I U O U



02-01-94Page 1 of 2

15.0

REFERENCES

Compendium of Superfund Field Operations Methods; EPA 540/P-87/001; OSWERDirective 9355.0-14; December 1987.

Data Quality Objectives for Remedial Response Activities; EPA/540/G-87/003;March 1987.

Guidance for Conducting Remedial Investigations and Feasibility Studies underCERCLA; Interim Final EPA/540/G-89/004; October 1988.

Interim Guidelines and Specifications for Preparing Quality Assurance Project Plans,QAMS-005/80. Office of Monitoring Systems and Quality Assurance. Office ofResearch and Development. USEPA 1980.

Laboratory Data Validation, Functional Guidelines for Evaluating Organics Analyses;EPA Data Review Work Group; February 1, 1988 with Region III modifications.

Laboratory Data Validation, Functional Guidelines for Evaluating Inorganics Analyses;EPA Data Review Work Group; June 13, 1988 with Region III modifications.

Macroinvertebrate Field and Laboratory Methods for Evaluating the Biological Integrityof Surface Waters; EPA/600/4-90/030; November 1990.

Methods for Chemical Analysis of Water and Wastes; EPA/600/4-79/020; 1983.

Preparation Aides for the Development of Category I Quality Assurance Project Plans.(EPA-600/8-91/003). February 1991.

Test Methods for Evaluating Solid Waste, Physical/Chemical Methods (SW-846);Update I (Draft), December 1987.

USEPA Contract Laboratory Program (CLP) Statement of Work (SOW) for OrganicsAnalysis - March 1990 (OLM01.0) with revisions up to August 1991 - OLM 0.1.8.

91C2628-1/QAPJP-KN.RPT/KPR4 15~1 . n r- 01-31-94



02-01-94Page 2 of 2

USEPA Contract Laboratory Program (CLP) Statement of Work (SOW) for InorganicsAnalysis - July 1988 (ILM02.0), with revisions up to September 1991.

USEPA Contract Laboratory Program (CLP) Statement of Work (SOW), forPolychlorinated Dibenzo-p-dioxins and Polychlorinated Dibenzofurans -September 1991 (DFLM01.1) with revisions.

Users' Guide to the Contract Laboratory Program; EPA OSWER Directive 9240.0-1;March 1990.

91C2628 1/QAPJP-KN.RPTYKPR4 15-2 01-31-94

A R 3 1 1 U 0 6

Tables

A R 3 1 I U 0 7

TABLE 1

QC LEVEL OF EFFORT FOR ANALYTICAL TESTINGREMEDIAL INVESTIGATION


Parameters QC Measure Frequency

Metals Calibration Blank (ICP andAA)

Initial CalibrationVerification (ICP and AA)

Continuing CalibrationVerification (ICP and AA)

Preparation Blank (ICP andAA)

Matrix Spike Analysis (ICPandAA)

Laboratory Control SampleAnalysis (ICP and AA)

Analytical Spike (AA-Furnace)

Interference Check Sample(ICP)

Laboratory Duplicate

Each calibration, beginning and end of eachrun, 10% frequency

Daily for each instrument setup

Beginning and end of each run; 10% frequencyor every 2 hrs.

One per analytical*0 batch

One per matrix-per site per analytical0' batch

One per analytical'0 batch

Each sample (at least a single analytical spikewill be performed to determine if the method of

standard addition is required for quantitation)

Beginning and end of each run or one per 4-hour shift

One per analytical*0 batch

Volatile OrganicCompounds andSemi-VolatileCompounds'2'

Laboratory Blank

Instrument Tune

Initial Calibration

Continuing Calibration

Laboratory Control Sample(Low Level CLP Only)

Second Column Confirmation

One per analytical'" batch

Each 12 hours of analysis

Subsequent to instrument tune and each timeinitial and/or continuing calibration failacceptable criteria

Each 12 hours

One per analytical'0 batch

/91C2628-3X2/QAPJP KN TBL

Gas chromatography methods, whereappropriate (e.g., pesticides)

A R 3 1 I U 0 8Page 1 of 2

TABLE 1(concluded)

Parameters QC Measure Frequency

Volatile OrganicCompounds andSemi-VolatileCompounds0'(concluded)

Matrix Spike Analysis One per matrix per site per analytical0' batch(Routine Level CLP Only)

Matrix Spike Duplicate One per matrix per site per analytical0' batchAnalysis (Routine Level CLPOnly)

Surrogate Spike Each sample, where appropriate (e.g., semi-volatiles)

PCDDs/PCDFs Laboratory Blank

Instrument Tune

Initial Calibration

Continuing Calibration

Window Defining Mix

Internal Cleanup Standards

Matrix Spike Analysis

Laboratory DuplicateAnalysis

One per analytical0' batch

Prior to calibration

Prior to sample analysis

Every 12 hours

Prior to initial calibration and any timeinstrument adjustments are made; or

When retention time failures occur duringcontinuing calibration

Each sample



Total SuspendedSolids andAlkalinity

Laboratory Blank

Laboratory Duplicate

Laboratory Control Sample




NOTES: An analytical batch for semi-volatiles and pesticide/PCB analyses consists of a group ofsamples extracted together.(1) An analytical batch consists of 20 samples or less, prepared or analyzed together with

a common QC sample. A case consists of one or more Sample Delivery Groups.(2) Includes pesticides and PCBs.

A R 3 I 11*09/91C2628-3X2/QAPJP KN.TBL 06-16-93/KPR1 Page 2 of 2

TABLE 2

SUMMARY OF QC SAMPLING AND ANALYSIS PLANREMEDIAL INVESTIGATION

FORMER KOPPERS COMPANY, INC. NEWPORT SITE, NEWPORT, DELAWARE

LaboratoryMatrix Parameters

Soil Borings TCL-VOCs+TICsTCL-BNAs+TICsTAL-MetalsTCL-Pesticides/PCBsPCDDs/PCDFs

Surface Soil TCL-VOCs+TICsTCL-BNAs + TICsTAL-MetalsTCL-Pesticides/PCBsPCDDs/PCDFs

Sediments TCL-VOCs+TICsTCL-BNAs + TICsTAL-MetalsTCL-Pesticides/PCBsPCDDs/PCDFs

Surface TCL-VOCs + TICsWater TCL-BNAs+TICs

Total Metalsi» Dissolved Metals=0 TCL-Pesticides/PCBs00 PCDDs/PCDFs_ TSS.p- Alkalinity

InvestigativeSamples

2072072074141

4444441010

1721721723535

6464646413136464

FieldDuplicates

11111133

33311

10101022

44441144

FieldBlanks

333-

—

——---~

444—

—333--

—--

Trip Rinsate"'Blanks Blanks

25 111111

"~ •?

3

33311

7 10101022

4 44441144

MS/MSDsand/or

MS/LabDuplicates0'

11/1111/1111/113/33/3

3/33/33/31/11/1

10/1010/1010/102/22/2

4/44/44/44/41/11/14/44/4

MatrixTotal

2792542545353

5656561414

2232162164343

8783838017178080

/91C2628-3X2/QAPJP-KN.TBL 05-07-93/KPR1 Page 1 of 2

TABLE 2(concluded)

Matrix

Groundwater(per round ofsamples -three roundstotal)

LaboratoryParameters

TCL-VOCs+TICsTCL-BNAs+TICsTotal MetalsDissolved MetalsTCL-Pesticides/PCBsPCDDs/PCDFs

InvestigativeSamples

3636363677

FieldDuplicates

222211

FieldBlanks

111

—--

—

TripBlanks

15

———~

—

Rinsate"'Blanks

222211

MS/MSDsand/or

MS/LabDuplicates0'

2/22/22/22/21/11/1

MatrixTotal

604545441111

NOTES: (1) Rinsate blanks for dissolved metals analyses will be filter blanks.(2) MS/MSDs for VOC, BNA, and Pesticide/PCB analyses, MS/laboratory duplicates for PCDDs/PCDFs and metals

(total and dissolved), and laboratory duplicates and laboratory control samples for TSS and alkalinity.TSS Total suspended solids.

CO


TABLE 3QUALITY CONTROL METHOD CRITERIA FOR ACCURACY

(SURROGATE SPIKE RECOVERIES)FOR ORGANIC PARAMETERS(WATER AND SOIL SAMPLES)


Accuracy as % Recovery

Water

Fraction

PurgeableVolatiles

Semi-volatiles

Pesticides/PCBs

PCDDs/PCDFs

Surrogate Compound

l,2-dichloroethane-d4

toluene-d,4-bromofluorobenzene

nitrobenzene-dj2-fluorobiphenylterphenyl-du

phenol-ds

2-fluorophenol2,4,6-tribromophenol2-chlorophenol-d4

l,2-dichlorobenzene-d4

tetrachloro-meta-xylene (TCX)decachlorobiphenyl (DCB)I3C12-2,3,7,8-TCDD(IS)13Cn-2,3,7,8-TCDF(IS)13C12-l,2,3,6,7,8-HxCDD(IS)13C12-1,2,3,4,6,7,8-HPCDF(IS)I3C12-OCDD(IS)37Cl4-2,3,7,8-TCDD(CS)

Low LevelCLP"'

NRNR80-120

40-11242-11024-14017-11316-10818-126NRNR

60-15060-150

RASCLpC)(3)

76-11488-11086-115

35-11443-11633-14110-11021-11010-123

33-110'16-110*

60-15060-150

25-15025-15025-15025-15025-15025-150

Soil/Sediment

RASCLp(2K3)

70-12184-13859-113

23-12030-11518-13724-11325-12119-122

20-130*20-130*

60-15060-150

25-15025-15025-15025-15025-15025-150

NOTES: RAS Routine Analytical Services(1) "USEPA Contract Laboratory Program (CLP) Statement of Work (SOW) for Low

Concentration for Organics Analysis". October 1992.(2) "USEPA Contract Laboratory Program (CLP) Statement of Work (SOW) for Organics

Analysis". Document No. OLM01.0 March 1990 with revisions up to OLM01.8(August 1991).

(3) "USEPA Contract Laboratory Program (CLP) Statement of Work (SOW) forPolychlorinated dibenzo-p-dioxins (PCDD) and Polychlorinated dibenzofurans(PCDF)". Document No. DFLMOl.l September 1991.

NR: Not Required*: Advisory Limits OnlyIS: Internal StandardCS: Cleanup Standard

/91C2628-3X2/QAPJP-KN.TBL 05-07-93/KPR1 A R 3 I U I 2

TABLE 4QUALITY CONTROL METHOD CRITERIA FOR ACCURACY

(MATRIX SPIKE RECOVERIES) AND PRECISION(RELATIVE PERCENT DIFFERENCE)

FOR ORGANIC PARAMETERS(WATER AND SOIL SAMPLES)


Fraction

Purgeablc Volatile

Semi-volatile(Base/Neutral/Acid)

Pesticides/PCBs

PCDDs/PCDFs

Spiking Compound

1,1-Dichloroe thaneTrichloroetheneBenzeneTolueneChlorobenzene

Phenol2-Chlorophenol1,4-DichlorobenzeneN-Nitroso-di-N-propylamine1,2,4- Trichlorobenzene4-Chloro-3-MethylphenolAcenaphthene4-Nitrophenol2,4-DinitrotoluenePentachlorophenolPyrene

gamma-BHCHeptachlorAldrinDieidrinEndrin4,4'-DDT

23,7,8-TCDF1,23,7,8-PeCDF1,2,3,6,7,8-HxCDF1,23,4,6,7,8-HpCDFOCDF23,7,8-TCDD1,23,7,8-PeCDD1,2,3,6,7,8-HxCDD1,23,4,6,7,8-HpCDDOCDD

Accuracy as

Water

RAS CLP

61-145(14)71-120(14)76-127(11)76-125(13)75-130(13)

12-110(42)27-123(40)36-97(28)41-116(38)39-98(28)23-97(42)46-118(31)10-80(50)24-%(38)9-103(50)26-127(31)

56-123(15)40-131(20)40-120(22)52-126(18)56-121(21)38-127(27)

50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)

% Recovery110'

Soil/Sediment

RAS CLP

59-172(22)62-137(24)66-142(21)59-139(21)60-133(21)

26-90(35)25-102(50)28-104(27)41-126(38)38-107(23)26-103(33)31-D7(19)11-114(50)28-89(47)17-109(47)35-142(36)

46-127(50)35-130(31)34-132(43)31-134(38)42-139(45)23-134(50)

50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)50-150(50)

sources:

RAS Routine Analytical Service(1) Relative Percent Difference (RPD) control limits noted in parentheses.(2) Accuracy and precision criteria not provided for low level CLP organics, since MS/MSD analyses not

required.

USEPA CLP March 1990 (OLM01.0) with revisions up to August 1991 (OLM01.8) for TCL Organics.USEPA CLP October 1990 (DFLM01.0) with revisions up to September 1991 (DFLM01.1) for PCDDs/PCDFs.

/91C2628-3X2/QAPJP-KN.TBL 05-07-93/KPR1 A R 3 I U I 3

TABLES

QUALITY CONTROL METHOD CRITERIA FOR ACCURACY(MATRIX SPIKE RECOVERIES) AND PRECISION

(RELATIVE PERCENT DIFFERENCE) FOR METALS AND INORGANICS(WATER AND SOIL SAMPLES)


Parameter

Metals-ICP

Thallium-GFAA

Arsenic-GFAA

Lead-GFAA

Selenium-GFAA

Mercury-CVAA

TSSAlkalinity

Method"'0'

EPA CLPEPA CLP

EPA CLPEPA CLP

EPA CLPEPA CLP

EPA CLPEPA CLP

EPA CLPEPA CLP

EPA CLPEPA CLP

160.2310.1

Matrix

WaterSoil

WaterSoil

WaterSoil

WaterSoil

WaterSoil

WaterSoil

WaterWater

Accuracy(% Recovery)

75-12575-125

75-12575-125

75-12575-125

75-12575-125

75-12575-125

75-12575-125

85-11585-115

Precision0"4'(RPD) %

2020

2020

2020

2020

2020

2020

2020

NOTES: (1) EPA CLP ILM02.0 revised September 1991 (ILM02.1).(2) 160.2/310.1 - USEPA 600/4-79-020 (1983).(3) Applicable only if both original and duplicate results are greater than

5 times the Contract Required Detection Limit (CRDL). If onfy oneresult is > 5 times CRDL, then ±CRDL will be used for control limits.If both results are < 5 times CRDL, control limits do not apply.

(4) Control limits for TSS and alkalinity provided by contract laboratory.Accuracy for these parameters will be based on results of laboratorycontrol samples.

RPD = Relative percent differenceICP = Inductively coupled plasma spectrometryGFAA = Graphite furnace atomic absorptionCVAA = Cold vapor atomic absorption

/91C2628-3X2/QAPJP KN.TBL 05-07-93/KPR1 A R 3 I m i t t P a g e l o f l

TABLE 6

QUANTITATION LIMITS FOR VOLATILE ORGANICS BY GC/MS(1)


VOCs

Chloromethane

Bromomethane

Vinyl chloride

Chloroethane

Methylene chloride

Acetone

Carbon disulfide

1,1-Dichloroethene

1,1 -Dichloroethane

1,2-Dichloroethene (total)

Chloroform

1,2-Dichloroethane

2-Butanone

1,1,1 -Trichloroethane

Carbon tetrachloride

Bromodichloromethane

1,2-Dichloropropane

cis- 1 ,3-Dichloropropene

Trichloroethene

Dibromochloromethane

Low Water*7'Mg/1

1

1

1

1

2

5

1

1

1

1

1

1

5

1

1

1

1

1

1

1

Routine Water0'Mg/1

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

RoutineSoil/Sediment^

Mg/Kg

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

/91C2628-3X2/QAPJP-KN.TBL 05-07-93/KPRI A R 3 I Page 1 of 2

VOCs

1, 1,2-Trichlore thane

Benzene

trans- 1,3-Dichloropropene

Bromoform

4-Methyl-2-pentanone

2-Hexanone

Tetrachloroethene

Toluene

1 , 1 ,2,2-Tetrachloroethane

Chlorobenzene

Ethyl benzene

Styrene

Xylenes (total)

Bromochloromethane

trans- 1,2-dichlorethene

cis- 1 ,2-dichloroethene

1,2-dibromoe thane

1,2-dichlorobenzene

13-dichlorobenzene

1,4-dichlorobenzene

TABLE 6(concluded)

Low Water®

Mg/1

1

1

1

1

5

5

1

1

1

1

1

1

1

1

1

1

1

1

1

1

Routine Water0'

Mg/i

10

10

10

10

10

10

10

10

10

10

10

10

10

——

~

—

—

—

—

NOTES: (1) Specific quantitation limits are highly matrixquantitation limits listed hereinalways belaboratory

(2) Low level

achievable. Thewill be based on wetCLP detection limits.

RoutineSoil/Sediment0'

Mg/Kg

10

10

10

10

10

10

10

10

10

10

10

10

10

—

—

——

——

—

dependent. Theare provided for guidance and may notquantitation limitsweight and as such

provided by thewill be higher.

(3) Routine CLP detection limits.

A R 3 I m i6/91C2628-3X2/QAPJP-KNTBL 05-O7-93/KPR1 PaBC 2 Of 2

TABLE?

QUANTITATION LIMITS FOR SEMI-VOLATILE ORGANICSBY GC/MS(1)


CompoundsSemi-volatiles (BNAs)

Phenol

bis(2-Chloroethyl)ether

2-Chlorophenol

1,3-Dichlorobenzene

1,4-Dichlorobenzene

1,2-Dichlorobenzene

2-Methylphenol

2,2 '-oxy bis (1-chloropropane)

4-Methylphenol

N-Nitroso-di-n-diproplamine

Hexachloroethane

Nitrobenzene

Isophorone

2-Nitrophenol

2,4-Dimethylphenol

bis(2-Chloroethoxy)methane

2,4-Dichlorophenol

1 ,2,4-Trichlorobenzene

Napthalene

4-Chloroaniline

Hexachlorobutadiene

4-Chloro-3-methylphenol

LowWater®

Mg/1

5

5

5

~

—

—5

5

5

5

5

5

5

5

5

5

5

5

5

5

5

5

Routine Water0'Mg/I

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

A R 3 I m i


/^g/Kg

330

330

330

330

330

330

330

330

330

330

330

330

330

330

330

330

330

330

330

330

330

330

7/91C2628-3X2/QAPJP-KN TBL 05-07-93flCPR 1 Paee 1 of 3

TABLE?(continued)


2-Methylnaphthalene

Hexachlorocyclopentadiene

2,4,6-Trichlorophenol

2,4,5-Trichlorophenol

2-Chloronaphthalene

2-Nitroaniline

Dimethylphthalate

Acenaphthylene

2,6-Dinitrotoluene

3-Nitroaniline

Acenaphthene

2,4-Dinitrophenol

4-Nitrophenol

Dibenzofuran

2,4-Dinitrotoluene

Diethylphthalate

4-Chlorophenylphenyl ether

. Fluorene

4-Nitroaniline

4,6-Dinitro-2-methylphenol

N-nitrosodiphenylamine

4-Bromophenylphenyl ether

Hexachlorobenzene

Pentachlorophenol

LowWater®

Mg/1

5

5

5

20

5

20

5

5

5

20

5

20

20

5

5

5

5

5

20

20

5

5

5

20

Routine Water0'Mg/1

10

10

10

25

10

25

10

10

10

25

10

25

25

10

10

10

10

10

25

25

10

10

10

25

A R 3 I l U I


Mg/Kg

330

300

330

800

330

800

330

330

330

800

300

800

800

330

330

330

330

330

800

800

330

330

330

800

1 8/91C2628-3X2/QAPJP-KN.TBL 05-07-93/KPR1 Paee 2 of 3

TABLE?(concluded)


Phenanthrene

- Anthracene

Carbazole

Di-n-butylphthalate

- Fluoranthene

Pyrene

Butylbenzylphthalate

3,3'-Dichlorobenzidine

- Benzo(a)anthracene

- Chrysene

bis(2-Ethylhexyl)phthalate

Di-n-octylphthalate

- Benzo(b)fluoranthene

_ Benzo(k)fluoranthene

- Benzo(a)pyrene

- Indeno(l,2,3-cd)pyrene

- Dibenz(a,h)anthracene

- Benzo(g,h,i)perylene

LowWater®«/l

5

5

—

5

5

5

5

5

5

5

5

5

5

5

5

5

5

5

Routine Water0'Mg/1

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10


Mg/Kg

300

300

330

330

330

330

330

330

330

330

330

330

330

330

330

330

330

330

NOTES: (1) Specific quantitation limits are highly matrix dependent. Thequantitation limits listed herein are provided for guidance and may notalways be achievable. The quantitation limits provided by the laboratorywill be based on wet weight and as such will be higher.

(2) Low level CLP detection limits.(3) Routine CLP detection limits.

A R 3 I H t l9/91C2628-3X2/QAPJP-KN TBL 05-07-93/KPR1 Page 3 of 3

TABLES

QUANTITATION LIMITS FOR ORGANOCHLORINEPESTICIDES AND PCBS(1)

FORMER KOPPERS COMPANY, INC NEWPORT SITENEWPORT, DELAWARE

Compounds

alpha-BHC

beta-BHC

delta-BHC

gamma-BHC (Lindane)

Heptachlor

Aldrin

Heptachlor epoxide

Endosulfan I

Dieldrin

4,4-DDE

Endrin

Endosulfan II

4,4-DDD

Endosulfan sulfate

4,4-DDT

Methoxychlor

Endrin ketone

gamma-Chlordane

Toxaphene

alpha-Chlordane

Endrin aldehyde

Low Waterro

Mg/l

0.01

0.01

0.01

0.01

0.01

0.01

0.01

0.01

0.02

0.02

0.02

0.02

0.02

0.02

0.02

0.10

0.02

0.01

1.0

0.01

0.02

Routine Water0'Mg/1

0.05

0.05

0.05

0.05

0.05

0.05

0.05

0.05

0.10

0.10

0.10

0.10

0.10

0.10

0.10

0.5

0.10

0.05

5.0

0.05

0.10


Mg/Kg

1.7

1.7

1.7

1.7

1.7

1.7

1.7

1.7

3.3

3.3

3.3

3.3

3.3

3.3

3.3

17.0

3.3

1.7

170.0

1.7

3.3

/91C2628-3X2/QAPJP KN.TBL 05XJ7-93/KPR1

A R 3PagC 1 of 2

TABLES(concluded)

Compounds

RoutineLow Water® Routine Water0' Soil/Sediment0'

Aroclor-1016

Aroclor-1221

Aroclor-1232

Aroclor-1242

Aroclor-1248

Aroclor-1254

Aroclor-1260

0.20

0.40

0.20

0.20

0.20

0.20

0.20

1.0

2.0

1.0

1.0

1.0

1.0

1.0

33.0

67.0

33.0

33.0

33.0

33.0

33.0

NOTES: (1) Specific quantitation limits are highly matrix dependent. Thequantitation limits listed herein are provided for guidance and may notalways be achievable. The quantitation limits provided by thelaboratory will be based on wet weight and as such will be higher.

(2) Low Level CLP detection limits.(3) Routine CLP detection limits.

BHC benzene hexachlorideDDT l,l,l-Trichloro-2,2-bis(p-chlorophenyl)ethane

(Dichlorodiphenyltrichloroethane)DDD DichlorodiphenyldichloroethaneDDE DichlorodiphenyldichloroethylenePCBs Polychlorinated biphenyls (Aroclors)

A R 3/91C2628-3X2/QAPJP-KN.TBL 05-07-93/KPR1 Page 2 of 2

TABLE 9QUANTITATION LIMITS FOR INORGANIC PARAMETERS0'


Analyte

METALS

Aluminum, Al

Antimony, Sb

Arsenic, As

Barium, Ba

Beryllium, Be

Cadmium, Cd

Calcium, Ca

Chromium, Cr

Cobalt, Co

Copper, Cu

Iron, Fe

Lead, Pb

Magnesium, Mg

Manganese, Mn

Mercury, Hg

Nickel, Ni

Potassium, K

Selenium, Se

Silver, Ag

Sodium, Na

Thallium, Tl

Vanadium, V

Zinc, Zn

WATER QUALITY

TSS

Alkalinity

NOTE: (1) The detection limits are based onAlkalinity which were supplied by

NR: Not Required.

Water (Mg/l)

200

60

10

200

5

5

5000

10

50

25

100

3

5000

15

0.2

40

5000

5

10

5000

10

50

20

5mg/l

20 mg/1

Soil/Sediment (mg/kg)

40

12

2

40

1

1

1000

2

10

5

20

0.6

1000

3

0.04

8

1000

1

2

1000

2

10

4

NR

NR

the CLP Statement of Work with the exception of TSS andthe contract laboratory.

A R 3 I 11*22/91C2628-3X2/QAPJP KN TBL 05-07-93rtCPRl PagC 1 Of 1

TABLE 10

QUANTITATION LIMITS FOR PCDDs/PCDFsFORMER KOPPERS COMPANY, INC. NEWPORT SITE

NEWPORT, DELAWARE

Compound

FURANS

2,3,7,8-TCDF

1,2,3,7,8-PeCDF

2,3,4,7,8-PeCDF

1,2,3,4,7,8-HxCDF

1,2,3,6,7,8-HxCDF

2,3,4,6,7,8-HxCDF

1,2,3,7,8,9-HxCDF

1,2,3,4,6,7,8-HpCDF

1,2,3,4,7,8,9-HpCDF

OCDF

DIOXINS

2,3,7,8-TCDD

1,2,3,7,8-PeCDD

1,2,3,4,7,8-HxCDD

1,2,3,6,7,8-HxCDD

1,2,3,7,8,9-HxCDD

1,2,3,4,6,7,8-HpCDD

OCDD

Water (ng/1)

10

25

25

25

25

25

25

25

25

50

10

25

25

25

25

25

50

Soil/Sediment0' (jig/kg)

1.0

2.5

2.5

2.5

2.5

2.5

2.5

2.5

2.5

5.0

1.0

2.5

2.5

2.5

2.5

2.5

5.0

NOTE: (1) Specific quantitation limits are highly matrix dependent. Thequantitation limits listed herein are provided for guidance and maynot always be achievable. The quantitation limits provided by thelaboratory will be based on wet weight and as such will be higher.

/91C2628-3X2AJAPJP-KN TBL 05-07-93/KPR1 A R 3 I I U 2 3 P ag e l o f l

TABLE 11

SAMPLE CONTAINERS, PRESERVATION, AND HOLDING TIME REQUIREMENTSFORMER KOPPERS COMPANY, INC. NEWPORT SITE

NEWPORT, DELAWARE

Matrix Parameter

WATER Volatile Organics

Semi-VolatileOrganics/Pesticides/PCBs

Metals (Dissolved)®

Metals (Total)

Total Suspended Solids

Alkalinity

PCDDs/PCDFs(Liquid for rinsate blank)

SOIL Volatile Organics

Metals

Semi-volatileOrganics/Pesticides/PCBs

PCDDs/PCDFs

Geotechnical Variables

Permeability

Container

3x 40 ml glass vialsTeflon™ septum

4x 1-liter amberglass bottle

Ix 1-liter plastic

Ix 1 -liter plastic

Ix 500 ml plasticor glass bottle

Ix 500 ml plasticor glass bottle

Ix 1-liter (or quart)amber glass bottle

2x40 ml glass vialsTeflon septa

Lx 8 oz widemouth glass jar

Ix 8 oz widemouth glass jar

Ix 4 oz widemouth glass jar

Ix 32 oz (can bejar or plastic bag)

1 x shelby tube

Preservation

Cool to 4°CHC1 to pH <2No headspace

Cool to 4°C

HN03 to pH <2Cool to 4°C

HN03 to pH <2Cool to 4°C

Cool to 4°C

Cool to 4°C

Cool to 4°C

Cool to 4°C

Cool to 4°C

Cool to 4°C

Cool to 4°C

Cool to 4°C

None

Holding Time

14 days

Extract - 7 daysAnalysis - 40 days

180 days28 days Hg

180 days28 days Hg

7 days

14 days

'Extract/Analysis - 45 days

14 days

180 days28 days Hg


'Extract/Analysis - 45 days

Not applicable

Not applicable

91C2628-1/TABLE11.QAP01-31-94/KPR4

A R 3 I | I * 2 UPage 1 of 2

TABLE 11(Continued)

Matrix Parameter Container Preservation Holding Time

SEDIMENT Volatile Organics

Metals

Semi-volatileOrganics/Pesticides/PCBs

PCDDs/PCDFs

Geochemical/GeophysicalVariables

2x40 ml glass vialsTeflon septa

1 x 8 oz widemouth glass jar




Cool to 4°C

Cool to 4°C

Cool to 4°C

Cool to 4°C

Cool to 4°C

NOTES: (1) Holding time from time/date of sample collection to sample extraction/analysis.(2) Filter before adding preservative (acid).* Analysis and extraction holding times are not specified in CLP method (see Table

laboratory uses 45 days for all extractions and re-analyses to be performed.

14 days

180 days28 days Hg


•Extract/Analysis - 45 days

Not applicable

15). The contracted

91C2628-1/TABLE11 .QAP01-31-94/KPR4 A R 3 M U 2 5 Page2of2

TABLE 12

SUMMARY OF ANALYTICAL METHODSREMEDIAL INVESTIGATION

FORMER KOPPERS COMPANY, INC. NEWPORT SITE, NEWPORT, DELAWARE

MethodMatrix Parameter Analytical Methoda) Reference

Soil/Sediment/SurfaceWater and Groundwater

Residential Well(Low Level CLP)

Total Suspended SolidsAlkalinity

TCL-VOCsTCL-BNAsTCL-Pesticides/PCBsTAL Metals(I)

PCDDs/PCDFs

TCL-VOCsTCL-BNAsTCL-Pesticides/PCBs

USEPA CLP OLM01.8, Aug 91USEPA CLP OLM01.8, Aug 91USEPA CLP OLM01.8, Aug 91USEPA CLP ILM02.1, Sept 91USEPA CLP DLFM01.1, Sept 91

USEPA CLP 10/92USEPA CLP 10/92USEPA CLP 10/92

160.2310.1

11123

444

55

NOTES: (1) Total and dissolved for surface water, groundwater, and residential water.(2) Residential and groundwater methods for first rounds, methods for these parameters

may be revised in subsequent rounds.TCL-VOCs = Target Compound List Volatile Organic CompoundsTCL-BNAs = Target Compound List Base/Neutral Acid extractablesTAL = Target Analyte List

Method References:

1. "USEPA Contract Laboratory Program (CLP) Statement of Work (SOW) for Organics Analysis" -Document No. OLM01.0 March 1990 with revisions up to OLM01.8 August 1991.

2. "USEPA Contract Laboratory Program (CLP) Statement of Work (SOW) for Inorganics Analysis" -Document No. ILM02.0 with revisions up to ILM02.1 September 1991.

3. "USEPA Contract Laboratory Program (CLP) Statement of Work (SOW) for Polychlorinateddibenzo-p-dioxins (PCDD) and Polychlorinated Dibenzofurans (PCDF)" - Document No. DFLM01.1September 1991.

4. "USEPA Contract Laboratory Program (CLP) Statement of Work (SOW) for Low ConcentrationWater for Organic Analysis." October 1992.

5. "Methods for Chemical Analysis of Water and Wastes, EPA 600/4-79-020." 1979 (revised 1983).

A R 3 I I U 2 6/91C2628-3X2/QAPJP-KN TBL 06-16-93/KPR1 Page 1 of 1

TABLE 12a

SUMMARY OF GEOTECHNICAL SAMPLES AND METHODSFORMER KOPPERS COMPANY, INC., NEWPORT SITE

NEWPORT, DELAWARE

Analysis

Moisture Content

Total OrganicCarbon

Percent OrganicMatter

Percent Sand, Silt&Clay

Specific Gravity

Permeability

Atterberg Limits

Redox Potential(Eh)

pH

Method

ASTM D2216

EPA 9060A

ASTM D2974

ASTM D422

ASTM D854

ASTM D5084

ASTM D4318

BMI 1599-001

ASTM D4972

Soils Samples

18

10

10

18

6

2

8

0

0

Sediment Samples

172

172

0

172

172

0

0

172

172

MethodReference

(D

(2)

(1)

(1)

(1)

(1)

(1)

(3)

(1)

Method References;

(1) 1990 Annual Book of ASTM Standards, Section 4 Construction; Volume 04.08 and Rock;Dimension Stone; Geosynthetics

(2) EPA-600/2-78-054, Field and Laboratory Methods Applicable to Overburdens and Mine Soils

(3) BMI Standard Operating Procedure 1599-001, Tentative Test Method for Determining Soil RedoxPotential;" Available from BMI upon request.

91C2628-3X2/TABLE12A.q«p/KPR2 6-23-93 • p O I 1 I. O 7 PagC 1 Of 1

TABLE 13

FIELD EQUIPMENTCALIBRATION AND MAINTENANCE REQUIREMENTS

FORMER KOPPERS COMPANY, INC. NEWPORT SITE/NEWPORT, DELAWARE

Equipment Task Frequency0' Maintenance

OVA

HNu 1.

2.

pH/Eh Meter 1.

Make sure hydrogen tank is full and allow 15 minutes forwarmup, ignite detector.

Perform calibration check by introducing a known methanestandard and adjusting instrument to correspond to calibrationstandard.

Perform internal calibration.

Introduce a known isobutylene standard and adjust instrumentto correspond to calibration standard.

Zero instrument

Immerse electrodes in buffer solution at pH 7 and adjust meterto proper reading. Rinse electrodes and immerse in buffersolution at pH 4 and pH 10 and adjust meter to proper reading.

Repeat above procedures until readings are within 0.1 pHunits of the buffer solution values. All buffer solutions and rinsesshould be at the same temperature.

Before each day's use Charge battery daily

Charge battery daily

Before each day's use

Weekly


Periodically during theday

Before each day's use Check batteries daily


CO

roCO

Note:(l)Site-Specific conditions may warrant a higher frequency.


Appendix G

A R 3 I 11 *29

IIIIIIIIIIIIIIIIIII

6.4.4 The analysis of the instrument performance check solution auscmeet the ion abundance criteria given below.

TABLE 1BFB KEY IONS AND ION ABUNDANCE CRITERIA

Mass Ion Abundance Criteria

50759596173174175176177

8.0 - 40.0 percent of mass 9530.0 - 66.0 percent of mass 95base peak. 100 percent relative abundance5.0 - 9.0 percent of mass 95 (see note)less than 2.0 percent of mass 17450.0 - 120.0 percent of mass 954.0 - 9.0 percent of mass 17493.0 - 101.0 percent of mass 1745.0 - 9.0 percent of mass 176

Note: All ion abundances must be normalized to m/z 95. thenominal base peak, even though the ion abundance of m/z 174be up to 120 percent that of m/z 95.

6.4.5 The criteria listed above are based on adherence to theacquisition specifications identified in paragraph 6.4.3. andwere developed for the specific target compound list associatedwith this Statement of Vork. The criteria are based onperformance characteristics of instruments currently utilizedin routine support of Program activities. Thesespecifications, in conjunction vith relative response factorcriteria for 23 target compounds (see Table 2), are designed tocontrol and monitor instrument performance associated with therequirements of this Statement of Uork.

6.4.6 The instrument performance check solution must be injected onceat the beginning of each 12-hour period, during which samplesor standards are to be analyzed. The twelve (12) hour timeperiod for CC/MS Instrument Performance Check (BFB), standardscalibration (initial or continuing calibration criteria) and*method blank analysis begins at the moment of injection of theBFB analysis that the laboratory submits as documentation of acompliant instrument performance check. The time period endsafter twelve (12) hours has elapsed according to the systemclock.

7. Calibration

7.1 Prior to the analysis of samples and required blanks, and after theinstrument performance check solution criteria have been met, eachCC/MS system must be calibrated at a minimum of five concentrations todetermine instrument sensitivity and the linearity of CC/MS responsefor the purgeable target compounds.

D-26/VOA OLM01.0

A R 3 I m30

7.2 Assemble a purge and trap device that meets the specification in 3.6.Condition the trap overnight at 180*C in the purge mode with an inertgas flow of at least 20 mL/min. Daily, prior to use. condition thetraps for 10 minuses while backflushing at IBO'C with the column at22D*C.

7.3 Connect the purge and trap device to a gas chromatograph. The gaschromatograph must be operated using temperature and flow rateparameters equivalent to those in 6.2. Calibrate the purge andtrap-CC/MS system using the internal standard technique (7.4).

7.4 Internal standard calibration procedure. The three internal standardsare Bromochloromethane. 1,4-Dlfluorobenzene, and Chlorobenzene-d5, at50 ug/L at time of purge. Separate Initial and continuing calibrationsmust be performed for water samples, and low level soil samples(unheated purge vs. heated purge). Extracts of medium level aoilsamples may be analyzed using the calibrations for water samples.

7.4.1 Prepare calibration standards at a minimum of fiveconcentration levels for each target compound and systemmonitoring compound, as specified in 5.5. Standards may bestored up to 24 hours, following the procedures in paragraph5.6.3.

7.4.2 Prepare a spiking solution containing each of the internalstandards using the procedures described in paragraph 5.4.3.

7.4.3 Verify that the CC/MS system meets the Instrument performancecriteria in paragraph 6.4 by injecting BFB. Analyze eachcalibration standard, according to paragraph 7.1, adding 10 uLof internal standard spiking solution directly to the syringe.

Tabulate the area response of the characteristic ions in theextracted ion current profile (EICP) against concentration foreach compound and internal standard and calculate relativeresponse factors (RRF) for each compound as follows:

RRF - — x —-Ais Cx

Where,

Ax - Area of the characteristic ion (EICP) for the compoundto be measured (see Table 4)

Ais - Area of the characteristic ion (EICP) for thespecific internal standard (see Table 3)

cis ~ Conc ntration of the internal standard

Cx - Concentration of the compound to be measured

D-27/VOA OLM01.0

A R 3 I m3l

IIIIIIIIIIIIIIII

Calculating the relative response factor of the Xylenes and thecis and trans isomers of 1,2-Dichloroethene requires specialattention. On packed columns, o-and p-Xylene Isomers coelute.On capillary columns, the m- and p-Zylene isomers coelute.Therefore, when calculating the relative response factor in theequation above, use the area response (A,) and concentration(C,) of the peak that represents the single isomer on the CCcolumn used for analysis.

For the cis and trans isomers of 1,2-Dichloroethene which maycoelute on packed columns but not on capillary columns, bothisomers must be present in the standards. If the two isomerscoelute, use the area of the coeluting peak and the totalconcentration of the two Isomers in the standard to determinethe relative response factor. If the two isomers do notcoelute, sum the areas of the two peaks and the concentrationsof the two isomers in the standard to determine the relativeresponse factor.

7.4.4 The average relative response factor (RRF) must be calculatedfor all compounds. Calculate the % Relative Standard Deviation(IRSD) of RRF values over the working range of the curve.

%RSD • Standard deviation x 100mean

Where.

Standard Deviation -

n

1-1n-1

1/2

Where.

Xi - each individual value used to calculate the mean

x - the mean of n values

n - the total number of values

7.4.5 The response factors of the compounds listed below (Table 2)must meet the minimum RRF criteria at each concentration leveland maximum %RSD criteria for the initial calibration, withallowance made for up to two volatile compounds. However, theRRFs for those two compounds must be greater than or equal to0.010, and the %RSD of those two compounds must be less than orequal to 40.0% for the initial calibration to be acceptable.

I D-28/VOA OLM01.2 1/91

AR3!

TABLE 2RELATIVE RESPONSE FACTOR CRITERIA FOR INITIAL AND CONTINUING

CALIBRATION OF VOLATILE ORGANIC COMPOUNDS

VolatileCompound

Bromome thaneVinyl chloride1 , 1- Dichloroe thene1 , 1 -Dichloroe thaneChloroform1.2 -Dichloroe thane1.1, 1 -Trichloroe thaneCarbon tetrachlorldeBromodichlorome thanecis - 1 .3-DichloropropeneTrichloroe theneDibromochlorome thane1.1. 2 -Trichloroe thaneBenzenetrans - 1 . 3-DichloropropeneBromoformTe crachloroe thene1.1,2, 2 -Tetrachloroe thaneTolueneChlorobenzeneEthylbenzeneStyreneXylenes (total)Bromofluorobenzene

MinimumRRF

0.1000.1000.1000.2000.2000.1000.1000.1000.2000.2000.3000.1000.1000.5000.1000.1000.2000.5000.4000.5000.1000.3000.3000.200

K ri w%RSD

20.520.520.520.520.520.520.520.520.520.520.520.520.520.520.520.520.520.520.520.520.520.520.520.5

tDiff

25.025.025.025.025.025.025.025.025.025.025.025.025.025.025.025.025.025.025.025.025.025.025.025.0

7.4.6 The following compounds have no Maximum %RSD, or Maximum%Dlfference criteria; however, these compounds HUAt meet aminimum RRF criterion of 0.010:

Acetone 1.2-Dichloropropane2-Butanone 2-HexanoneCarbon disulfide Methylene chlorideChloroethane 4-Methyl-2-pentanoneCbloromethane Toluene-dg1,2-Dichloroethene (total) 1,2-Dichloroethan*-d^

7.4.7 A check of the calibration curve must be performed once every12 hours (see paragraph 6.4.6 for the definition of the twelvehour time period). Check the relative response factors ofthose compounds for which RRF values have been established. Ifthese criteria are met. the relative response factors for allcompounds are calculated and reported. A percent difference ofthe daily relative response factor (12 hour) compared to theaverage relative response factor from the initial curve is

D-29/VOA OLM01.2 1/91

A R 3 I IU33

IIIIIIIIIIIIIIIIIII

SECTION IV

calculated. Calculate the percent difference for each compoundand coapare with the maximum percent difference criteria listedabove. For negative percent difference values, the value mustbe greater than or equal to -25.0%. but less than 0%. As withthe initial calibration, up to two volatile compounds in Table2 may fail to meet the minimum RRF or maximum %D criteria, butthe RRFs of those two compounds must be greater than or equalto 0.010. and the percent differences must be less than orequal to 40.0% for the continuing calibration to be acceptable.

7.4.8 Internal standard responses and retention times in allstandards must be evaluated during or immediately after dataacquisition. If the retention time for any internal standardchanges by more than 0.50 minutes (30 seconds) from the latestdaily (12 hour) calibration standard, the chromatographicsystem must be inspected for malfunctions, and corrections madeas required. The extracted ion current profile (EICP) of theinternal standards must be monitored and evaluated for eachstandard. If the EICP area for any internal standard changesby more than a factor of two (-50% to +100%), the massspectrometric system-must be inspected for malfunction, andcorrections made as appropriate. When corrections are made,re-analysis of samples analyzed while the system wasmalfunctioning is required.

7.5 Each CC/MS system must be calibrated upon award of the contract,whenever the Contractor takes corrective action which may change oraffect the initial calibration criteria (i.e., ion source cleaning orrepair, column removal or replacement, etc.), or if the continuingcalibration acceptance criteria have not been met.

7.6 If time remains in the 12 hour time period after meeting the acceptancecriteria for the initial calibration, samples may be analyzed. It isnot necessary to analyze a continuing calibration standard, if theinitial calibration meets the calibration acceptance criteria above. Amethod blank la, necessary. Quantify all sample results against theinitial calibration standard that is the same concentration as thecontinuing calibration standard (SO ug/L).

7.7 If time does not remain in the 12-hour period beginning with theinjection of the instrument performance check solution, a new injectionof the instrument performance check solution must be made. If the newInjection Beets the ion abundance criteria for BFB. then a continuingcalibration standard Bay be injected.

7.8 The concentrations of volatile target compounds in the continuingcalibration standard are given in paragraph 5.5.3.

7.9 The response factors for the continuing calibration standard must meetthe criteria given in paragraph 7.4.5 prior to the analysis of anyblanks or samples.

D-30/VOA OLM01.3 2/91

A R 3 I

SECTION IV

4.3.1 Prior to the analysis of any samples, blanks, orcalibration standards, the Contractor Bust establishthat the CC/MS system Beets the Bass spectral ionabundance criteria for the instrument performancecheck solution containingdecafluorotriphenylphosphlne (DFTPP) .

4.3.2 The analysis of the instrument performance checksolution Bay be performed as follow*:

o As an injection of up to 50 ng of DFTPP into theCC/MS

o By adding 50 ng of DFTPP to the calibrationstandards (paragraph 3.2) and analyzing thecalibration standard.

4.3.3 The analysis of the instrument performance checksolution Bust Beet the ion •>*"»"<-Tf T criteria givenbelow.

TABLE 1DFTPP KEY IONS AND ION ABUNDANCE CRITERIA FOR QUADRAPOLE MASS SPECTROMETERS

Mass Ion Abundance Criteria

51 30.0-80.0 percent of Bass 19868 Less Chan 2.0 percent of mass 6969 Present70 Less than 2.0 percent of Bass 69127 25.0-75.0 percent of Bass 198197 Less Chan 1.0 percent of Bass 198198 Base peak, 100 percent relative abundance (see note)199 5.0-9.0 percent of BASS 198275 10.0-30.0 percent of BASS 198365 Greater Chan 0.75 percent of BASS 198441 Present but less Chan BASS 443442 40.0-110.0 percent of Bass 198443 15.0-24.0 percent of mass 442

NOTE: All ion abundances MUST be normalized Co m/z 198, Che nominal basepeak, even Chough Che ion Abundances of m/z 442 Bay be up to 110 percent thatof m/z 198.

D-40/SV OLM01.0

A R 3 I m35

SEC7IOS IVi4.3.4 The abundance criteria listed above Bust be met for

•* 50 ng injection of DFTPP. The BASS speccrua ofDFTPP must be acquired in the following Banner.Three scans (Che peak apex scan and the scans

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immediately preceding and following Che apex) areacquired and averaged. Background subtraction isrequired, and muse be accomplished using a singlescan prior Co Che elutlon of DFTPP. Rote: Allsubsequent standards, samples. MS/MSD, and blanksassociated with a DFTPP analysis auat use IdenticalBASS spectroBeter instrument conditions.

mfl 4.3.5 The criteria above are based on adherence to theacquisition specifications identified in paragraph

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4.3.4. The criteria are baaed on performancecharacteristics of instruments currently utilized inroutine support of Program activities. Thesespecifications, in conjunction with relative

•response factor criteria for 54 target compounds(see Table 2), are designed Co control and monitorinstrument performance associated with therequirements of this Statement of work.

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4.3.6 The instrument performance cheek solution must beanalyzed once at Che beginning of each 12-hourperiod during which samples or standards areanalyzed.

The twelve (12) hour time period for A CC/MS systeminstrument performance check and standardscalibration (initial or continuing calibrationcriteriA) begins AC the aoawne of injection of CheDFTPP analysis thAt the laboraeory submits ASdocumentation of A compliant instrument performancecheck. The time period ends After twelve (12) hourshas elapsed according Co eh* system clock.

5. Calibration

5.1 Prior to the anAlysis of samples and required blanks, and After theinstrument performance check solution criteria have been met, eachCC/MS systea muse be CAllbrated AC A minimal of five concentrAtions codetermine instrument sensitivity And the lineATlty of CC/MS responsefor the seaivolACile target compounds. - •

5.2 The Internal standards are added to all calibration standards and allsample extracts (including blanks, matrix spikes, and matrix spikeduplicates) Just prior Co analysis by CC/MS. A 10 uL Aliquot of theinternal standard solution should be added Co A 1 aL Aliquot ofcalibration standards. The internal standards specified In paragraph3.1 should permit most of the seaivolACile cargac compounds co haverelative retention times of 0.80 Co 1.20, using Che assignments ofinternal standards to target compounds given in Table 2.

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SECTION IV

5.3 The quantitation ions for each internal standard Are given in Table 3.Use the primary ion listed In Table 3 for quantitation, unlessinterferences Are present. If interferences prevent Che use of theprimary ion for • given internal standard, use the secondary ion(s)listed in Table 3.

5.4 Prepare calibrACion starxiarda AC A Bint mum of five concentration levelsfor each target compound And surrogate, AS specified in paragraph 3.2.Analyze 2 uL of eech calibrACion standard and cabulata Che Area of theprimary characteristic Ion against eoneencration for each compoundincluding ehe surrogAte compounds. A 2 uL injection is reoulred.Calculate relative response factors (RRF) for each compound usingEquation 1.

Where,

AX - Area of the characteristic ion for Che compound Co be measured(see Table 4)

- Area of ehe char AC ter is tic ion for the specifie internalstandard (see Table 3)

- ConcentTAtion of the internal standard (ng/uL) VP

GX - ConcenCTAtion of Che compound to be measured (ng/uL) $&

5.5 The average relaclve response factor (RRF) must be CAlculAted for Allcompounds. CalculACe Che % Relaclve Standard Deviation (%ESD) of CheRRF values for Che initial calibration using the following equation:

%RSD - Standard Deviation x 100Mean

Where,

Standard Deviation -

nI <xi -

1=1

1/2

n-1

Where I

xi - •ach individual value used Co calculate Che BAAB I

x — Che mean of n values I

n - the total number of values I

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SECTION IV

5.6 Response factor criteria have been established for the calibration ofthe seaivolatile target compounds and seaivolaeile surrogate compounds.

5.6.1 The response factors of Che compounds listed in Table 5 musemeet Che minimum RRF criteria at each concentration level andmaximum %RSD criteria for Che initial calibration, withallowance Bade for up Co four seaivolACile CATget And surrogatecompounds. However, Che RRFs for Chose four compounds muse begreater Chan 0.010, And ehe %RSD of chose four compounds mustbe less than or equal Co 40.0% for Che initial calibration tobe acceptable.

RELATIVE RESPONSE FACTOR CRITERIA FOR INITIAL AND COKTINUINCCALIBRATION OF SEMIVOLATILE TARGET COMPOUNDS

Seal volatileCompounds

Phenolbls(-2-Chloroethyl)ether2 - Chlorophenol1 , 3-Dichlorobenzene1 ,4-Dichlorobenzene1.2- Dichlorobenzene2 -Methylphenol4 -MechylphenolN-Nlcroso - Dl - propylaaineHexachloroe thaneNitrobenzenelaophorone2-Nicrophenol2,4- Diae chy Ipheno 1bis ( -2-Chloroethoxy)me thane2 ,4-Dlchlorophenol1 . 2 . 4-TrichlorobenzeneNaphthalene4 - Chloro- 3 -aethylphenol2 -Mathylnaphthalane2.4, 6-Tr ichlorophenol2,4,5-Trichlorophenol2 - ChloronaphthalanaAeenaphthylene2 , 6 -Dinitro tolueneAcenaphcheneDlbenzofuran2, 4 -Dinitro toluene4 -Chloropheny 1 - pheny letherFluorene4-BroBophenyl-phenyletherHexAchlorobenzenePencaehlorophenol

MinimumRRF

0.8000.7000.8000.6000.5000.4000.7000.6000.5000.3000.2000.4000.1000.2000.3000.2000.2000.7000.2000.4000.2000.2000.8001.3000.2000.8000.8000.2000.4000.9000.1000.1000.050

Maxlm*Bi Maximum%RSD %Diff

20.5 25.020.5 25.020.5 25.020. 25.020. 25.020. 25.020.20.20.20.20.20.20.20.20.20.20.20.20.20.20.!20.!20.!20.!20.20.20.20.20.20.

25.025.025.025.025.025.025.025.025.025.025.025.025.025.0

i 25.0i 25.0i 25.0i 25.0

25.025.025.023.025.025.0

20.5 25.020.5 25.020.5 25.0

(continued)

AR3

SECTION IV

TABLE 5 (continued)RELATIVE RESPONSE FACTOR CRITERIA FDR INITIAL AND CONTINUING

CALIBRATION OF SEMTVOLATILE TARGET COMPOUNDS

SeaivolaclleCompounds RRF ttSD %Dlff

PhenanthreneAnthraceneFluoran thenePyreneBenzo(a)anchraceneChryseneBenzo (b) fluoran theneBenzo (k) fluorantheneBenzo ( a)pvrenelndeno(l,2.3-cd)pyreneDibenzo( a, h) anthraceneBenzo(g.h, DperyleneNi cr obenzene - d52 - FluorobipnenylTerphenyl-dj4Phenol -d52 - Fluorophenol2 - Chlorophenol - d41.2- Dichlor obenzene - d*

0.7000.7000.6000.6000.8000.7000.7000.7000.7000.5000.4000.5000.2000.7000.5000.8000.6000.8000.400

20.20.20.20.20.20.20.20.20.20.20.20.20.20.20.20.20.20.20.

25.025.025.025.025.025.025.025.025.025.025.025.025.025.025.023.025.025.025.0

5.6.2 The following compounds have no Maximum %RSD,•Difference criteria; however, these ccminimum RRF criterion of 0.010:

or Ma-ciauaC A

2,2'-oxybis(l-Chloroprop4-ChloroanilineHexachlorobucadieneHexAchlorocyclopentadiene2-NieroanilineDlaethylpbChalate3-Nltroanlline2,4-DinlCrophenol4-NitrophenolDiethylphthalate

) 4-Bitroanillne4,6.Diait3»-2-BeehvlpbenolN-NicroAodlpbeoyLaaliMDi-n-bueylphChAlAC*ButylbenrvlphehAlatA3.3*-Dlchlorobenzidlnebis(2-Ethylbexyl)phthalateDi -n-occylphchAlAce2,4,6-Tribroewph*nolCarbazola . |

5.7 A check of the CAlibrAtion curve must be performed once every 12 hours(sje paragraph A. 3.6 for Che definition of ehe twelve-hour time period).Cheek ehe relative response frvctors of those compounds for which RRFvalues have been esCAblished. If these criterle ATA met. ehe relativeresponse factors for all compounds are calculated and reported. Apercent difference of Che dAily relative response facCor (12 hour)compared co ehe average relative response factor froa Che iniCiAl curveis calculated. Calculate ehe percent difference for each compound Andcompare with Che maximum percent difference criteria listed above. Fornegative percent difference value*, Che value Bust be greACer than orequal Co -25.0%, but less than 0%.

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SECTION IV

As with the initial calibration, up to four semivolaCile targetcompounds in Table 5 may fail to meet the minimum RRF or maximum IDcriteria, but che RRFs of Chose four compounds muse he greater Chan orequal Co 0.010, and Che percent differences must be less than or equalto 40.0% for che concinuing calibration to be acceptable.

5.8 Internal standard responses and retention times in all standards must beevaluated during or iamedlACely After daca acquisition. If che retentiontime for any internAl standard changes by aore Chan 0.50 ainutes (30seconds) froa ehe latest daily (12 hour) calibration standard, ehechromatographic system must be inspected for mslf unctions, Andcorrections made AS required. The extracted ion current profile (EICP)of che InternAl standards muse be monitored and evAluated for eachstandard. If che EICP area for any internal scandArd changes by morethan a factor of two (-50% Co +100%), the BAAS speccroaetric system mustbe inspected for malfunction, and corrections made AS appropriate. Whencorrections are Bade, re-analysis of samples analyzed while Che systemwas malfunctioning is necessary.

5.9 Each CC/MS system aust be calibrated upon award of eh* contract,whenever the Contractor takaa corrective action which may change oraffect the initial calibration criteria (I.e., ion source cleaning orrepair, column removal or replacement, etc.), or if eh* continuingcalibration acceptance criteria have not been met.

5.10 If tiae remains In Che 12 hour Ciae period After meeting eh* acceptancecriteria for che initial calibration, samples may be Analyzed. Ic isnot necessary Co analyze a concinuing calibration standard, if eheinitial CAlibrAClon standard chat is che ssae concenerACion AA ehecontinuing calibration standard meets eh* continuing caUbraeionacceptance crlteriA. Quaneify All saaple results against che initialcalibration standard that Is ehe SAB* concentration AA ehe continuingcalibration standard (SOng/2uL).

5.11 If time does NOT remain in the 12-hour period beginning with eh*injection of the instrument performance check solution, a new injectionof che inseruaeac performance check soluclon ausc b* a*d*. The DFTPPaay be included in eh* concinuing CAlibrAClon scandArd.

5.12 If che Injection of ehe instruaene perforaAnce check solution Beets checriteriA in Table 1, calculate che response faccors for ehe continuingcalibration scandArd and che percent difference of eh* response factorsfroa che Bean response factors in che inielAl calibrACion.

5.13 The response factors froa che concinuing calibration scandard must meetche criteria in Table 5 prior co che analysis of Any blanks or samples.

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fet> SECTION n:

of the instrument blank Chat bracketts the front end of the samples.Because che 12-hour time period is timed from injection of theinstrument blank until che injection of che last sample, each 12-hourperiod may be separated by che length of one chromatographic run. thatof the analysis of the last sample. While che 12-hour period may notbe exceeded, the laboratory BJZ tun instrument blanks and standardsmore frequently, for Instance co aeeoaodata staff working on 8-hourshifts.

5.2 Before any samples are analyzed, it is necessary for the Contractor tocomplete an acceptable initial calibration sequence (see paragraph 6).

5.3 After the initial calibration, che analysis sequence may continue aslong as acceptable instrument blanks. Performance Evaluation Mixtures,and Individual Standard Mixtures A and B are analyzed at the requiredfrequency (see paragraph 7). This analysis sequence shows only theminimum required blanks and standards. More blanks and standards maybe run at the discretion of Che Contractor; these must also satisfy ehecriteria presented in paragraph 7 in order to continue the runsequence.

5.4 An analysis sequence Bust also include all required matrix spike/matrixspike duplicate analyses and method blanks, hue ehe Contractor maydecide at what point in the sequence they are Co be analyzed.

5.5 A scandArd of Any identified Aroclor Bust be run within 72 hours of itsdetection in A aaaple chromatogram.

6. Initial Calibration

6.1 Initial Calibration Sequence

6.1.1 Before Any SA^ples Are analyzed, 1C 1* neeessary for cheContTACtor co complete eh* inlei*! CAlibrAClon sequence givenbelow.

NOTE: Steps 16 and 17 AT* used AA part of Ch* ealibrACionverification as well (see paragraph 7).

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INITIAL CALIBRATION SEQUENCE

1. Resolution Check2. Performance Evaluation Mixture3. Aroclor 1016/12604. Aroclor 12215. Aroclor 12326. Aroclor 12427. Aroclor 12486. Aroclor 12549. ToxAphene10. Low Point Standard A11. Low PoinC Scandard B12. Midpoint Standard A13. Midpoint Standard B14. High Point Standard A15. High Point Standard B16. Inscrumenc Blank17. Performance Evaluaeloa Mixture

6.1.2 Samples aay be analyzed only after eh* j«fH«t calibrationacceptance criteria (6.2) ATA met. Ocharwi**, eh* analyticalsystem is not functioning AdequAtAly for use vich thisprotocol.

6.1.3 The inltJAl CAlibrAClon aay eonclnu* Co b* ua*d AA long AA cheanalytical ays tea reaAln* uoder concrol. The proof ebAC eheanalytical system is under concrol is provided by eh* Analysesof ehe Performance EvAluation MlxcureA. If the** analys** donot aeet Che criteria described la paragraph 7, Appropriatecorrective Action must b* taken. And eh* inlet*! calibrationsequence must b* repeated. The ealibracion eequence must alsob* repeated if any aajor change in ln*crua*ne hardware orinscrumenc p*rAa*e*rA is Bade (e.g., if A n*w column isinstalled or If che detector temperature Is changed).

6.2 InitiAl Calibracion Accepcance Criteria (apply Co each CC column Iindependently) (

6.2.1 The initial calibration sequence must be anAlyzed in che orderlisted in paragraph 6.1 using the optimized CC/EC operecingconditions described in paragraph 4. The standards must b*prepared according to paragraph 3. Calculace the calibrationfactors and retention times According co paragraphs 8-10.

6.2.2 The resolution criterion is that che oapch of the valley |between two Adjacent peaks in the Resolution Check Mixture musebe greAter chAn or equal Co 60.0% of the height of che shorter |peAk. The poorest resolution on ehe DB-608 column probkbly

- will be between DDE And Dieldrin, between Methoxychlor AndEndrin ketone And between Endosulfan I and gamma-Chlordan*. Onche DB-1701 column, resolution difficulties aosc frequentlyoccur between Endosulfan I and gamma-Chlordan*, and betweenMechoxyehlor and Endosulfan sulfate.

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6.2.3 The breakdown of DDT and Endrin in both of the PerformanceEvaluation Mixtures must be less than 20.0 percent, and thecombined breakdown of DDT and Endrin must be less than 30.0percent where,

EQ.2

% Breakdown DDT - Amount found in ny fDDD+DDE> * 100Amount in ng of DDT injected

EQ.3

% Breakdown Endrin -

AtBQUTit found in ng fEndrin aldehyde + Endrin ketone} * 100Amount of Endrin injected In ng

EQ.4Combined % Breakdown - %Breakdown DDT + %Breakdown Endrin

6.2.4 All peeks in both of Che Performance Evaluation Mixtures must• be 100 percent resolved on both columns.

6.2.5 The absolute retention times of each of Che single component

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pesticides and surrogates in both of che PEMs must be withinChe retention time windows determined froa Che three-pointinitial calibration, in paragraph 8.4.

6.2.6 The relative percent difference of the calculated amount andChe true amount for each of Cb* single component pesticides andsurrogates in boeh of eh* PEMs Bust b* IAAA Chan or equivalentCo 25.0 percent, using equation 5.

6.2.7 AC least one chromatogram froa AAch of eh* two IndividualStandard Mixtures A And B, run during eh* tMMml cAlibrACion,must yield peaks that give recorder deflections of 50 Co 100percent of full scale.

6.2.8 The resolution between any two adjacent peaks in the midpointconcentrations of Individual SCandard Mixtures A and B in eh*inieial calibration must b* greater than or *ou*l to 90.0percent.

6.2.9 Thi % RSD of ehe calibration factors for each single componenteargee compound aust be leas than or equal Co 20.0 percent,except AS noted below. The % RSD of the ealibrAClon factorsfor Che two surrogates must be leas Chan or equal Co 30.0percent. Up to two single component CArget compounds (hue notsurrogates) per column may exceed the 20.0 percent limit for%RSD, but chose compounds must have a % RSD of leas than orequal to 30.0 percent.

%RSD — Standard Deviation x 100Mean

B]

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Where.

S 2 1/2

2, (xt - x)*Standard Deviation - i-1

n-1

Where.

xt - each Individual value used tc Calculate the mean

x » che aean of n values

n - ehe total number of VA!U*A

6.3 Corrective Action

6.3.1 If eh* technical acceptance criteria for ehe inieialcalibrACion ATA not aee, inspect eh* system for problem*. Itmay b* necessAry Co change the column, bake ouC Che detector,clean Che injection pore, or take ocher corrective actions toachieve che Acceptance crlteriA.

6.3.2 Contamination should be suspecced A* A cause if eh* detectorcannot achieve ACceptAble lineATicy using Chi* aechod. In checAse of light contaaination, Mng out the detector at Anelevated c*ap*rACure (350*C) should b* sufficient Co AchieveACceptAble perforaancA. In ehe caa* of heavy contaminAtion.passing hydrogen through eh* d*C*ceor 1-2 hour* AC an elevetedteaperACure BAJ correce eh* problem. In Che CAAA of severecontamination, che detector aay require servicing by che ECDmanufacturer. DO NOT OPEN THE DETECTOR. THE ECD CONTAINSRADIOCHEM1CAL SOURCES.

6.3.3 If a laboratory cleans out a detector using An elevatedtemperature, che BCD electronics must be turned off during th.bak* ouc procedure.

6.3.4 Afcar bake ouc or hydrogen reduccion, ehe deCecCor aust berecellbrated using Che initial calibrAtion sequence.

6.3.5 Inieial calibrition technicAl acceptance criceria MUST b* metbefore Any samples or required blank* Are analyzed. Anysamples or required blanks analyzed after ehe inieialcalibration criteria have not been met will require reanalysisAC no additional cost co Che Agency.

7. Calibration Verification

7.1 Three types of analyses are used Co verify Che calibracion And eveluateinstrument performance. The analyses of instrument blanks, PerformAnceEvaluation Mixtures (PEM). and Che aid point concentration of IndividualStandard Mixtures A and B constitute the continuing

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calibration. Sample data are not acceptable unless bracketed byacceptable analyses of instrument blanks, PEM, and both IndividualStandard Mixtures A and B.

7.2 An instrument blank and Che Performance Evaluation Mixture must bracketone end of a 12-hour period during which sample data are collected, anda second instrument blank and Che Che aid point concentration ofIndividual Standard Mixtures A and B must bracket ehe other end of the12-hour period.

iiII

7.3 For che 12-hour period immediately following the inieial calibrationsequence, Che inscrumenc blank and che PEM that are Che last two steps

I in Che initial calibration sequence bracket che front end of that 12-hour period. The injection of che instrument blank starts ehebeginning of that 12-hour period (see paragraph 5.1). Samples may be

( injected for 12 hours from the injection of Che instrument blank. Thethree injections <«••««araly A£CJX Chat 12-hour period must be aninstrument blank. Individual ScandArd Mixture A, and Individual

_ Standard Mixture B. The inscrumenc blank muse be analyzed first,I before either standard. The Individual Standard Mixtures may be' analyzed in either order (A.B or B.A).

7.4 The analyses of the instrument blank and Individual Standard Mixtures Aand B immediately following one 12-hour period may be used to begin chesubsequent 12-hour period, provided that they meet Che acceptancecriteria in paragraphs 7.8-7.14. La chat instance, eh* subsequent 12-hour period Bust be bracketed by Che acceptable aaAlyses of Aninstrument blank and a PEM, in that order. Those two analyaea aay inturn be used Co brack*c che front end of yet another 12-hour period.This progression may continue every 12 hour* until such time as any ofche instrument blanks, PEMs, or Individual Standard Mixtures fails eomeet che acceptance criteria in paragxvhs 7.8-7.14. The 12-hour timeperiod begin* wich eh* injection of eh* inscrumenc blank. Standards(PEM or Individual Standard Mixtures), samples and required blanks maybe injected for 12:00 hours froa ehe time of injection of cheinscrumenc blank.

7.5 If more than 12 hours have elapsed since eh* injeccion of eheinstrumenc blank that brackscad a previous 12-hour period. Anacceptable insertiMnc blank and PEM BUJ£ be analyzed in order eo starta new sequence. * Ibis requirement applies evem if no analyses wereperformed since that standard(s) was injected.

7.6 After a break in sample analyses, Che laboratory may only resume theanalysis of samples using the current initial calibration forquantitation by analyzing an acceptable inscrumenc blank and a PEM.

7.7 If ehe encire 12-hour period is not required for ehe analyaea of allsamples to be reported and all data collection is to be stopped, cheincomplete sequence must be ended with either the instrument blank/PEMcombination or ehe inscrumenc blank/Individual Standard Mixture* A andB combination, whichever was due to be performed at che end of 12-hourperiod.

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7.B Analysts are cautioned Chat running an instrument blank and a Iperformance evaluation aixcure once every 12 hour* i* che ainimumcontract requirement. Lace elutlng peaks aay carry over froa oneinjeccion co the next if highly complex samples are Analyzed or if theGC conditions are unstable. Such carryover is unacceptable.Therefore, It Bay be necessary co run instrument blanks And performanceevaluation mixtures more often Co avoid discarding datA.

.7.9 The requirements for running Che instrument blank*, Performance |Evaluation Mixture, and Individual ScandArd Mixture* A And B Are waivedwhen no samples, method blank*, or BAtrix spikes ATA run during that12-hour period. After A break la cample AnAlyci*, A laboratory mayresume che analysis of samples, method blank*. And BAtrix spikes andaay use che current initial calibration for quancleaclon on^y After AnAcceptable FEN i* run (paragraph* T.2 - 7.6). If A successful PEMcannot b* run after An interrupt:.-a. An accApcable inlclal calibrationmust be run before sample daCA may b* collected. All acceptable •ampleanalyses muse be bracketed by acceptable performance evaluationmixtures and instrument blanks.

7.10 Technical Acceptance Criteria (Apply eo eech CC column independently) |

7.10.1 All *ingle component pesticides And surrog*t*s In ehePerformance Evaluaeion Mixture* used eo demon*tr*ee continuingcalibration Bust be 100 percent re*olv*d. Th* rvaolueionbetween Any two AdJAcenc peak* in Che aldpoinc concencratlon*of Individual Standard Mixtures A And B in Ch* laitl*!CAlibrAClon must be greater Chan or equal to 90.0 percent.

7.10.2 The Absolute retention time for e*ch of th* single componentpesticides And surrogates in Che PEMs and. "id poineconcentration of eh* IndlviduAl Standard Mixture* us*d todemonscrate continuing calibrAtion must b* vitals eh* r*t*ntiontime window determined froa Che -diree-point iaitiAl calibrationin paragraph 8.4.

7.10.3 The reLacive percent difference of Che calculated saounc And |the true Amount for each of th* cingle component peccleide* Andsurrogates in ehe PEM and aid poinc concentration of eh*Individual Standard Mixtures used Co damon*cr*t* concinuingCAlibrAClon Bust be less than or equel to 25.0 percent, usingEquation 5.

* Cc.lclRPD x 100 EQ. 5

Cnoa

- true concentration of each analyte |

- calculACAd eoneencrACion of eech analyte froa eh*analyses of che standard

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Note: The vertical bars in Che equation indicate the absolutevalue, hence RPD is always a positive number.

7.10.4 The percent breakdown of DDT and Endrin in che PEM must be lessChan or equal to 20.0 percent on both columns. The combinedbreakdown of DDT and Endrin must be less than or equal to 30.0percent on both columns.

7.10.5 All instrument blanks must meet the acceptance criteria inparagraph 15.3.

7.11 Corrective Action

7.11.1 If the technical acceptance ericeria for Che calibrationverification are not met, inspect the system for problems and

__ cake corrective action Co achieve Che acceptance criteria.

^ 7.11.2 Major corrective actions such as replacing Che CC column orbaking out ehe detector will require that a new Initial

•calibration be performed and meets the technical acceptancecriteria in 6.2.

•

7.11.3 Minor corrective actions may not require performing a newinitial calibration, provided Chat a new analysis of chestandard (PEM or Individual Mixture) ChAC originally failed checriteria and an associated instrument blank immediately after

mm che corrective action do meet all che acceptance criteria.

7.11.4 If che analysis of che standard and instrument blank in 7.11.3fall any of che technical acceptance criteria, a new initialcalibration mu££ be performed.I

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8. Determination of Absolute Retention Ti»*a1

8.1 During Che initial calibration sequence, absolute retention times (RT)are determined for All single response peccicid**. ehe surrogates, andat lease three major peaks of each auleieoaponeme analyca.

8.2 For single component peseicides, an RT i* measured in **ch of Chreecalibration standards and che mean RT is calculated AA Che average ofChe three VAlues. An RT i* aeasured for Che surrogAtaa in each of ehechree Analy*A* of Individual Mixture A during eh* initial calibrationand Che Bean RT i* calculated as che average of Che three value*.

8.3 A retention time window is calculated for each single component analyteand surrogate by using the list in paragraph 8.4. Windows are centeredaround Che mean absolute retention time for che Analyte establishedduring ehe inieial calibrations.

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8.4 Retention time windows for single And multicomponent analyses andsurrogates.

Retention Time WindowCompound in Minutes

alpha-BHC ±0.05beta-BHC ± 0.05lamma-BHC ± 0.05d*lca-BHC ± 0.05Heptachlor ±0.05Aldrin ± 0.05alpha-Chlorodan* ± 0.07gamma-Chlorodan* ±0.07Heptachlor epoxide ±0.07Dieldrin ±0.07Endrin ± 0.07Endrin aldehyde ± 0.07Endrin ketone ± 0.07DDD ± 0.07DDE ± 0.07DDT ± 0.07Endosulfan I ± 0.07EndoAulfAn II ±0.07EndoAulfAn sulfat* ±0.07Itothoxycblor ±0.07Aroelors ±0.07Toxaphene ±0.07TetrAchloro-m-xylen* ± 0.05Decachlorobiphenyl ±0.10

8.5 For each muleicoaponent AnAlytA. che RT* for Chree to five peaks arecalculated froa Che inielAl ealibrACion standard analy*iA. An RTwindow of ±0.07 minut*s 1* used for All multicomponent aoAlyt* p*aks.

8.6 Analytes are identified when peaks are observed in the RT window forche compound on boch CC column*.

9. Calibration Factors for Sltiylej Component Pesticides

9.1 During the initial calibrAtion sequence, eh* ContTAcCor Bust **tabll*h 'che magnitude of eh* linear ECD response range for each ainglecomponent pe*clcide And AurrogAt* on AAch column and for each CCsystem. This i* Accomplished by anAlyzing ehe Individual SeandardMixtures A and B at chree concentrations during eh* initial c*librAtironsequence in pAragraph 6.

9.2 The linearity o£ ehe instrument i* determined by CAlculAting A percentrelative standard deviation (%RSD) of Che calibracion fActor* froa Athree-point CAlibration curve for each tingle component poscicid* andsurrogate. Either peak area or peak height may b* used eo calculatecalibracion fACtors used in ehe %RSD equation. For example, it 1*permitted to calculate linearity for Endrin baaed on p**k area and cocalculate linear icy for Aldrin baaed on peak height. It 1* not

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permitted within A %R5D calculation for an analyte to use calibrationfactors calculated froa both peak area and peak height. For example,it is na£ permitted to calculate che calibracion factor for ehe lowpoint standard for endrin using peak height and calculate the midpointand high point standard calibration factors for endrin using peak area.

9.2.1 Calculate ehe calibracion factor for each single componentpesticide And currogACA over ehe iniclAl calibration rangeusing Equation 6. The calibration factors for eh* surrogatesare calculated froa ehe chree analyses of Individual StandardMixture A only.

___ 9.2.2 Calculate ehe aean and ehe %RSD of ehe calibration factors for• each single componenc pesticide and surrogate over the initial^ calibration range using Equations 7 and 8.

•CF — Peak Area (or Hetyht> of tjjf. SfiTUJlTd EQ. 6

Mass Injected (ng)

% RSD -— x 100

EQ. 8

CF - CalibrACion fACtor

Where.

,SCandard Deviation - ' _

n-1

I1/2

1 cr- £ J.

1

I

I

I

I

I

I

I

I

I

I

Where,

Xi - eAch individual value uaed Co cAlcuLetA che Been

x - eh* B*An of n valu**

n - eh* total number of values

9.2.3 The linear icy of th* c*librAtion i* considered Acceptable wheneh* % RSD of eh* three point calibration i* less Chan 20.0percent except A* noc*d in Che following.

The % RSD of che two surrogates muse b* leas than or equal to30.0 percent. Up co two single componenc car get compounds (but |not •urrogAtas) per column a*y exceed eh* 20.0 percent limitfor % RSD., but Chose compound* Bust have a % RSD of less Chanor equal Co 30.0 percent.

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A R 3 I

9.2.4 If ehe linearity requirements listed above are met. ChecAlibration fACtor froa ehe aid point concentration standard isused for quantltation of each single component pesticide.

9.3 Sample analysis may not proceed until a satisfactory calibration hasbeen demonstTAted.

10. Calibration Factors for Tpraphene and Aroelqr^

10.1 Toxaphene and Aroclor* require only a single-point calibration and theypresent special analytical difficultie*. Because of eh* Alteration ofthese materials in ehe environmenc, ie 1* probable that samples whichcontain lultieomponent analytes will give patterns similar to, but notidentical with. Choi* of eh* •eandarda.

10.2 A sec of three Co five major peaks i* selected for each mulcicomponencanalyte. R*e*ntion Ciae* (*e* 8.4) and calibration faceor* ATAdetermined froa ehe initial calibrACion analysis for each peak.Guidance for che choice of which peaks Co use is given in paragraph13.9

11. Acceptance Criteria toT Chromatograms of Calibration Stan* ar<jg

The identification of single component pesticides by gaschroaatographic methods is based primarily on r*nc*nclon cim* data.The retention time of che ipex of A p**k can be verified only froa Anon-scale chromatogram. The identification of aulticoaponent analytasis based primarily on recognition of pattarn* of ntaation cim**displayed on a chromatogram. Therefore, ehe following requiremencsapply co all data presented for single componenc and mulcicomponencanalytes.

11.1 The chromacograma that resule froa eh* Analy*** of th* l**olution CheckMixture, che Performance Evaluation Mixture, and IndlvlduAl StandardMixtures A and B during Che inltJAl calibracion sequ*nce ausC displayche single component analytea present in each standard AC greater Chan10 percenc of full *cal* buC IAA* Chan 100 percent of full Acale.

11.2 The chromatograms, for at lease one of Che ehre* an*lyees each ofIndividual SCAndard Mixture* A And B froa eh* initial c*libr*tlonsequence, must display ehe single componenc analyt** At greater Chan 50percenc and less than 100 percent of full scale.

11.3 The chromaeogram* of Che standards for the muleicomponanc analytesanalyzed during the InitiAl CAllbrAtlon Aequence BU*C dicplay th* peakschosen for identification of each analyt* at grAat«r Chan 25 percentand less Chan 100 percent of full scele.

11.4 For Any sCAndard eoncaining Alpha-BBC, eh* bAsellne of ehe chroaatograa- must return Co below 50 p*re*nc of full scale before che elution cim*

of alpha-BHC, And return Co below 25 pereenc of full scale After Cheelution time of alpha-BHC and before eh* elucion time ofdecachlorobiphenyl.

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AR3! 11*50

IIII

11.5 If a chromacogram is replotted electronically to meet requirement*, chescaling factor used must be displayed on che chromacogram.

11.6 If ehe chromacogram of any standard needs Co be reploccedelectronically to meet these requirements, both the Inieialchromatograa and ehe replotted chromacogram must to submitted in chedata package.

12. fiPT1* Analysis

12.1 Unless ambient camperacure on-column injection is used (see paragraph4.2), che injeceor muse be heated co at lease 200'C. The optimized gaschromatographic conditions from paragraph 4 must be used.

^ 12.2 The injection muse be made on-column by using either automatic ormanual injection. If autoinjectors are used. 1.0 uL injection volumes

•may be used. Manual injecCion* ahall use ae least 2.0 uL injectionvolumes. The same injection volume must be used for all standards,samples, and blanks associated with che earn* inieial calibration. If a

•

single injecCion i* used for two CC columns attached to a (ingleInjection port, it may be necessary Co use an injecCion volume greaterChan 2 uL. However, Che same injection volume must be used for ellanalyses.

^ 12.3 Analysis of a sample on both CC columns is required for all samples,blanks, matrix spikes, and matrix spike duplicates.

12.4 The requirements for che analysis sequence Apply Co both CC column* andfor all Instruments used for Chase analyses.

12.5 The laboratory will Identify and quantitate analyte peak* based on RTand calibracion factor established during ehe inieial calibrationsequence, as long a* an acceptable calibration verification (see

• paragraph 7) i* performed every 12 hour*.

12.6 The protocol 1* Intended Co achieve che quancitation limics ahown inExhibit C whenever poaaibl*. If •ample chromacogram* have ineerferlngpeaks, a high baseline, or off-ecele peaks, Chen Choee Maple* auat b*reanalyzed following dilution, further cleanup, or z**xerAcclon.Samplea which eannoc be made eo m**c ehe given specificACiona afcar on*reexeraceion and Chree-step eLianup (CPC. Florisil, And sulfur removal)are reported in Che SDG NATTAtive And do not require further analyai*.No liaic i* plAced on ehe number of reextraction* of samples Chat maybe required because of contaminated method blank*.

12.7 The sample must b* analyzed at the moat concentrated level that i*consistent with achieving satisfactory chroaatography (defined below).If dilution is employed solely co bring a peak wirhln Che calibrationrange or to get A aulticomponent pattern on scale. Che results for both

I . che more and ehe less concentrated extract must be reported. The(

Iresulting changes in quantieaclon limics and surrogate recovery must bereported also for che diluted sample*.

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8

10.1 Summary

10.1.1 The instrument is calibrated with a blank, 0.2 ug/L, 0.5ug/L, 1.0 ug/L, and 5.0 ug/L mercury solution (in thatorder).

10.2 Initial Calibration Procedures

10.2.1 Instrument is warned as follows: Lamp B is warmed for10-15 minutes by adjusting it to 100X absorbance. LampA is warmed for 10 - 15 minutes by adjusting it to OXabsorbance. Instrument set-up and optimization isperformed according to • the instrument manualspecifications.

10.2.2 A digested calibration blank is analyzed and the XAbsorption is recorded on the strip chart recorder. Theresult is then converted to absorbance and recorded onthe mercury log sheet. After the blank, the digestedcalibration standards are analyzed and theirabsorbencies recorded.

10.2.3 The correlation coefficient for the curve must be >.0.995. If it is not, redigestion and recalibration isrequired.

10.2.4 Initial Calibration Verification (ICV)

After the calibration has been performed, a standard ofknown concentration from an independently preparedsolution must be analyzed to verify the curve. Resultsof this standard must be within + 20X of the true value.If not, the calibration curve and samples must bereprepared and reanalyzed. This standard is also takenthrough the digestion procedure with the samples.

10.2.5 Initial Calibration Blank

This sample is carried through the digestion with thesamples. The result of this standard must be less thanor equal to the absolute value of the CRDL. If not.reprepare the standards and samples and recalibrate.

10.3 Continuing Calibration Procedures

10.3.1 Continuing Calibration Verification (CCV).

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b.1.5

6.1.6

6.1.7

6.1.8

6.2 Standards

b.2.1

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Sulfuric Acid , H,SO., Concentrated: Reagent grade.V I

Sulfuric Acid, 0.5 N: Dilute 14.0 ml of concentratedsulfuric acid to 1 liter in Type II water.

Nitric Acid, Cone. : Reagent grade of low mercury content

Stock Mercury Solution: A 1000 ug/ml mercury stocksolution is purchased from a commercial vendor. Thestandard is NIST traceable.

Working Mercury Solution: Make successive dilutions ofthe stock mercury solution to obtain a working standardcontaining 1 ug per ml. This working standard and thedilutions of the stock mercury solution should beprepared fresh daily. Acidity of the working standardshould be maintained at 0.15X nitric acid. This acidshould be added to the flask as needed before theaddition of the aliquot.

6.2.1.1 Calibration Standards for Mercury are prepared at0.2, 0.5, 1, and 5 ug/1

6.2.2 Matrix Spike Solution: Prepared from Mercury stocksolution by adding 1 ml of stock solution to a 1 litervolumetric flask, 150 ul of cone, nitric, and dilutingto the mark with ASTM Type II water.

6.2.3 ICV Solution: Mercury ICV Stock Solution is obtainedfrom EMSL/LV. An alternate source for the ICV solutionhas been identified.

6.2.3.1 Preparation of the ICV/CCV working calibrationstandard: Partially fill a 100 ml volumetricflask with ASTM Type II (reagent) water. Add 2•1 of concentrated nitric acid and 0.5 ml of thestock ICV solution. Dilute to the mark with ASTMType II water. Prepare fresh daily.

6.2.4 Laboratory Control Sample (LCS)

A solid LCS must be prepared with each batch of solidmatrix samples. The LCS material is supplied byEMSL/LV. An alternate source for the LCS material hasbeen identified. The LCS material is prepared as permanufacturer's instructions.

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9.2.8 Immediately attach the bottle to aeration apparatus.

9.3 Standards Preparation

9.3.1 Calibration Standards

9.3.1.1 10 ml volumes of Hg standards at 0.2 ug/1, 0.5ug/1, 1.0 ug/1 and 5 ug/1 concentrations areprepared.

9.3.1.2 The 10 ml volumes of standards are preppedaccording to procedures in section 9.2.

9.3.2 ICV/CCV

9.3.2.1 A 10 ml volume of a mid-point range standard forMercury is prepared

9.3.2.2 The 10 ml volume of standard is prepped accordingto procedures in 9.2.

9.3.3. Laboratory Control Sample, Solid Matrix

9.3.3.1 Weigh a manufacturer's requested portion ofstandard material.

9.3.3.2 Prepare according to procedures described insection 9.2.

9.3.4 ICB, CCB, Prep Blank

9.3.4.1 Place 10 ml of reagent water in the BOD bottle.

9.3.4.2 Prepare each blank according to the procedures in9.2

9.4 QC Sample Preparation

9.4.1 A single matrix spike must be prepared with each batchof the same type, same matrix samples. The matrix spikeis prepared by adding 1.0 ug/1 of mercury to the 0.2 gportion of sample.

9.4.2 A sample duplicate must be prepared with each batch ofthe same type, same matrix samples.

10. INSTRUMENT CALIBRATION

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6

Nickel Nitrate Solution (0.1X): Dissolve 0.496 s. ofreagent grade Nit NO- ).,6H.,0 in reagent water and dilute to100 ml. ' : :

Sulfuric Acid (l.OX): Dilute 1.0 ml of reagent ?rndeH,SO, to 100 ml with reagent water

Ammonium phosphate (IX): Dissolve 1 g of reagent grade(NHj),HPO, in 100 ml of reagent water

Hydrogen peroxide, 30X of reagent grade

6.2

b.1.3

6.1.4

6.1.5

6.1.6

Standards

6.2.1 ICV/CCV Solutions are supplied by EMSL/LV. An alternatesource has been identified if it should be needed. ICV-2 Standard contains arsenic and selenium. ICV-4Standard contains lead and thallium. Concentrations aresupplier and batch dependent.

6.2.1.1 Arsenic and Selenium:

Partially fill a 100 ml volumetric flask withASTM Type II (reagent) water. Add 4 ml of 1:1nitric acid. Pipet 5 ml of the ICV-2 solutioninto the flask. Fill the volumetric flask to themark with reagent water.

6.2.1.2 Lead and Thallium:

Partially fill a 100 ml volumetric flask withASTM Type II (reagent) water. Add 4 ml of 1:1nitric acid. Pipet 5 ml of the ICV-4 Solutioninto the flask. Fill the volumetric flask to themark with ASTM Type II water.

6.2.2 Calibration Standards Preparation:

From the stock standard prepare a series of standardsthat define the linear range of the instrument bringingall final volumes to 100 ml with reagent water. Theleast concentrated standard must be at the CRDL. Thestock standard is prepared commercially and is NISTtraceable. Dilutions of lead and thallium stockstandards are prepared with 4 ml of 1:1 nitric. Forarsenic and selenium standards, 2 ml of 30X hydrogenperoxide are added along with 2 ml of 1:1 nitric acid.

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6.2.2.1 3 or 4 calibration standards and a blank areprepared by analyst or instrument. The workingranges of the standards are as follows:

As 10 ppb - 80 ppbSe 5 ppb - 80 ppbPb 3 ppb - 80 ppbTl 10 ppb - 80 ppb

6.2.3 Analytical Spike Preparation:

From the calibration stock, solution prepare analyticalspiking solutions so that the concentrations in thesamples are as follows:

As 20 ppbSe 10 ppbPb 20 ppbTl 20 ppb

Dilutions of the stock standards are prepared withreagent water, and 4 ml of 1:1 nitric acid in a 100 mlvolumetric flask taken to volume.

6.2.4 CRA Standard

CRA standard is prepared from the purchased calibration stocksolution. The final concentration for each analyte in thesolution are as follows:

As 10 ppbSe 5 ppbPb 3 ppbTl 10 ppb

Dilutions of the stock standard are madevolumetric flask, with reagent water and 4 mlacid.

in a 100 mlof 1:1 nitric

7.

8.

SAMPLE PRESERVATION AND STORAGE

7.1 Samples are stored as extracts in plastic or glass containers.

HOLDING TIMES

8.1 The holding time is six months from date of sample receipt to thecompletion of analysis.

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acid to 500 ml of reagent water

6.2 Standards

6.2.1 ICV (Initial Calibration Verification) and ICB (InitialCalibration Blank)

6.2.1.1 Partially fill a 100 ml volumetric flask withASTM Type II water I reagent water).

6.2.1.2 Add 4 ml of 1:1 nitric acid

6.2.1.3 Pipet 10 ml of the ICV-1 Solution into the flask.ICV solutions are supplied by EMSL/LV. Analternate source has been identified

6.2.1.4 Pipet 10 ml from the ICV-3 solution into theflask.

6.2.1.5 Fill the volumetric flask to the mark with TypeII water (reagent water).

6.2.1.6 ICV solution 1 contains Al, Ba, Be, Cd, Ca, Cr,Co, Cu, Fe, Pb, Mg, Mn, Ni, K, Ag, Na, V, and Zn.Solution 3 contains Sb. Concentration aremanufacturer-dependent.

6.2.1.7 ICB is prepared by taking 2 ml 1:1 Nitric acidand 10 ml of 1:1 hydrochloric acid; dilute to 1liter in a volumetric flask with ASTM Type IIwater.

6.2.2 Calibration Standards

6.2.2.1 From purchased stock standards (NIST traceablequality) prepare a series of standards to be usedin instrument calibration. Below is the list offinal calibration standard concentrations

Standard 1: 10 PPM Ba,Ca,Cd,Co,Cr,Cu,Mg,Mn,Pb,V,Zn; 100 PPM K

Standard 2: 1 PPM Ag.Be; 10 PPM Al,Fe,Na,Ni

Standard 3: 10 PPM Sb,Se

6.2.2.2 Acidify standards with 2 ml of 1:1 HNOj and 10 ml1:1 HC1 per 100 ml reagent water.

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6.2.2.3 Calibration Blank Solution is prepared in thelaboratory by adding 2 ml 1:1 nitric acid and 10ml 1:1 hydrochloric acid diluted to a liter withASTM Type II water.

6.2.2.4 Store prepared standards in unused polyethylene

6.2.3 QC Standards

6.2.3.1 CRI Standard is prepared from the purchased stocksolution of NIST traceable quality. Finalconcentration for each analyte in the solutionare as follows:

Sb 120 ug/L Cu 50 ug/L Zn 40 ug/LBe 10 ug/L Mn 30 ug/L Pb 2 x IDLCd 10 ug/L Ni 80 ug/LCr 20 ug/L Ag 20 ug/LCo 100 ug/L V 100 ug/L

Fe, Al, Ba, Ca, Mg, K, and Na do not requireCRI Standard Analysis.

6.2.3.2 ICS (Interference Check Standard Solution) A andAB are obtained from EMSL/LV and prepared as permanufacturer's instructions. Concentrations aredetermined by manufacturer. An alternate sourcefor the ICS A and AB solutions are available.

7. PRESERVATION AND STORAGE

7.1 Samples are stored in plastic or glass containers.

8. HOLDING TIMES

8.1 The holding time is six months from date of sample receipt to thecompletion of analysis.

9. OPERATING CONDITIONS AND CALIBRATION

9.1 Instrument Tuning

9.1.1 Follow the instrument manufacturer's recommendations forinstrument set-up and optimization before analysis.

9.2 Recommended Instrument Conditions

9.2.1 Recommended instrument conditions (i.e., RF power, viewing

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8

height, nebulizer flow, argon flow) are very specific to thetype of instrument being utilized. Simultaneous instrumentsoptimize a sensitive mid-wavelength element such as cadmium tooptimize instrument operating conditions before sampleanalysis.

9.2.2 Instrument operating conditions as described in themanufacturer's instrument manual should be applied.

9.3 Initial Calibration

9.3.1 After warm-up period, instrument set-up, and optimization ofinstrument parameters, calibration can be initiated. Acalibration is performed using a calibration blank and atleast one standard that lies in the linear range of theinstrument. A set of verification standards is analyzed asdescribed below.

9.3.1.1 An ICV of a concentration and source differentfrom the calibration standards is analyzed forall desired metals and wavelengths. Results forthe ICV must be within +/- 10X of the expectedvalue. If not, the initial calibration must berepeated for those elements that failed criteria.

9.3.1.2 An ICB is analyzed following the ICV. Theabsolute value of the ICB must be less than orequal to the Contract Required Detection Limit(CRDL). If not, calibration must be repeated forthose elements that failed criteria. The ICBmust be analyzed for all desired metals andwavelengths.

9.3.1.3 A CRI is prepared at a concentration of twice theContract Required Detection Limit for all metalsexcept Ba, Pb, Fe, Ca, Na, Al, and K. Lead isprepared at 2x the IDL. CRI standards must berun at the beginning and end of each run, with aminimum of twice per eight hours. No acceptancecriteria has been established for CRI Recoveries.

9.3.1.4 Interference Check Standard A (ICSA)

9.3.1.4.1 The ICS(A) solution contains theinterfering elements (calcium, magnesium,aluminum, iron) at high concentrations.The ICS(A) is analyzed to determine whetherinter-element corrections are accurate. The

A R 3 I |i»59

Appendix H

A R 3 1 I U 6 0


FIELD AUDIT CHECKLIST

Site Name

Location

Study Date (s): Audit Date:

Phone Number

Contractor/State Personnel

Address

Site Manager

Other Personnel and Affiliation

ASARCO\SAP\APPDXH.KPR4 H-1 A R 3 i me


TABLE 11-1. FIELD AUDIT CHECKLIST (Continued)

Y.N. or NA

PLANNING AND PREPARATION

1) What document(s) is(are) relevant to this audit?

Date(s) Issued:

SAMPLING

General Procedures

1) Do field staff have a copy of the Sampling and AnalysisPlan?

2) Were samples collected starting with the least likelycontaminated and proceeding to the most likelycontaminated?

Remarks

3) Was sampling equipment protected from possiblecontamination prior to sample collection?

If No, explain

Y = YesN = NonconformanceNA = Not Applicable

ASARCO\SAP\APPDXH.KPR4 H-2

A R 3 I I U 6 2



Y.N. or NA

4) If equipment was cleaned in the field, were

proper procedures used?

If No, explain

5) What field instruments were used during this

investigation?

6) Were field instruments properly calibrated?

If No, explain

7) Were calibration procedures documented

in the field notes?

Remarks

8) Were the samples chemically preserved in the field?

If No, explain

(9) Does field sampler have a sample cooler and

proper forms, labels, tape, and ice?

10) Were the samples iced?

ASARCO\SAP\APPDXH.KPR4 H-3 » D O I | (. C O



Y.N. or NA11) Were samples for selected parameters

field filtered?

If yes, list parameters and describe procedures

12) Is the chain-of-custody form completed properly?

13) Were field documentation activities completedin accordance with the QAPP and SOP?

14) Were waste water/cuttings contained and disposedof according to the QAPP and SOP?

Well Sampling N/A

1) Was depth of well determined?

2) Was depth of water determined?

3) Were the above depths to water comparable to waterlevels in the general area?Describe how the depths were determined.

4) How was the volume of water originally present in each well

determined

5) Was the volume determined correctly?

ASARCO\SAP\APPDXH.KPR4 A R 3



Y.N. or NA

6) How was completeness of purging determined?VolumeMeasureTime/Flow Rate

Cond./dissolved oxygen

Clarity

7) Was a sufficient volume purged?

8) Was pump utilized?If no, describe the method of purging (bailer - includetype and construction material, pump - include type)

9) How were the samples collected?Bailer

PumpCombination

Construction material of bailer:

Design of bailerOpen Top

Closed Top

Other

10) If a pump was used, describe how it was cleaned beforeand/or between wells.

ASARCO\SAP\APPDXH.KPR4 * H-5

A R 3 I I U 6 5



11) Were field instruments calibrated and calibration data

recorded prior to use?

12) Were field measurements conducted and documented accordingto manufacturer's recommendations or SOP?

13) Was the sample properly transferred from bailer to sample

bottle (i.e., was the purgeable sample agitated, etc.)?

14) Was the rope or line discarded after use at each well?

Surface Water Sampling

1) What procedures and equipment were used to collectsurface water samples?

Who collected samples?

2) Did the sampler wade in the stream during sample collection?

If yes:

Did the sampler face upstream while collecting sample?

Did the sampler ensure that sediments were not collected

along with the water?



4) Were field measurements conducted and documented according

to manufacturer's recommendations or SOP?

Y.N. or NA

ASARCO\SAP\APPDXH KPR4 H-6 A R 3 I 1 ^ 6 6



Y.N. or NA

5) Note any deficiencies observed during the collection ofthe surface water samples

Waste. Sludge. Soil/Sediment Sampling

1) What procedures including equipment were used to collectsoil/sediment samples

2) Were the soil/sediment samples well mixed prior to placingthe sample in the sample container?

3) Note any deficiencies observed during the collection ofthe soil/sediment samples

Soil Sampling

1) Is soil sampling equipment assembled according tothe Sampling and Analysis Plan?

2) Are samples taken in advance of the lead auger?

3) Are the sample liners properly sealed using a teflon sheet,cap and duct or electrical tape?

4) Is the boring grouted upon completion

5) Is sampling equipment decontaminated?

6) Is the drilling equipment decontaminated?

7) Are cuttings placed in drums?

ASARCO\SAP\APPDXH .KPR4 H-? R R 3 M U 6 7



Y.N. or NA

8) Is a bound notebook used to record all drilling activities?

Comment:

9) Are detailed boring logs kept for each boring?

Other Sampling

1) What other types of samples were collected during this

investigation?

2) What procedures were used for collection of these samples?


QUALITY ASSURANCE/QUALITY CONTROL

(While all of these QA/QC procedures are not necessarily used, please identify

the specific techniques which were employed by sampling personnel.)

1) Did the sampling personnel utilize any field blanks?

ASARCO\SAP\APPDXH KPR4 A R 3 im68



2) Were any equipment rinsates collected?

If Yes, list:

3) Were any duplicate samples collected?

If Yes, list the types (parameter coverage, etc. and

describe their collection.

43) Were any spiked samples utilized?

If Yes, list the types (parameter coverage, etc. and

describe their handling.

FIELD DOCUMENTATION AND CHAIN-OF-CUSTODY

1) Were split samples collected by EPA?

2) Were chain-of-custody records completed for all samples?

3) Were all samples properly sealed at the time of collection?

4) Were samples kept in a secure place after collection?

5) Were all sample labels and chain-of-custody forms signed

by sample collector(s)?

Y.N. or NA

ASARCO\SAP\APPDXH.KPR4 H-9 A R 3 I | l *69



6) Were sampling locations adequately documented?

If No, explain

7) Was sampling documented with photographs?

If Yes, was a photolog maintained?

8) Were the samples shipped to a contract laboratory?

If Yes, were the samples properly packed for shipment?

ASARCO\SAP\APPDXH.KPR4 H-10

Y.N. or NA

A R 3 I I U 7 0


FIELD AUDIT CHECKLIST

Site Name

Location

Study Date (s): Audit Date:

Phone Number

Contractor/State Personnel

Address

Site Manager

Other Personnel and Affiliation

ASARCO\SAP\APPDXH.KPR4 H-I A R 3 l l i * 7 l



Y.N. or NA

PLANNING AND PREPARATION

1) What document(s) is(are) relevant to this audit?

Date(s) Issued:

SAMPLING

General Procedures

1) Do field staff have a copy of the Sampling and AnalysisPlan?

2) Were samples collected starting with the least likelycontaminated and proceeding to the most likelycontaminated?

Remarks

3) Was sampling equipment protected from possiblecontamination prior to sample collection?

If No, explain

Y = YesN = NonconformanceNA = Not Applicable

ASARCO\SAP\APPDXH.KPR4 A R 3 i m 7 2



Y.N. or NA

4) If equipment was cleaned in the field, were

proper procedures used?

If No, explain

5) What field instruments were used during thisinvestigation?

6) Were field instruments properly calibrated?If No, explain

7) Were calibration procedures documentedin the field notes?

Remarks

8) Were the samples chemically preserved in the field?

If No, explain

(9) Does field sampler have a sample cooler andproper forms, labels, tape, and ice?

10) Were the samples iced?

ASARCO\SAP\APPDXH.KPR4 H-3 A R 3 i m ? 3



Y.N. or NA11) Were samples for selected parameters

field filtered?

If yes, list parameters and describe procedures

12) Is the chain-of-custody form completed properly?

13) Were field documentation activities completedin accordance with the QAPP and SOP?

14) Were waste water/cuttings contained and disposedof according to the QAPP and SOP?

Well Sampling N/A

1) Was depth of well determined?

2) Was depth of water determined?

3) Were the above depths to water comparable to water

levels in the general area?Describe how the depths were determined.

4) How was the volume of water originally present in each well

determined

5) Was the volume determined correctly?

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Y.N. or NA

6) How was completeness of purging determined?

Volume

MeasureTime/Flow RateCond./dissolved oxygen

Clarity

7) Was a sufficient volume purged?

8) Was pump utilized?If no, describe the method of purging (bailer - includetype and construction material, pump - include type)

9) How were the samples collected?BailerPumpCombination

Construction material of bailer:

Design of bailerOpen Top

Closed TopOther

10) If a pump was used, describe how it was cleaned before

and/or between wells.

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Y.N. or NA



12) Were field measurements conducted and documented accordingto manufacturer's recommendations or SOP?

13) Was the sample properly transferred from bailer to sample

bottle (i.e., was the purgeable sample agitated, etc.)?

14) Was the rope or line discarded after use at each well?

Surface Water Sampling

1) What procedures and equipment were used to collectsurface water samples?


2) Did the sampler wade in the stream during sample collection?If yes:

Did the sampler face upstream while collecting sample?

Did the sampler ensure that sediments were not collected

along with the water?

3) Were field instruments calibrated and calibration datarecorded prior to use?

4) Were field measurements conducted and documented according

to manufacturer's recommendations or SOP?

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Y.N. or NA

5) Note any deficiencies observed during the collection of

the surface water samples

Waste, Sludge. Soil/Sediment Sampling

1) What procedures including equipment were used to collect

soil/sediment samples

2) Were the soil/sediment samples well mixed prior to placing

the sample in the sample container?

3) Note any deficiencies observed during the collection of

the soil/sediment samples

Soil Sampling

1) Is soil sampling equipment assembled according tothe Sampling and Analysis Plan?

2) Are samples taken in advance of the lead auger?

3) Are the sample liners properly sealed using a teflon sheet,cap and duct or electrical tape?

4) Is the boring grouted upon completion

5) Is sampling equipment decontaminated?

6) Is the drilling equipment decontaminated?

7) Are cuttings placed in drums?

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Y.N. or NA

8) Is a bound notebook used to record all drilling activities?Comment:

9) Are detailed boring logs kept for each boring?

Other Sampling

1) What other types of samples were collected during thisinvestigation?

2) What procedures were used for collection of these samples?


QUALITY ASSURANCE/QUALITY CONTROL

(While all of these QA/QC procedures are not necessarily used, please identifythe specific techniques which were employed by sampling personnel.)

1) Did the sampling personnel utilize any field blanks?

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2) Were any equipment rinsates collected?

If Yes, list:

3) Were any duplicate samples collected?If Yes, list the types (parameter coverage, etc. anddescribe their collection.

43) Were any spiked samples utilized?If Yes, list the types (parameter coverage, etc. and

describe their handling.

FIELD DOCUMENTATION AND CHAIN-OF-CUSTODY

1) Were split samples collected by EPA?

2) Were chain-of-custody records completed for all samples?

3) Were all samples properly sealed at the time of collection?

4) Were samples kept in a secure place after collection?

5) Were all sample labels and chain-of-custody forms signedby sample collector(s)?

Y.N. or NA

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AR3 I m79



6) Were sampling locations adequately documented?If No, explain

7) Was sampling documented with photographs?

If Yes, was a photolog maintained?

8) Were the samples shipped to a contract laboratory?

If Yes, were the samples properly packed for shipment?

ASARCO\SAPVAPPDXH.KPR4

Y.N. or NA

H-10 A R 3 I I U 8 0

sdms docid 2009027 bbi - united states environmental

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