cec project 91 187 · foster ptizi xi • 790 hobdty orlv* • pittsburgh. pennsylvania 15220...

QUALITY ASSURANCE PROJECT PLAN

FOCUSED REMEDIAL INVESTIGATION

OPERABLE UNIT 2AND

OPERABLE UNIT 5* «r

OSBORNE LANDFILL SITEGROVE CITY, PENNSYLVANIA

Prepared for:

COOPER INDUSTRIESHOUSTON, TEXAS

CEC Project 91 187

June 29, 1993

Civil & Environmental Consultants, Inc.Mtl 4665 Cornell Road Suite 255 Pittsburgh 601 Holiday Drive Foster Plaza 3

Cincinnati. Ohio 45241 Pittsburgh, Pennsylvania 1S220Phone (613) 469 - 0200 Phone (412) 921 - 3402Fax (613) 469 - 0216 Fax (412) 921 - 1B15

Section 1.0Revision No. 0Date: 6/29/93

Page

1.0 TABLE OF CONTENTS 12.0 INTRODUCTION 23.0 PROJECT DESCRIPTION 44.0 PROJECT ORGANIZATION AND RESPONSIBILITY 135.0 QUALITY ASSURANCE OBJECTIVES 226.0 SAMPLING PROCEDURES 347.0 SAMPLE CUSTODY 353.0 CALIBRATION PROCEDURES AND FREQUENCY 389.0 ANALYTICAL PROCEDURES 3910.0 DATA REDUCTION, VALIDATION, AND REPORTING 4011.0 QUALITY CONTROL PROCEDURES 4212.0 PERFORMANCE AND SYSTEM AUDITS 4313.0 PREVENTATIVE MAINTENANCE 4414.0 DATA ASSESSMENT PROCEDURES 4615.0 CORRECTIVE ACTION PROCEDURES 4716.0 QUALITY ASSURANCE REPORTS 49

FIGURES

Figure 1 - Site Location 5Figure 2 - Existing Site Conditions 6Figure 3 - Schedule 12Figure 4 - Project Organization 15

TABLES

Table 5-1 - Laboratory QA, Objectives 24Table 5-2 - Sampling Summary 25Table 5-3 - Analytical QA Objective 26Table 5-4 - Detection Limits 31

APPENDICES

Appendix A - Field Investigation PlanAppendix B - CEC Corporate Quality Assurance ManualAppendix C - Chester LabNet's QA/QC ProgramAppendix D - Free-CoTs QA/QC Program

QAPP-OU2 and OU5 -1-

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2.0 INTRODUCTION

The Administrative Order on Consent for Remedial Investigation/FeasibilityStudy (Order) for Operable Units 2 (OU2) and OU5 for the Osborne LandfillSite, filed by the Environmental Protection Agency (EPA) on October 13,1992, requires that Cooper Industries (Cooper) or Its Contractor preparea Quality Assurance Project Plan (QAPP) for the proposed Focused RemedialInvestigation (RI). OU2, as defined by EPA, 1s the sediment in thewetland adjacent to the southwest site boundary. OU5 1s defined by EPA asthe Homewood Aquifer. For the purposes of this RI, OU5 also Includes agroundwater verification study of the Connoquenesslng and BurgoonAquifers, mine void, and residential wells near the site.

This QAPP specifies the minimum procedures that will be used to assure theprecision, accuracy, completeness, and representativeness of Its dataknown and documented. In addition, the QAPP specifies the quality levelsthat data must meet 1n order to be acceptable.

This QAPP for the remedial Investigation of OU2 and OU5 for the Osbornesite presents specific procedures proposed by Civil & EnvironmentalConsultants, Inc. (CEC) to collect quality data. This QAPP addresses:

The QA objectives of the project.

Specific QA and QC (quality control) procedures that will beImplemented to achieve these objectives.

Staff organization and responsibility.•>

The requirements of EPA with regard to QA focuses on the acquisition ofenvironmental data of known and acceptable quality. Other aspects of the


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project, such as engineering analysis and report preparation, will becontrolled by Internal requirements of CEC's Quality Assurance Program.


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3.0 PROJECT DESCRIPTION

3.1 Site Background Information;3.1.1 Site Location and Description; The Osborne Landfill site 1s

located 1n Pine Township, Mercer County, Pennsylvania. TheOsborne site 1s situated Immediately north of Pine StreetExtension, one-half mile east of Grove City. See Figure 1.

The site 1s an abandoned Brookvllle Coal seam strip mine, andhas an area of approximately 15 acres. Disposed materialextends from near Pine Street through the strip mine pit toa 5- to 10-foot high slope of trash and debris adjacent tothe large pond at the north end of the site. The majority ofthe material 1n the pit appears to be dark, coarse foundrysand. Slag, scrap metal, wood, paper, and plastic matter arefound scattered around the entire site. There are threeponds located on site. The large pond (Pond No. 1) has asurface area of about one acre, and was estimated to be about20 feet deep. Pond No. 2 has a surface area of about 8,000square feet, and was estimated to have a depth varying fromabout 2 to 10 feet. Pond No. 3 has a surface area of about500 square feet, and 1s periodically dry. The ponds andother site features are shown on Figure 2.

The land Immediately surrounding the landfill 1s used foragricultural purposes. Effects of the past mining operationsare evident near the site. Adjacent to the top of the stripmine hlghwall on the north 1s a large field owned by Mr.Keith McDougal, present owner of the Osborne site. The areato the east 1s mostly wooded. New homes have recently beenbuilt further north of the site along Enterprise Road. These


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4000REFERENCE: U.S.C.S. 7.5* TOPOGRAPHIC MAP GROVECITY QUADRANGLE PENNSYLVANIA. DATED: 1961.PHOTOREV1SED: 1981. SCALE: 1*=2000f 2000

SCALE IN .FEET

Civil & Environmental Consultants, Inc.Foster Ptizi XI • 790 HoBdty Orlv* • Pittsburgh. Pennsylvania 15220

(4121921-3402 • (800)385-2324 • Fix (412) 921-1115

SITE LOCATIONOSBORNE LAND FILL SITE

OU2 AND OU5 REMEDIAL INVESTIGATIONQUALTTY ASSURANCE PROJECT PLAN

OWN. BY; J.C.CHKD. BY:

APPROVED BY: SCALE:1" 2000'

DATE:8/12/91 91187 FIGURE 1

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homes are about 800 feet from the site and aretopographically upgradlent. Several older rural homes alsoexist to the east. South and east of the landfill are low-lying brush and wetlands on both sides of Pine Street. Alarge pond, estimated to be approximately three to four acresIn size, 1s located at the northern portion of the wetland.

3.1.2 Site History; Strip mining probably began near the site gatealong Pine Street Extension 1n the early 1900's. As theoverburden was removed, It was placed along the westernboundary of the site. Since the Brookvllle Coal seam wasabsent to the south, a larger volume of mine spoil wasremoved and piled successively as the operations moved fromsouth to north. Actual periods of deep mining and stripmining operations could not be determined; however, stripmining activities probably concluded 1n the late 1940's. Thestrip mining resulted 1n the formation of a 1,500-foot longpit through the site. Early topographic maps show anelongated pond 1n the pit between the north and south wallsof the stripped area.

From the 1950's until 1963, Mr. Samuel Mooney operated thesite as a disposal area. The operation continued under theownership of Mr. James Osborne from 1963 until 1978 whenoperations were suspended at the site the PennsylvaniaDepartment of Environmental Resources (DER). Disposalactivities apparently began 1n the southeast section of thesite by dumping Into the pond formed by strip mining. Thedisposal operations were terminated prior to completion offilling of the strip pit, which has resulted 1ri the formationof the large pond at the north end of the site.


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Materials disposed at the site allegedly Included foundrysand, Industrial waste, and municipal refuse. Slag, scrapmetal, wood, paper, and plastic matter can be found scatteredaround the site, along with a significant volume of foundrysand. All disposal activities were apparently conductedwithin the 6-acre area created by the coal strippingoperations. Drums, however, were Initially found throughoutall portions of the 15-acre site.

DER brought the site to the attention of the EPA forInclusion under the "Superfund11 p'rogram, following somepreliminary sampling by DER and the EPA Region III TechnicalAssistance Team. EPA subsequently ranked the site using theMitre Hazard Ranking System, and proposed the site forInclusion on the National Priority List (NPL).

Following listing on the NPL, Cooper entered Into a ConsentOrder with DER and Implemented an Initial Remedial Measure(IRM) to remove surface wastes that could potentially result1n environmental hazards or hinder remedial Investigationactivities. During the summer of 1983, a chain-link securityfence was Installed around the site perimeter, and a drum andsoil removal program was Implemented. Approximately 600drums and 45 cu. yds. of contaminated surface soils wereremoved from the site.

3.2 Focused RI Objective: The objective of the Focused RI for OU2 andOU5 at the Osborne Landfill Site will be the collection ofadditional data and the analysis of the new and existing data to:


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Determine whether the low level of contamination In thewetland has had a significant Impact on the environment ofthe wetland.

Determine whether accumulating in animals inthe wetland.

Establish If site contaminants have Impacted water in theHomewood Aquifer.

Verify that the municipal well system'win not be Impacted bysite contaminants by way of the Connoquenessing and BurgoonAquifers.

Further delineate the extent of vinyl chloride contaminationIn the mine pool east of the site.

•Verify that selected residential wells have not been Impactedby site contaminants.

3.3 Summary of OU2 Activities:

B1oaccunmlat1on Study; Samples of earthworms will be collected fromthe wetland area just north of Pine Street Extension at thesouthwest corner of the site. Background samples of earthworms willalso be collected from a strip mining wetland environment noteffected by the site. The earthworm samples will be analyzed todetermine if Aroclor 1254 Is accumulating 1n animals at the site.


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Bioassav Study; Sediment samples will be collected for the bioassaystudy during the bloaccumulatlon field activities. The chronicbioassay test on fathead minnows and cerlodaphnla will be performedusing sediment pore water collected from the wetland and off-sitepond. Five concentrations and one control will be tested on eachsample. Sediment samples will be collected from two locations inthe off-site pond and two locations in the wetland.

3.4 Summary of OU5 Activities

Geophysical Survey; A geophysical surve/ will be performed toassess the Integrity of the existing monitoring wells prior tosampling any wells 1n the Homewood, Connoquenesslng, or BurgoonAquifers. The down hole surveys will Include natural gamma, gammagamma, and high resolution density. The findings and conclusions ofthe geophysical survey will be submitted to EPA in a memorandum.

UnmaunnH AniH f av« Voy-lf traHnn CfuHv* ^ irt' slSftwll Pl i lit Pt lnunicwuuu Muinicr yen iicauiun JIUUY. 4;JTO?::IIKI|JIIS;::HiO-H;j uuisj:itytyVxt,y s i m

will be performed to obtain additional groundwater data from theHomewood Aquifer. The first sampling event will consist of samplingall nine of the existing Homewood Aquifer wells

while the second event will consist of sampling onlythe four Homewood wells 1n which volatile organic compounds weredetected during the 1989 RI,

Connoouenesslnq and Burgeon Aquifers Verification Study; Three newmonitoring wells will be screened In both the Connoquenesslng andBurgoon Aquifers. The new monitoring wells and three previously

QAPP-OU2 and OU5 -10- ^

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: : Section 3.0Revision No. 0Date: 6/29/93

Installed monitoring wells will be sampled. In addition, all of thewells In the Connoquenesslng and Burgoon aquifers will be measuredto estimate the groundwater flow direction 1n these aquifers.

Mine Pool Investigation: m monitoring wells will bescreened in the mine void. All mine void monitoring wells will besampled to estimate the limit of vinyl chloride contamination.

Residential Well Sampling; The six residential wells sampled duringthe 1989 RI will be resampled. One new residential well will alsobe sampled. Sampling will be performed quarterly for one year.Pine Township personnel will perform the actual sampling. CEC willassist Township personnel during the sampling by providingassistance with proper sampling and custody procedures.

3.5 Schedule; The schedule for proposed RI activities 1s Included onFigure 3.

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4.0 PROJECT ORGANIZATION AND RESPONSIBILITY

4.1 Personnel Assignments; CEC has overall responsibility for theremedial Investigation activities. CEC was selected by Cooper, andlater approved by EPA to perform the required tasks. The followingresponsibilities have been assigned for the project:

Remedial Project Manager (RPM)Frank Vavra (EPA)215-597-0676

U.S. Environmental Protection Agency841 Chestnut BuildingPhiladelphia, Pennsylvania 19107Project Coordinator/Cooper Industries ReviewMichael J. O'Brien (Cooper)713-739-5612

Cooper IndustriesFirst City Tower, Suite 4000P. 0. Box 4446Houston, Texas 77210Project Manager (PM)Kenneth R. Miller (CEC)412-921-3402

Civil & Environmental Consultants, Inc.Foster Plaza XI790 Holiday DrivePittsburgh, Pennsylvania 15220Quality Assurance ManagerJames M. Roberts (CEC)412-921-3402

Review Team Leader (RTL)James P. Nairn (CEC)412-921-3402


Section 4.0Revision No. 0Date: 6/29/93 ^

Corporate QA Manager (QAM)James M. Roberts412-921-3402

Assistant Project Manager (APM)Jeffrey C. Woodcock (CEC)412-921-3402

Field Operations/On-Site Coordinator (OSC)CEC Personnel412-921-3402

Data CompletenessD. Scott Rasmussen (CEC)412-921-3402

A project organization chart 1s presented on Figure 4.

4.2 Personnel Qualifications; The following summarizes thequalifications of the proposed project team:

\JKenneth R. MUler. P.E. (Pro.lect Manager); Mr. Miller has more than14 years experience providing a wide range of environmental, civil,and geotechnlcal engineering services. These Include severalcurrent Investigation, design, and remedial action projects onhazardous waste sites. He directed all public sector hazardouswaste projects for ICF Technology's Pittsburgh, Pennsylvania officefrom the mid- to late-1980's prior to joining CEC. In thiscapacity, Mr. Miller was responsible for directing projects of avalue of more than $5 million annually that primarily Involved theperformance of remedial Investigations, feasibility studies,remedial design, and remedial action Implementation at Superfundsites. Mr. Miller was responsible for the technical review andquality control on all projects, as well as schedule and budgetperformance. This work Included the performance - of up to 15projects simultaneously 1n states ranging from Massachusetts to

QAPP-OU2 and OU5 -14- \J

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Texas. The work directed by Mr. Miller consistently received highevaluation from the sponsoring agencies.

Jeffrey C. Woodcock (Assistant Pro.lect Manager); Mr. Woodcock hasten years of experience managing and Implementing environmental andgeotechnlcal projects. Mr. Woodcock has developed remedial designsfor the remediation of environmental problems and supervised theImplementation of remedial actions. He has also managed numerousunderground storage tank projects. These projects have Includedboth in-place closure and removal of storage tanks. He has managedthe Investigation of contamination resulting from storage tanks,developed soil and groundwater remediation plans and specifications,and Implemented remediation of soil and groundwater. Mr. Woodcockhas also managed environmental site assessments, CERCLAInvestigations, and foundation studies.

James P. Nairn fRTLl: Mr. Nairn has more than 19 years experienceconducting and managing environmental assessments at Industrialfacilities nationwide where organic solvents, coatings, resins,electroplating wastes, primary metals manufacturing wastes, organicand Inorganic adds, PCBs, asbestos, pesticides, coal tar and woodtreating chemicals were manufactured or disposed. Mr. Nairn's areasof experience Include conducting environmental assessments andaudits and developing and Implementing remedial constructionprojects. He has authored several publications dealing withgroundwater and related topics, and has prepared manuals detailingstandard procedures for conducting subsurface Investigations andgroundwater monitoring programs at Industrial/hazardous waste sites.He also has experience in mining geology, mine reclamation, dam

»construction and Inspection, subsurface investigations, grouting andlaboratory soils and materials testing. He also has prepared expert


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testimony 1n cases related to groundwater contamination andremediation. Mr. Nairn 1s currently a member of the EnvironmentalCommittee of the Coal Division of AIME, and has recently beenelected chairperson of the MAGLEV Environmental AdvisorySubcommittee.

James M. Roberts (OAH); Dr. Roberts was the lead quality assuranceofficer at ICF Technology where he monitored the Superfund qualityassurance/quality control objectives and procedures on work plans,Remedial Action Master Plans, Remedial Investigations/FeasibilityStudy projects, and Feasibility Study/Conceptual Design projects.Dr. Roberts has over 15 years experience managing the engineeringdesign and construction Inspection of solid waste disposalfacilities for various Industrial groups. These projects haveIncluded site remediation prior to development, design of accessroads, slurry walls, cutoff walls, storm water collection systems,design of berms, dikes, surface Impoundments, design of cappingsystems, regradlng design, design of Industrial waste treatmentsystems, final grading design, and both operational and post-closuregroundwater monitoring systems. He has served as an expert witnessin both state and federal courts. He has published numeroustechnical papers on unique engineering-related topics and projects.

D. Scott Rasmussen (Data Completeness); Mr. Rasmussen has degrees1n chemistry and environmental chemistry, and has more than tenyears experience 1n conducting and managing environmental assessmentand compliance projects at Industrial, commercial, and residentialproperties in the eastern United States. Mr. Rasmussen's areas ofexpertise Include conducting environmental assessments and facilityaudits, and developing remediation and permit compliance programs.He has prepared spill prevention and control plans for the paper,


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Section 4.0Revision No. 0Date: 6/29/93 ->

plastics, and cement Industries, and managed large-scale siteassessments for highway expansions Involving up to 85 Individualproperties. Mr. Rasmussen also has experience in air emissionsource permit preparation, wetland soils delineation, and strip minerevegetatlon. He has managed hazardous waste remediation projectsInvolving contaminated asbestos removal, Ignltable wastes, and PCBs.He has also prepared expert witness testimony regardingenvironmental concerns with a proposed coal-fired co-generationfacility.

4.3 Subcontractors; CEC anticipates utilizing"three subcontractors toperform the OU2 RI activities and three subcontractors to performthe OU5 RI activities. The proposed OU2 subcontractors are AquaticSystems Corporation, Free-Col Laboratories, Inc., and ChesterLabNet. The proposed OU5 subcontractors are Pennsylvania Drilling —Company, Appalachian Geophysical Surveys, and Chester Labnet. s—'

Aquatic Systems Corporation (ASC) will perform bioaccumulation testson earthworms collected from the wetland and control area. Theearthworms will be analyzed for They will alsocollect sediment for the chronic bioassay testing. ASC, located 1nPittsburgh, Pennsylvania, Is an environmental consulting firm whichprovides specialized aquatic sampling and marine survey services.ASC personnel are experienced in all aspects of benthicmacrolnvertebrate surveys. These Include study design, samplecollection, taxonomic Identification, statistical analysis, dataInterpretation, and report preparation. ASC personnel havecollected biota, water, and sediment samples at 15 NPL sites in thelast 10 years. All of ASC personnel participate 1n an approvedHealth and Safety and Medical Monitoring Program. ASC has the


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equipment required to sample macrolnvertebrates from streams,rivers, and lakes.

ASC's address 1s P. 0. Box 15390, Pittsburgh, Pennsylvania 15237.ASC's telephone number Is 412-367-1000.

Free-Col Laboratories, Inc. will perform a chronic bioassay test onsediment pore water using populations of cerlodaphnla and fatheadminnows. Free-Col 1s an Independent testing facility located 1nMeadvllle, Pennsylvania, specializing in analytical services forenvironmental protection, occupational health, Industrial hygiene,food processing, and process quality control. Free-Col provides awide range of laboratory, field, and consulting services to clients1n Industry, government, and commerce. Free-Col maintains stringentprotocol and quality assurance procedures In support of Usscientific Instrumentation and Internal operating procedures, andalso participates in several national and state certificationprograms. They also have extensive experience In developing fieldand biological monitoring, and have performed hundreds oftoxlclty/bloassay tests, several Toxic Reduction Evaluations (TRE),and field stream studies.

Free-Col's address 1s P. 0. Box 557, Cotton Road, Meadvllle,Pennsylvania 16335. Their telephone number 1s 814-724-6242.

Pennsylvania Drilling Company will perform test drilling andsubsurface sampling. Pennsylvania Drilling 1s a geotechnlcal andenvironmental drilling contractor located In McKees Rocks,Pennsylvania. Pennsylvania Drilling operates over 20 drill rigsmounted on trucks, trailers, skids and tracks, and has drilledthroughout the trl-state area, .Including several projects 1n the


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Grove City area. Pennsylvania Drilling also previously drilled atthe site for EPA. Pennsylvania Drilling has experience drilling andInstalling deep monitoring wells. They have also drilled onhazardous waste sites for CEC. Pennsylvania Drilling's fieldpersonnel are health and safety trained, and medically monitored Inaccordance with OSHA regulations. Pennsylvania Drilling Is a memberof the Diamond Core Drill Manufacturer's Association, the NationalDrilling Contractors Association, and the National GroundwaterAssociation.

Pennsylvania Drilling's address 1s 500 Thompson Avenue, McKeesRocks, Pennsylvania 15136. Pennsylvania Drilling's telephonenumber Is 412-771-2110.

Appalachian Geophysical Surveys will perform downhole surveys toprovide data to appraise the Integrity of wells previously Installed1n the Homewood, Connoquenesslng, and Burgoon Aquifers. AppalachianGeophysical Surveys 1s a geophysical logging and consulting companylocated in Apollo, Pennsylvania. Their professional staff hasextensive experience performing geological and geophysicalInvestigations for hydrology and engineering studies. All of theiroperators are degreed professionals with training both Inmaintenance and repair of the logging equipment, as well as Ingeophysical log Interpretation. Appalachian Geophysical Surveysoperates four fully equipped geophysical logging trucks andextensive support equipment.

Appalachian's address Is 276 Pennsylvania Route 366, Apollo,Pennsylvania 15613. Appalachian's telephone number 1s 412-327-8119.


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Chester LabNet (Chester) will analyze ground water samples obtainedby CEC from the monitoring wells and tissue samples submitted byAquatic Systems. Water samples collected from the residual wellswill also be submitted to Chester. Chester Is a full -serviceenvironmental testing laboratory with facilities in Pennsylvania,Texas, and Oregon. Chester has state-of-the-art Instrumentation andcomprehensive analytical capabilities. Chester's Houston laboratory1s a member of the EPA Contract Laboratory Program and will be usedto perform the low level volatile organic analyses required for thisproject. The laboratory has performed low level VOC analyses fortSuperfund projects 1n the past and Is familiar with the methodproposed In this Work Plan.

Chester's address 1s Cherrlngton Corporate Center, 600 ClubhouseDrive, Coraopolls, Pennsylvania 15108. Chester's telephone number1s 412-269-5708.


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5.0 QUALITY ASSURANCE OBJECTIVES

The overall QA objective Is to develop and Implement procedures for fieldsampling and reporting that will provide data to support remedialInvestigation activities. Specific procedures to be used for sampling,reporting, Internal quality control, audits, preventatlve maintenance andcorrective actions are described In other sections of this QualityAssurance Project Plan. The purpose of this section 1s to define goalsfor the level of QA accuracy, precision, representativeness andcompleteness required during the Investigation. +

The data objectives for the remedial Investigation are as follows:

Determine whether the low level of contamination In the wetland hashad a significant Impact on the environment of the wetland.

Determine whether accumulating in animals In thewetland.

Establish if site contaminants have Impacted water in the HomewoodAquifer.

Verify that the municipal well system will not be Impacted by sitecontaminants by way of the Connoquenesslng and Burgoon Aquifers.

Estimate the extent of vinyl chloride contamination in the mine pooleast of the site.

Verify that selected residential wells have not been Impacted bysite contaminants.


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Analytical methods that will be used to collect data can be one of fivelevels. These levels are summarized on Table 5-1. Level I and Level Vdata will be collected during the remedial Investigation for OU5. Asampling and analysis summary for the design Investigation Is presented onTable 5-2.

5.1 OA/OC Parameters; The quality assurance objective for analyticaldata 1s to collect environmental monitoring data of known andacceptable quality. A summary of the objectives 1s presented onTable 5-3. In order to meet this objective, the following QA/QCparameters will be addressed:

PrecisionAccuracy (selected analyses)Completeness

- Representativeness (qualitative)

Precision: Precision refers to the level of agreement amongrepeated measurements of the same parameter on the same sample. It1s stated in terms of standard deviation, relative percentdifference, range, or relative range. The overall precision of apiece of data 1s a mixture of sampling and analytical factors. Theanalytical precision Is much easier to control and quantify becausethe laboratory 1s a controlled, and therefore measurableenvironment. Sampling precision 1s unique to each site, making 1tmuch harder to control and quantify. The goals for each factor willbe addressed here separately.

Sampling precision will be checked by obtaining one duplicate sampleduring each sampling event for the monitoring wells. Precision will


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TABLE 5-1SUMMARY OF ANALYTICAL LEVELS

LEVEL V Non-standard methods. Analyses which i«y require inethod modification and/or development. Theobjective of non-standard analytical support is to provide data that cannot be obtained throughstandard avenues of analytical support. Analytical support of this type may involve theresearch, development, and documentation of a method, or, more typically, the Modification ofan existing method.

LEVEL IV This level Is characterized by rigorous QA/QC protocols and documentation and providesqualitative and quantitative analytical data. The CLP Routine Analytical Services (RAS)provide for analyses of all types of media for Hazardous Substance List (HSL) organic compoundsand priority pollutant inorganic compounds. Level IV analyses are used for most RI/FSactivities. However, the use of Level IV data may not be required for many RI/FS purposes.Level IV analyses are typically used for confirmation of lower level data, risk assessment,and to obtain highly documented data.

LEVEL HI Laboratory analysis using methods other than the CLP RAS. This level Is used primarily insupport of engineering studies using standard EPA approved procedures. Some procedures maybe equivalent to CLP RAS, without the CLP requirements for documentation. Generally, theanalyses performed using Level III techniques are designed to provide confirmed identificationand quantification of organic and inorganic compounds in water, sediment, and soil samples.Level III also provides data for site characterizations, environmental monitoring, confirmationof field data, and to support engineering studies (e.g., design, modeling, and pilot/benchstudies).

LEVEL II Field analysis. This level is characterized by the use of portable analytical instrumentswhich can be used on-site, or in mobile laboratories stationed near a site (close-supportlabs). Depending upon the types of contaminants, sample matrix, and personnel skills,qualitative and quantitative data can be obtained. Level II analytical support is designedto provide real-time data for ongoing field activities or when Initial data will provide thebasis for seeking laboratory analytical support. Level II analysis can also be utilizedeffectively when a phased approach Is used for field sampling. In a phased sampling effort.the results of the first phase guide the development of subsequent phases, and, thus, real-timedata are important.

LEVEL I Field screening. This level Is characterized by the use of portable instruments which canprovide real-time data to assist in the optimization of sampling point locations and for healthand safety support. Data can be generated regarding the presence or absence of certaincontaminants (especially volatile*) at sampling locations. Tht objective of Level I analysesis to generate data which are generally used in refining sampling plans and determining theextent of contamination at this site. This type of support also provides real time data forhealth and safety purposes. Additional data which can effectively be obtained by Level Ianalyses include pH, conductivity, temperature, salanity, and dissolved oxygen.

REFERENCE: Data Quality Objectives for Remedial Response Activities, EPA/540/S-87/003, March 1987.

TABLE5-1/160

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*J i— ^ r>»o o S -•r- co inX 4J >» ^CMs> > > s> > > i—i > o c 4 - > m m** O -r- 3-ex > £ t-O ^ t- 50C M W O «/> «O O O =J O CO T>fc. - ••- -o T- a CDJ= C C C C S NU CO CO O CO S3 >>

i - * C M CO ^ CO «3- in tO O> t. S- 1- • CO«•—• «-^ ««^ ««*» «-» «-^ «-^ «-^ C O O*O O CM C•*• c s re*j 0) o> m 03 5E

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O) M f 4J 4J Z +J E COo » C P — 4-*<e<eo.cooC T3Cn -^ c— *NW «flr— f— »— fc. r—•r- C C 1* CL> M ^ CJ O O •» O 4- r—&. co t- o % ?— •—. in > > o > oj

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«o "c c §-£-^ o 5 s - * ' t . > > t a > t « cf^ O S O V> C ^C f- ^M o O 9 QJ CU (• O O O«2 -e SE g ce gg ^ o coo: rr OP-I- o>r-^- __ _ * J C S C O C• e c u o w o cr o > o _ _ _x: £ K » S- U O O V) «rt 3E T3 TO v>

*J T31- CU i— -t- 0>C CTli— Or- .r- C 0}i- C^ Er-U. «y» c£»r— Cr— r- « A S 4 - » —»—•. .—.*-. ~.CO O tt) O OJ C rs O> «r- O) i— WO OrHCMCO^-intO

co *J csc o c c«— i. ca o o oj o s— — - — —— — — -- — f _i _i u— _i g> i

M

AR30709i»

TABLE 5-3ANALYTICAL QA OBJECTIVES

>»»x

Precision Accuracy CompletenessActivity/Parameter Method % fa) % (bl % (c}

Low Level VOCs OLC02.0 ±20 90-110 90

TCL VOCs EPA 524.1 ±20 90-110 90

Pentachlorophenol EPA 525 ±20 90-110 90

b1s(2-ethyhexyl)phthalate EPA 525 ±20 90-110 90

Arochlor 1254 EPA 8080 ±10 90-110 90

Bioassay Study EPA 600/4-89/001 NA , NA 90

BloaccumulatlonStudy EPA OB 10/90 NA NA 90

Temperature EPA 170 ±20 90-110 90

Dissolved Oxygen EPA 360 ±20 90-110 90

Hardness/Alkalinity EPA 200/310 ±20 90-110 90

pH EPA 150 ±20 90-110 90

Conductivity EPA 120 ±20 90-110 90

(a) Precision expressed as relative percent difference.(b) Accuracy expressed as percent spike recovery.(c) Completeness expressed as percent useable valid data compared to total

expected data under correct normal conditions.

TABLE5-3/160

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be evaluated by calculating the relative percent difference (RPD) asfollows:

RPD « difference between the two measured values x 100average of the two measured values

The RPD will be calculated for each analytical parameter. Targetprecision values (I.e., RPDs) are Included on Table 5-3. If thesecriteria are not met, a careful examination of the samplingtechniques, sample media, and analytical procedure will be conductedto Identify the cause of the unacceptable RPD and the usability ofthe data.

Laboratory precision will be addressed by the laboratory analysis ofduplicate samples, as specified In Chester's QA manual (Appendix C)and the methods specified 1n Table 5-3. The RPD for each analyticalparameter will be calculated as a measurement of precision, aspresented on Table 5-3.

Accuracy; Accuracy refers to the difference between a measuredvalue for a parameter and the true value for the parameter. It 1san Indicator of the bias 1n the measurement system. Sources oferror measured by this parameter Include the sampling process, fieldcontamination, preservation, handling, sample matrix, samplepreparation, and analytical technique.

The overall accuracy (see Table 5-3) will be assessed by collectingblind field blanks. The accuracy goal for the field blanks will bethat they contain less than the laboratory method detection limit(MDL). If analytes are detected In the blanks above the HDL, the


AR307096


sample data will be compared with the blank data and may be rejectedor qualified, depending on the relative amounts present.

Laboratory accuracy will be evaluated by analyzing spiked samples.The accuracy objectives for these analyses are specified InChester's QA manual and the methods specified In Table 5-3. Ifthese criteria are not met, a careful evaluation of the data will beperformed to determine the source of the error and usability of thedata.

Completeness; Completeness 1s a measure of the amount of usableInformation relative to the number of samples collected. Missingdata may reduce the precision of estimates or Introduce bias, thuslowering the confidence level of the conclusions. Completeness hasbeen historically presented as a percentage of the data that 1sconsidered valid.

The amount and type of data that may be lost due to sampling oranalytical error cannot be predicted or evaluated in advance. TheImportance of any lost or suspect data will be evaluated in terms ofthe sample location, analytical parameter, nature of the problem,decision to be made, and the consequence of an erroneous decision.In general, the QA objective for this project 1s to obtainanalytical results for at least 90 percent of the samples that arecollected.

Representativeness; Representativeness 1s a measure of the degreeto which the measured results accurately reflect the medium beingsampled. It 1s a qualitative parameter which 1s addressed throughthe proper design of the sampling program in terms of sample


AR307097


location, number of samples, and actual material collected as a"sample" of the whole.

Sampling protocols (discussed In Appendix A) have been developed toassure that samples collected are representative of the media.Field handling protocols (e.g., storage, handling in the field, andshipping) have also been designed to protect the representativenessof the collected samples. Field documentation specified in AppendixA will be used to establish that protocols have been followed andthat sample Identification and Integrity have been maintained.

•»

5.2 Performance Evaluation Samples; Performance evaluation (PE) samplesthat have low concentrations of VOCs of concern (vinyl chloride andTCE) will be analyzed, along with the samples analyzed during themonitoring well sampling. One PE sample will be obtained duringeach of the two anticipated rounds of well sampling. See Table 5-2.

5.3 OA Sample Collection; To evaluate the sampling effort, QA sampleswill be analyzed. One round of QA samples will be collected duringthe monitoring well sampling and one round will be obtained duringthe sampling at the beginning of the pump test. The QA samplescollected in the field will Include:

Trio Blank: One trip blank will be Included with the samplesfrom each sampling effort of the monitoring wells. The blankwill consist of high-purity distilled water prepared by thelaboratory and shipped with the sample bottles for theproject. The sample will be analyzed for TCL VOCs.

«Duplicates; One duplicate groundwater sample will becollected during each monitoring well sampling effort and


AR307098


analyzed for the complete range of parameters listed on Table5-2. Additionally, duplicate samples will be obtained fromMonitoring Wells UMU2, UMU3, UMW5, and MWH4 during bothrounds of sampling and analyzed for low level VOCs.

Field Blanks: One field blank will be prepared for VOCanalysis per each sampling effort. The blank will consist oflaboratory-supplied distilled water which has been rinsedacross decontaminated sampling equipment.

5.4 Laboratory Quality Control Procedures: Analytical methods that havebeen selected for the design Investigation have, In general,specified schedules for calibration standard analysis and otherquality assurance activities. Laboratories must submit evidencethat they have met all such method-specific requirements, Includingactual results for those standards and QA samples. Specific QAprocedures are detailed in Chester's QA manual (Appendix C) and theprocedures Identified In the methods listed on Table 5-3.Laboratory analyses for VOC sampling of monitoring wells will beperformed using low level VOC methods and will not Include CLPdeliverable data packages.

5.5 Method Detection Limit: The method detection limits for theproposed analyses are presented on Table 5-4.

5.6 Survey Standards: Surveying will be performed by experienced CECpersonnel. Survey field notes will be recorded in bound fieldnotebooks, and each page will be numbered, dated, and Initialed

QAPP-OU2 and OU5 -30- \J

AR307099

TABLE 5-4i DETECTION LIMITSO

A. VOLATILE ORGANIC COMPOUNDS

Low LevelCompounds CAS Number 524.1 fuo/L) VOCs fug/11

1. Chloromethane 74-87-3 10 12. Bromomethane 74-83-9 10 13. Vinyl Chloride 75-01-4 10 14. Chloroethane 75-00-3 10 15. Methylene Chloride 75-09-2 5 26. Acetone 67-64-1 10 57. Carbon D1sulf1de 75-15-0 5 18. 1,1-Dichloroethene 75-35-4 5 . 19. 1,1-01Chloroethane 75-34-3 5 110. c1s-l,2-D1chloroethene 156-59-4 5 1•11. trans-l,2-D1chloroethene 156-60-5 5 112. Chloroform 67-66-3 5 113. 1,2-Dichloroethane 107-06-2 5 114. 2-Butanone 78-93-3 10 515. Bromochloromethane 74-97-5 5 1

^ 16. 1,1,1-TrlChloroethane 71-55-6 5 117. Carbon Tetrachloride 56-23-5 5 118. BromodlChloromethane 75-27-4 5 119. l,2-D1chloropropane 78-87-5 5 120. c1s-l,3-D1chloropropene 10061-01-5 5 121. Trlchloroethene 79-01-6 5 122. Dlbromochloromethane 124-48-1 5 123. 1,1,2-Trlchloroethane 79-00-5 5 124. Benzene 71-43-2 5 125. trans-l,3-D1chloropro- 10061-902-6 5 1

pene26. Bromoform 75-25-2 5 127. 4-Methyl-2-pentanone 108-10-1 10 528. 2-Hexanone 591-78-6 10 529. Tetrachloroethene 127-18-4 5 130. 1,1,2,2-Tetrachloro- 79-34-5 5 1

ethane31. 1,2-Dlbromomethane 106-93-4 5 "132. Toluene 108-88-3 5 133. Chlorobenzene 108-90-7 5 134. Ethylbenzene 100-41-4 5 . 135. Styrene 100-42-5 5 1

AR307IOO

Table 5-4 (continued)Page 2

36. Xylenes (total) 1330-20-7 5 137. 1,3-01 chlorobenzene 541-73-1 5 138. 1,4-DI chlorobenzene 106-46-7 5 139. 1,2-DI chlorobenzene 95-50-1 5 140. l,2-D1bromo-3-

chloropropane 96-12-8 5 1

B. SEMI -VOLATILE ORGANIC COMPOUNDS

Compounds CAS Number Detection Limit fug/11

1. Pentachlorophenol 87-86-5 0.62. b1s(2-ethyhexyl)

phthalate 117-81-7 f 0.3C. OTHER ANALYSES

Parameter Detection Limit (ug/1)

Aroclor 1254 (Water) 1.0Aroclor 1254 (Tissue) 160.0

TABLE5-4/160

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using Indelible Ink. Wellhead elevations will be determined towithin 0.01 foot.

Upon completion of the survey effort, the data and calculations willbe summarized in tabular form and will be checked by a secondemployee.


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6.0 SAMPLING PROCEDURES

Detailed sampling procedures are provided in the Field Investigation Plan(FIP), Appendix A.

Coordination with Chester and Free-Col will be performed by CEC's projectmanager or assistant project manager.


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7.0 SAMPLE CUSTODY

Sample tags and forms used to document custody are Included in Section 3.2of Appendix A, Field Investigation Plan. Sample bottles and reagents willbe supplied by Chester and Free-Col.

Custody procedures for this project will be based on the proceduresdetailed in "NEIC Policies and Procedures, * EPA-330/9-78-001-R, revisedJune 1985. These procedures divide custody Into three areas: samplecollection, laboratory, and final evidence files. Each' of these 1saddressed 1n this section.

A sample or evidence file 1s under custody if any of the followingconditions are met:

- The sample 1s In possession;The sample 1s, In view, after being in your possession;The sample was In possession and placed in a secure location; orThe sample is in a designated secure area.

7.1 Field Custody Procedures; The procedure outlined below willdocument custody from collection until arrival at the laboratory:

7.1.1 The field sampler has custody of the samples from the timethey are collected until they are transferred to the samplepackager.

7.1.2 All bottles are tagged with sample number and location by thesampler and/or packager. Sample tags are completed for eachsample using waterproof Ink. The sample tag will Indicate


AR307IOI*


the project name, date sampled, preservative added (if any),the parameters to be analyzed, and the sampler.

7.1.3 The sample numbers and locations are listed on the chain-of-custody (COC) form. Specific details for completing thecha1n-of-custody form are given 1n Appendix A. Whentransferring possession of the samples, the Individualsrelinquishing and receiving will sign, date, and note thetime on the COC form. This form documents transfer of samplecustody from the sampler to another person, to the sampleshipper, or to a secure storage are!.

7.1.4 Shipping containers are secured with strapping tape andcustody seals for shipment to the laboratory. The custodyseals are covered with clear plastic tape.

7.1.5 The samples are sent by common carrier, and a copy of thebill of lading Is retained as part of the permanentdocumentation. Commercial carriers are not required to signoff on the custody form.

7.1.6 Whenever samples are split with a source or governmentagency, a separate sample receipt 1s prepared for thosesamples and marked to Indicate with whom the samples arebeing split. The person relinquishing the samples shouldrequest the representative's signature acknowledging samplingreceipt. If the representative is unavailable or refuses,this 1s noted on the form.

7.2 Laboratory Custody Procedures; Laboratory custody procedures areadopted by reference as those required by the Contract Laboratory


AR307I05


Program. All laboratories utilized to analyze samples will berequired to following CLP procedures.

7.3 Evidence File Custody Procedure; The project files, along with allrelevant records, reports, logs, field notebooks, pictures,subcontractor reports and data reviews, will be maintained In asecure, limited access area and under custody of the project managerin a locked file cabinet.


&R307I06


8.0 CALIBRATION PROCEDURES AND FREQUENCY

All Instruments and equipment used during this project will be operated,calibrated, and maintained according to the manufacturers' guidelines andrecommendations. Operation, calibration, and maintenance will beperformed by personnel who have been properly trained In these procedures.A routine schedule and record of Instrument calibration and maintenancewill be maintained throughout the duration of this project.

The specific calibration procedures and calibration frequency for eachanalytical method specified in Section 5 wilt be followed. Theseprocedures are Included in the Chester and Free-Col QA manual (Appendix Cand D) and the specific procedures for the proposed analyses. At aminimum, Instrument calibration will be checked dally and recalibrated Ifthe reading 1s outside established control limits.


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9.0 ANALYTICAL PROCEDURES

The analytical procedures for each analysis planned are presented on Table5-3. Chester will perform chemical analyses on water earthworm samplescollected during the RI. The analytical procedures utilized by Chesterare specified in the laboratory QA manual Included as Appendix C. CLPdata packages will not be prepared for the analytical analyses performed.Free-Col will perform bioassay testing using sediment samples collectedduring the RI. The procedures used by Free-Col are included in the QAManual Included in Appendix D.


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10.0 DATA REDUCTION, VALIDATION, AND REPORTING

10.1 Data Validation; CEC personnel will validate all laboratoryanalytical data generated during the design Investigation.Validation criteria are presented on Table 5-3. CEC valldators willbe advised as to which samples are blanks and duplicates, and thefinal Intended use of the data. Once completed, the validation willbe reviewed by the PM to assure that the allowable uses of qualifieddata and the meaning of the data qualifiers are clearly understood.

Field data will not be put through a formal"validation, but will bechecked by the Field Operations leader for problems.

10.2 Data Reduction; Laboratory data will be reduced in accordance withprocedures specified In the analytical method. Final data reductionwill begin upon completion of the validation process. Data will beevaluated as It compares to project objectives and summarized Intoa usable format for data manipulation. QA samples, Including blanksand duplicates, will be used to evaluate the precision, accuracy,and representativeness in accordance with procedures in Section 5.1.

The raw data collected from project sampling tasks and used inproject reports will be Identified and Included in a separateappendix within the final report. Where test data have beenreduced, the method of reduction will be described.

Calculations will be checked and documents will be proofed Inaccordance with procedures Included in CEC's Corporate QA ManualIncluded in Appendix B.


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10.3 Report Preparation; During report preparation, data reduction andmanipulation will occur. All calculations and other forms of datareduction will be checked by the Project Manager, or his designee,and the CEC review team. In addition, each report will be reviewedby the CEC review team for accuracy and consistency. Completesample results on laboratory data sheets will be appended to thereport with data summaries Included in the body of the report. TheQVQC analytical data will be Included In an appendix withdiscussion of the significance of the QVQC results included In thebody of the report.


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11.0 QUALITY CONTROL PROCEDURES

11.1 Laboratory: Internal quality control procedures for chemicallaboratory analyses will follow guidelines specified in the methodspresented on Table 5-3. Quality control requirements are specifiedfor Instrument tune and performance, Instrument calibration, blanks,surrogate recoveries, matrix spikes/ duplicates, plus other qualitycontrol parameters. In addition, PE samples will be performed forlow level volatile organic analysis of monitoring well samples.Field blanks will be collected to check for sample contaminationresulting from the field activities, while field duplicates will becollected to check data precision.

11.2 Field Analyses: Field analyses are performed on site, and do notInvolve samples that are collected and retained. All field analysesand measurements will be recorded in permanently bound fieldlogbooks, dated, and signed with Indelible Ink by field personnel.The primary QVQC objective 1s to obtain reproducible measurementsto a degree of accuracy consistent with limits Imposed by analyticalmethodologies used and the Intended use of the data. Qualitycontrol procedures will be limited to checking the reproducibilityof measurements by taking multiple readings and by calibration ofInstruments (where appropriate).


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12.0 PERFORMANCE AND SYSTEM AUDITS

CEC's Quality Assurance Manager (QAM), James M. Roberts, 1s responsible tomonitor and audit performance of QA procedures to assure that projects areperformed in accordance with approved quality assurance procedures, theQAM conducts these audits as described In Section 6.0, Audit Program, ofthe CEC Quality Assurance Manual (Appendix B). An audit will be scheduledduring field activities to evaluate the execution of sampleIdentification, sample control, chaln-of-custody procedures, fieldnotebooks and sampling procedures.


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13.0 PREVENTATIVE MAINTENANCE

13.1 Field Analysis; Several types of field Instrumentation will be usedduring the Osborne design Investigation, Including:

HNu or Organic Vapor AnalyzerLEL/02 MeterWater analyzer (combined pH, temperature, conductivity meterWater level data logger

Specific operating Instruments for the field equipment are given inAppendix A. The following preventative maintenance generalguidelines should be followed. Refer to the Instruction manual foreach piece of equipment if more details are needed.

Be certain each Instrument 1s working properly before goingto the field. Perform a dally calibration to be sure itfalls within the correct range. Calibration will beperformed at the beginning, at mid-day break, and at the endof each work day, and calibration data will be recorded inIndelible ink 1n field logbooks.

Make sure the proper electrical power is available in thefield.

When not in use, store the pH electrode in pH 4 boot, not indistilled water.

If the pH electrode becomes coated with oil or otherorganics, rinse It with acetone or methanol, then water.


AR307I13


Know what you are doing before you operate anyInstrumentation. Get Instruction or help if you are unsure.

Do not push the OVA or HNu probe Into the ground.

Charge all battery operated Instruments dally.

Take extra electrical line for the submersible pump and extraextension cords.

13.2 Field Equipment Repair and Replacement; Spare expendable componentsof field equipment (electrodes, batteries, etc.) will be kept on-slte for simple repairs. If equipment cannot be repaired within theday on which failure occurs, replacement equipment will be obtainedfrom CEC's main office for use the next working day. All fieldrepairs will be documented in the field logbooks listing Instrumenttype, model, serial number, and person performing the repair.

13.3 Laboratory Analysis; Maintenance procedures and schedules .for allanalytical Instruments will be in strict accordance with therecommendations of the equipment manufacturers. Routine maintenancewill be performed by laboratory personnel as needed. SpecializedInspection and maintenance of major equipment Items will beperformed by trained service personnel from the manufacturer inaccordance with Instrument service contracts. All records ofInspection and maintenance will be dated and documented inlaboratory record books.


AR307I\k


14.0 DATA ASSESSMENT PROCEDURES

Following validation, the designee of CEC's PM will assess the data todetermine precision, accuracy, representativeness and completeness. Theactual sampling techniques used by the field crew will be reviewed by thePM for deviations from the written sampling procedures. If deviations arefound, their Impact on the representativeness of data will be assessed.

Lost or suspect data will be evaluated In terms of sample location,analytical data lost (fraction, Individual parameter, etc.), decision tobe made with the data, and risk associated with'an-erroneous decision.Critical locations or critical analytical data will be examined todetermine their accuracy and Impact on the overall objectives of theproject. Significant data quality problems will be addressed 1n the QAsection of the preliminary design submittal.


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15.0 CORRECTIVE ACTION PROCEDURES

15.1 Laboratory Analyses: If the quality control audit results 1ndetection of unacceptable conditions or data, the PM will beresponsible for developing and Initiating corrective action. Thecorrective actions will be Implemented only after approval by Cooperand EPA. Corrective action may Include:

Reanalyzing the samples, if holding time criteria permit;

Resampling and analyzing;

Evaluating and amending sampling and analytical procedures;or

- Accepting data, acknowledging level of uncertainty.

15.2 Field Analyses; Variability among multiple readings or descriptionswill be assessed on-site, and, if judged excessive by any sitepersonnel and/or the Field Operatlons/Onslte Coordinator,Instruments or equipment will be recalibrated (if appropriate) andthe measurement repeated. If the variable Item Is a description ofmaterials encountered, the description will be cross checked againstbackground or reference materials and with the FieldOperatlons/Onslte Coordinator. If variability remains unacceptablyhigh or Instruments fall to be properly calibrated, the ProjectManager will be notified to Initiate corrective action.

15.3 Response to Corrective Actions; Corrective actions taken 1nresponse to audits will be reviewed with laboratory and fieldpersonnel to ensure that the same problems will not be repeated.


RR307II6


Both laboratory and field personnel will be required to Identifyprocedures that will be used to avoid repeating errors or conditionsthat resulted in the problems.


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16.0 QUALITY ASSURANCE REPORTS

No separate QA report for this project Is anticipated. The preliminarydesign report will contain a separate QA section that summarizes dataquality Information collected and evaluated during the project. Thissection of the report may Include, but 1s not limited to, the following:

QA management (any changes)Status of completion of the QA project planSignificant quality problems and status of corrective actionsResults of QA performance auditsResults of QA systems auditsAssessment of data quality in terms of precision, accuracy,completeness and representativenessQuality assurance related training

Any modifications to this Plan based on the results of audits or QAproblems Identified will also be noted In the final report.

OAPP-OU25/16D


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APPENDIX A

FIELD INVESTIGATION PLAN

AR307I19

TABLE OF CONTENTSO

Page

1.0 Summary of Field Activities 12.0 Data Acquisition Procedures 2

2.1 Rock Borings 22.2 Well Installation 72.3 Water-Level Measurement 13

3.0 Sample Collection Procedures 173.1 Sample Quantity, Preservative, and

Bottle Requirements 173.2 Sample Packing and Shipping 213.3 Groundwater Sampling 263.4 Filtration , 343.5 Bioassay Sediment Sample Collection 363.6 Bloaccumulatlon Earthworm Sample Collection 39

4.0 Equipment Use Procedures 434.1 HNU Photoionization Detector 434.2 Water Analyzer 474.3 LEL/02 Meter 52

FIGURES

Figure 1 - Boring Log 5Figure 2 - Monitoring Well and Sample Location Plan 8Figure 3 - Well Completion Log 11Figure 4 - Preservation Summary 18Figure 5 - Chain of Custody 23Figure 6 - Casing Inside Diameter Sheet 32Figure 7 - Groundwater Monitoring Data Sheet 33Figure 8 - Reference Site Location Plan 40

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1.0 SUMMARY OF FIELD ACTIVITIES

Several data needs must be filled to determine if remedial action 1s necessaryfor OU2 and OU5. The tasks that will be performed Include:1. A bioassay and bloaccumulation study to determine whether the low level of

contamination In the wetland has a significant impact on the environmentof the wetland.

2. Installation of additional monitoring wells to verify the municipal wellsystem will not be impacted by site contaminants by way of theConnoquenesslng and Burgoon Aquifers.

3. Installation of additional monitoring wells to further delineate theextent of vinyl chloride contamination in the mine pool.

4. Sampling selected residential wells to verify they have not been impactedby site contaminants.

The activities that will be performed for each of the operable units aredescribed in the following Items.OU2 Field Activities: Bloaccumulation and bioassay studies will be performed forOU2. .Samples of earthworms will be collected from the wetland area of concernand a area. The samples will be analyzed to determine if contaminantsare acl:uluTaTfng in the tissues of earthworms. Sediment samples will becollected from the wetland and off-site pond for the bioassay study. The chronicbioassay tests will be performed on fathead minnows and ceriodaphnia usingsediment pore water.OU5 Field Activities: A geophysical survey will be performed prior to samplingto assess the integrity of the existing monitoring wells in the Homewood,Connoquenesslng, and Burgoon Aquifers. The findings and conclusions of thegeophysical survey will be submitted to EPA in a memorandum, along withrecommendations for use or abandonment of the wells.

:Si.$&:5S&xM:;&!§MS;S;^separate sampling events will be performed to obtain additional groundwaterfrom the Homewood Aquifer. The first sampling event will consist of sampling allnine of the existing Homewood Aquifer while thesecond event will consist of sampling only the four Homewood wells in whichvolatile organic contamination was detected during the 1989 RI.Three new monitoring wells will be screened In both the Connoquenesslng andBurgoon Aquifers and iff new wells will be screened in the mine void. The newand previously installed* monitoring wells will be sampled. In addition, waterlevels in the Connoquenesslng and Burgoon Aquifers will be measured to estimatethe groundwater flow direction.The six residential wells sampled during the 1989 RI. ^ _ _ » _. _ _' • * • • M • V.V.VAVJ«ViV.VrA-i VA%%VV.WAV*WWrtVp % *l/ V ^ ii»W%W««'will also be sampled. Sampling will be performed quarterly for one year.

FIP-OU2 & OU5 -1- 6/29/93

AR307I2I

2.0 DATA ACQUISITION PROCEDURES

^ 2.1 ROCK BORINGS

I. APPLICATION

This procedure Is applicable to the drilling of borings in competent rock.II. PROJECT-SPECIFIC REQUIREMENTS

A. NUMBERING SYSTEM

Borings will be numbered in accordance with Section 2.2, "WellInstallation."

B. BORING LOCATIONS, DEPTHS, AND DRILLING METHODS

Boring locations will be as specified in Section 2.2.Six deep monitoring wells, and three shallowmonitoring wells will be installed in the rock borings. The threewells to the mine void, and the threewells to the Connoquenessing Aquifer will be drilled using rotarymethods without sampling. The three deep wells to the BurgoonAquifer will be cored.No soil sampling will be performed.

C. COMPLETION OF BORING

Borings will be completed as monitoring wells, in accordance withSection 2.2.

D. DECONTAMINATION

Decontamination of drilling rigs and equipment will take place onlyIf wastes or volatile organic contamination, as Identified byorganic vapor readings above background, are encountered duringdrilling activities. If wastes or other contamination are notencountered, the drilling rigs and equipment will be decontaminatedat the completion of all drilling activities. Equipment will bedecontaminated on-slte with decontamination fluids allowed to drainonto the site surface.If wastes or contamination are encountered in borings, the drillingrig and equipment will be decontaminated on-slte prior to beginningthe next boring. Decontamination fluids will be collected anddischarged Into one of the on-site ponds.

FIP-OU2 & OU5 -2- 6/29/93

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III. PROCEDURE

A. Prior to any drilling activities, have all burled utilities andtanks located. Also note the location of overhead wires. Theextended derrick must be greater than 20 feet from any high-powerlines. It may be necessary to relocate a boring to avoid utilities,tanks, or overhead wires.

B. Setup and level the drill rig over the boring location.C. Monitor the borehole and the breathing zone over the borehole with

the organic-vapor detector.D. Advance the boring to auger refusal.E. Withdraw the augers and Install a temporary casing to maintain the

borehole. If hollow-stem augers of sufficient diameter have beenused to advance the soil boring, these may act as a temporarycasing.

tF. Advance the borings using coring or rotary methods. When coring is

performed, five or ten foot runs are acceptable. Core runs will benumbered sequentially for each boring (Example: MW-7, Run 1, 25-35feet). Each core box will be marked with the Boring I.D., RunNumber(s), and cored Interval (Example: MW-7, Runs 1-2, 25-40 feet).Core boxes will be wrapped in plastic tarpaulins and stored on-site.If EPA approves as an alternative, rock core will be transported toCooper's facility 1n Grove City for storage.Following completion of coring, ream the boring to 8 inches indiameter using rotary methods.For the borings where coring will not be performed, advance theborings to the required depth using rotary methods.

G. Record the boring log in a field notebook and transfer to a BoringLog Form, or record directly on the form.1. Field notes are to include, as a minimum:

Boring NumberSoil DepthMaterial Description (as discussed below)Weather ConditionsOrganic-Vapor ReadingsEvidence of Contamination (visual observance or odor)Water Conditions (including measured water levels)Daily Drilling Footage and Quantities (for billingpurposes)Notations on Man-Placed MaterialsDrilling Method and Borehole DiameterAny Deviations for Established PlansRun NumberRun Length

FIP-OU2 & OU5 -3- 6/29/93

AR307I23

RecoveryRQDRock Type, ColorDescription of ContactsInternal Structures or FossilsFracture Spacing in Qualitative Terms, Orientation ofFractures, Description of Fracture Fillings orSlickensidesWater Gain or Loss During Drilling

2. For rotary borings, a log should be prepared from chips, andshould Include:

Rock type and colorApproximate depth of contacts.

Test any potentially calcareous materials for calclte withhydrochloric acid.

H. The run number and depth Interval labels wifl be placed in the coreboxes adjacent to the corresponding rock core. Filled and labeledcore boxes will be photographed.

I. Complete the boring as specified in Section 2.2.IV. DOCUMENTATION

A. DOCUMENTS TO BE PREPARED

Complete a Boring Log (Figure 1) for each boring.B. DISPOSITION OF DOCUMENTS

Completed logs should be placed in the Originals file, with copiesto the Project file and project manager.

V. PRECAUTIONS AND COMMON PROBLEMS

A. Identification of the water table can be difficult in low-permeability materials. Rock may appear to be dry for a greatdistance below the water table. Testing the "feel" of cuttingsduring air-rotary drilling can be helpful in assessing if thegroundwater level has been encountered when drilling through lowpermeability formations.

B. The outside of a rock core is often a very poor indicator of theactual rock type. It is necessary to break the core (aftermeasuring RQD) to get an accurate rock description.

VI. EQUIPMENT AND SUPPLIES

- Drilling rig- Carpenters rule

FIP-OU2 & OU5 -4- 6/29/93AR307I21*

CIVIL & ENVIRONMENTAL CONSULTANTS, INC.'roject__________________________ Project No..levation

late

1 1

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Field Engiriser

DESCRIPTION

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WOBUJU. .CUSSIHCATI01

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REMARKS*

*Pocket Penetrometer Readings Project No. ___ -Boring No. \ J

FIGURE 1AR307I25

Rock hammerAdd bottleCamera and FilmHNu

VII. REFERENCES

None

FIP-OU2 & OU5 -6- 6/29/93

AR307I26

2.2 WELL INSTALLATION

I. APPLICATION

This procedure is applicable to the installation of monitoring wells inunconsolidated material or bedrock.

II. PROJECT-SPECIFIC REQUIREMENTS

A. NUMBERING SYSTEM

The following well numbers will be used:Monitoring Wells Installed to Mine Void:

MWV7MWV8

Monitoring Wells Installed to Connoquenesslng Aquifer:CW1CW2CW3

Monitoring Wells Installed to Burgoon Aquifer:BW1BW2BW3

B. WELL LOCATIONS AND DEPTHS

Monitoring well locations are shown on Figure 2. The monitoringwells Installed to the mine void are estimated to be about 50 feetdeej__________________ _~l orf g~ ^

estimated to be about 150 feet deep,while the monitoring wells Installed to the Burgoon Aquifer areestimated to be about 275 feet deep.

C. CONSTRUCTION MATERIALS

Well Material: Schedule 40 PVC, threaded, flush joint.Well Diameter: 4 inches

FIP-OU2 & OU5 -7- 6/29/93

AR307I27

EPA REGION IIISUPERFUND DOCUMENT MANAGEMENT SYSTEM

DOCJDPAGE #

IMAGERY COVER SHEETUNSCANNABLE ITEM

SITE NAME__

OPERABLE UNIT

ADMINISTRATIVE RECORDS- SECTION_UL_VOLUME

REPORT OR DOCUMENT TITLE

P \ 0,1 rcyrJ- yier)DATE OP DOCUMENT £)P- (

DESCRIPTON OF IMAGERY ___ 3

NUMBER AND TYPE OF IMAGERY

L^. I .XN /^ 1 / \ / \ £\ 1 J 1 - Jl «^ X%

,n-^3

yimiJcn™ \,e//

ITEM(S) 1 Ovfrtsi^ea fn$p

Screen Length: 5 feet of prepacked screen In mine void. All otherwells receive 10 feet of screen.Screen Slot Size: 0.010 Inches (#10 slot)Filter-Pack Material: Coarse-grained sandBackfill: Cement grout with 3-5% bentonite addedProtective Casings: Above grade, with lock

D. OTHER CONSIDERATIONS

Mine void monitoring wells are to have minimum 6-foot high welllocation markers.

III. PROCEDUREA. Drill the boring in accordance with Section 2.1, "Rock Borings."fB. Develop the boring to remove cuttings and sediment prior to placing

well materials. Use pumping or bailing methods to develop theboring.

C. Assemble the appropriate well materials and lower them into theborehole. Place a cap over the top of the well to prevent material

. from falling Into it.D. Place the appropriate filter-pack material around the screen (except

prepacked mine void wells) to the desired level, at least two feetabove the top of the screen. Pour the material slowly, and monitorwith a weighted tape measure to check the level and determinewhether the pack has bridged. For wells greater than 150 feet deep,a tremie pipe will be used to place the filter pack. The filterpack materials will then be tamped into place to prevent bridging.The thickness of this seal will be approximately 10 feet.

E. Install a seal over the pack by dropping bentonite pellets in thesame manner. In the mine void wells, install a packer in competentbedrock above the mine void prior to placing bentonite. A minimumtwo-foot thickness of bentonite is required. IF THE BENTONITE ISABOVE THE WATER LEVEL, ADD SEVERAL GALLONS OF POTABLE WATER TOHYDRATE THE PELLETS. Walt for five to ten minutes to allow thepellets to swell.

F. Mix the grout as specified in Section II.C. Lower a hose or tremiepipe to the bottom of the annul us. Pump grout to fill the boreholeto the ground surface, while withdrawing the pipe/hose..

G. Allow the grout to set overnight, then install the appropriateprotective casing. Secure with neat cement or concrete asnecessary.

FIP-OU2 & OU5 -9- 6/29/93

AR307I29

H. Develop the well by pumping and/or balling until turbidity isadequately reduced. Adequate reduction in turbidity will be made ^Jbased on the judgment of the Field Operations/On-Site Coordinator.If this method 1s not successful, surging with a surge tool may behelpful. For pumping wells, additional techniques may be required.Development water for the mine void wells will be collected anddischarged into an on-s1te pond. Development water for all othermonitoring wells will be discharged to the ground surface.

NOTE: If hollow-stem augers or temporary casing have been Installed,these should be Incrementally withdrawn as pack and backfill materials areemplaced.

IV. DECONTAMINATION

Unless otherwise specified in Section II, no specific decontamination isrequired for this operation.

V. DOCUMENTATION' fA. DOCUMENTS

Complete a Well-Completion Log (Figure 3) for each well Installed.Information to be presented on the form includes:1. Self explanatory2. Well number in accordance with Section II.A. above. ,3. Self explanatory -/4. Your Initials5. Date of completion of Installation6. Borehole diameter7. Well diameter3. Distance from the top of inner casing to water surface9. Self explanatory10. Material and diameter of outer casing, Indication whether lock

and inner cap were added11. Material used for surface seal, usually neat cement or

concrete12. Riser material, Including wall thickness (schedule)13. Material used to fill annular space, usually grout, bentonite,

or cement-bentonlte slurry14. Material used for lower seal, usually bentonite pellets15. Grain-size and specification of material used for filter

medium, such as pea gravel, Ottawa sand, etc.16. Screen slot size, in Inches. 110 screen has a slot size of

0.010 Inches, 120 has size of 0.020 Inches, etc.17. Circle If the screen is wound (continuous slot) or is machine

slotted. Note If some other screen type (such as hand-slottedor drilled) Is used.

18. Material of construction for the well screen19. Describe how any overdrilled borehole was filled and sealed,

or whether caving occurred before well Installation.FIP-OU2 i OU5 -10- 6/29/93

AR307I30

WELL -COMPLETION LOG iKiSKIPROJECT NAME: WELL NO.*PROJECT NO.' GEOLOGIST/ENGINEER' DATE INSTALLED' / /

AP AND CASING'.

SURFACE SEAL'

MEASURED WATER LEVEL-._______L FROM TOP OF

DATE MEASURED' / * '>

GROUND SURFACE DEVELOPMENT METHOD,

COMMENTS/RESULTS'

NSTALLATION PROBLEMS/COMMENTS •_________

NOTES'.

WELLSLOT SIZE'.SLOT TYPE* CONTINUOUS SLOTTED OTHER'.MATERIAL'______________________

aBANDONED BOREHOLEACKFILL'_________

\ j

L" ""-•""- Civil & Environmental Consultants. Inc.Pittsburgh, Pennsylvania

ftR307!3l FI6URE3

20. Method of purging, surging, or other well development21. Results of well development, such as turbidity of discharge .>

after development, or poor development due to poor yield.Also include pumping rate(s) if a submersible pump is used todevelop the well.

22. Any problems during well Installation, such as floating wellmaterials, difficulty in emplacing pack or backfill, caving,etc.

23. Any other observations24. Depth of feature from ground surface25. Surveyed and calculated elevationsThis information may be recorded in a field log book for latertransfer to the boring log.

B. DISPOSITION OF DOCUMENTS

Completed logs should be placed In the Originals file, with copiesto the project file and the project manager.#

VI. PRECAUTIONS AND COMMON PROBLEMS

A. If the boring is not adequately cleaned, the filter pack will notsettle appropriately, and the screen will be badly clogged with mud.This can be a particular problem with air rotary. This situation 1sbest remedied while the drill tools are still in the boring.Repeatedly allow water to collect In the boring, then flush it outwith clean drilling fluid. W

B. If the well materials float during Installation, remove them andclean the boring as indicated above.

C. Monitor grout takes when working in highly fractured material orfill. Grout can migrate around the seal and enter the screen.

D. Measure the pH if you think there may be a problem with groutmigration. Grout 1s very alkaline.

E. Note on the well log any unusual conditions during wellInstallation. These may later help to explain problems with wellfunction or water quality.

VII. EQUIPMENT AND SUPPLIES

A. Weighted tape measureB. Bailers and/or pump, with appropriate hoses, lines, etc.C. pH meter or paperD. Field log bookE. Blank boring logsWell materials and supplies are generally furnished by the drillingsubcontractor. •

VIII. REFERENCES ^

NoneFIP-OU2 i OU5 -12- AR3U / I 0£ 6/29/93

2.3 WATER-LEVEL MEASUREMENT

I. APPLICATION

This procedure is applicable to measurement of water levels in wells.II. PROJECT-SPECIFIC REQUIREMENTS

A. WELL SCHEDULE

Water level measurements will be obtained from the following wellsduring all sampling events:

Homewood Aquifer Monitoring Wells:HWH1 UMW1 UMW5MWH2 UMW2MWH3 UMW3MWH4 UMW4

Connoquenesslng Aquifer Monitoring Wells:MWU1 CW1MWU2 CW2

. MWU3 CW3MMW1

Burgoon Aquifer Monitoring Wells:MWB1 DMW3MWB2 BW1DMW1 BW2DMW2 BW3

B. PREFERRED METHOD

Chalked tape or sounding should be used. Alternative method isInterface probe.

C. DECONTAMINATION

Standard, as discussed below.D. OTHER REQUIREMENTS

NoneFIP-OU2 & OU5 -13- 6/29/93

AR307I33

III. PROCEDURE

A. CHALKED-TAPE METHOD

1. Rub the first five feet of a steel surveyor's chain orfiberglass tape with carpenter's chalk.

2. Lower the tape into the well until the end of the tape entersthe water.

3. Record the tape footing at the wellhead to ±0.01 feet.4. Pull the tape out of the well and read the tape footage of the

water mark to ±0.01 feet. The difference between the readings1s the water level. Do not correct the measurement for thedistance between the wellhead and the ground surface.

B. SOUNDING METHOD

1. Attach a small flat or hoilow-bottom-weight or sounder to theend of a tape measure.

2. Lower the sounder Into the well and listen for the sound ofthe weight hitting the water surface.

3. When this Is heard, pull the sounder back a few inches andredrop it by 1/4 Inch increments until the sound is heard ~~ ,again. \*s

4. Subsequent smaller Increments of lowering the sounder willallow water level measurement to within 0.05 feet.

5. Measure the length from the zero mark on the tape measure tothe bottom of the weight. Add this value to all fieldmeasurements made with the sounder. Do not correct fieldmeasurements for the distance between the top of casing andthe ground surface.

C. INTERFACE PROBE METHOD

Push On/Off Button to Turn On1. Lower probe Into petroleum product. Horn will sound steadily

when gap is fully Immersed in oil product. Slowly raise probeup until sound stops, lower until sound is just heard again,to refine ullage level. Yellow light will be on in oil, offin air.

2. Read the tape marking and note as the surface Uquid ullagelevel.

3. Slowly lower probe through the product, searing for the oil-water interface. When probe reaches xater level, it will /

FIP-OU2 & OU5 -14- 6/29/93 ^

AR307I31*

begin to beep. Joggle probe up, then down to refine waterentry point. Red Interface light will flash. Read tape bysubtracting this reading from full tank depth. Water levelcan be determined. Total tank product height Is thedifference between surface level and Interface level.

. 4. Minimum water depth which can be gauged 1s 3/8 Inch (9.5 mm).5. Temperature of heavy oil may not exceed 110°.Auto Shutoff Feature: After approximately 5 minutes of power on,the unit will auto-shut off. A chirping sound will be heard,warning Impending shut off. Press power on/renew button to continueoperation. During 5 minute Interval, a short "alive" beep Is heard.

IV. DECONTAMINATION

No decontamination 1s required if water levels are measured before wellsare purged or if the site 1s not contaminated. See Project-SpecificRequirements. If obvious contaminants adhere to the tape, Immerse thesoiled portion of the tape in a bucket of clean water and wipe with apaper towel .

IV. DOCUMENTATION

A. DOCUMENTS

Record water levels in a field notebook or Field Data Sheet.B. DISPOSITION OF DOCUMENTS

Dated and Initialed copies of the field data should be given to theproject manager and placed in the project file, or the data shouldbe Incorporated into a trip report to the project manager and file.


A. Measurement of water levels In pumping wells or cascading wells orboreholes can be difficult. Installing a narrow PVC access tubeInside the well casing can make obtaining accurate readings easier.

B. Sounding can be difficult in noisy areas or with deep wells.VI. EQUIPMENT AND SUPPLIES

A. CHALKED-TAPE

Steel or fiberglass tape measure (steel preferred)Carpenters chalkPaper towels

FIP-OU2 t OU5 -15- 6/29/93

AR307I35

B. SOUNDING

Steel or fiberglass tape measureSteel sounding device

C. INTERFACE PROBE

Interface probeV. REFERENCES

None

FIP-OU2 i OU5 -16- 6/29/93

AR307I36

3.0 SAMPLE COLLECTION

3.1 SAMPLE QUANTITY, PRESERVATIVE, AND BOTTLE REQUIREMENTS

I. APPLICATION

This procedure is applicable to samples collected for the analyses listedin Figure 4.


Samples will be numbered In accordance with Section 3.3, "GroundwaterSampling," Section 3.5, "Bioassay Sediment Sample Collection," and Section3.6, "Bloaccumulation Earthworm Sample Collection."

III. PROCEDURES

Sample quantity, preservative, and bottle requirements are presented inthe table following this section. Samples must be kept cool with ice fromthe time of collection. Preservatives will *be added as necessaryImmediately upon collection. Preservatives should be added to watersamples after filtration.

IV. EQUIPMENT

5-gallon buckets with 1 Ids and sample bagsCoolers or refrigerator

- IcePlastic bagsPostal tape

V. PRECAUTIONS

N/A

VI. REFERENCES

40 CFR 136, Guidelines Establishing Test Procedures for the Analysisof Pollutants Under the Clean Water Act, USEPA, July 1985.Methods for Chemical Analysis of Water and Wastes, EPA 600/4-79-020,July 1985.Test Methods for Evaluating Solid Waste, Physical/Chemical Methods(3rd ed.), SW-846.

FIP-OU2 i OU5 -17- 6/29/93

AR307/37

SAMPLE BOTTLES, QUANTITIES, PRESERVATIVES, AND HOLDING TIMES

PRESERVATION SUMMARY FOR WATER SAMPLES

2. Reconaended 4 Mount ofParameter Container Preservative "* Holding Time SaapU

BACTERIOLOGICAL

Colifora, Fecal and Total P.8 Cool, 4°C & hours 2500.008X

PVmCAL PROPERTIES

Acidity P.8 Cool. 4°C U days 250 a*Alkalinity P.O Cool, 4°C U days 250 BlBlocheaical Oxygen Deaand P.fl Cool, 48C 48 hours 1 |Carbonaceous P,8 Cool, 4°C 48 hours t I

Bromide P,S Hont Required 28 days 250 rtCarbon. Total Organic 6 only Cool, 4 C 28 days 2 x 40 ml

HjS04 ta pH <2 *Cheaical Oxygen Demand P,6 Cool, 4°C 28 days 250 it

HjSO, to pH <2Cltioridt P,0 Nona Required 28 days 250 alChlorine, Residual P.6 Nona Required Analyze Innediately 100 a*Color P,6 Cool, 4aC 48 hours 500 «lConductivity P,tt Cool, 4°C 28 days 250 «4(Specific Conductance) „ .

Cyanide, Total and P.6 Cool, 4°C 14 days" 11Amenable ta Chlorination MaON to pN >12

0.6fl ascorbic acid^Fluor id* P only None required 28 days 250 «lHalogens, Total Organic P,6 Cool, 4 C 28 days 250 ml

H^ to pH <2Hardness P,G HMO, to pM <2 6 months 150 *HNitrogenAnsonia P.6 Cool, 4°C 28 days 500 «l

HjS04 to pH <2Kjeidahl Nitrogen P.O Cool, 4°C 28 days 1 I

N,S04 to pH <2Nitrate P.O Cool, 4°C 48 hours 250 BlNitrate/Nitrite P.8 Cool. 4°C 28 days 250 mi

HjS04 to pN <2Nitrite P.O Cool, 4°C 48 hours 250 miOrganic P,Q Cool, 4°C 28 days 1 I

MjS04 to pM <2

ICTALS

Chronius V! P,8 Cool, 4°C 24 hours 250 BlMercury7 P.8 HNO, to pH <2 28 days 250 mlHetals, except above7 P.8 HHOj to pH <2 6 months 1 I

Oil and Grease 6 only Cool, 4°C, HC1 or 28 days 1 IH2S04 to pH <2 - "

Oxygen, Dissolved G, bottle Fix on site and 8 hours 300 sHwinkler and top store in darkProbe 6, bottle None required Analyzt Innediately 300 al

and topPetroleua Hydrocarbons, G only Cool, 4 C 28 days 1 ITotal Recoverable HC1 to pH <2(TRPN) by 1R

pM (Hydrogen ion) P,6 Hone required Analyze inwdiataly 100 Bl

1R307I38 FISWE4

PRESERVATION SMMXT FOR UATER SAMPLES (continued) p*>* 2

Recommended t Amount ofV 7smeter Container1 Preservative2'3 Holding Tire Sample Required

Phenolic* G only Cool, 4°C 28 days 11Hj$04 to pti <2

PhosphorusElemental G only Cool, 4°C 48 hours 250 BlOrthophosphate P.fi Filter Iswediately. 48 hours 1 I

Cool, 4 CTotal P,C Cool, 4°C 28 days 250 at

NjS04 to pH <2Solids (Residue)Filterable (TDS)Non-Filterable (TSS)TotalVolatile (TVS)

Settleablc SolidsSilicaSulfateSulfide

SulfiteSurfactants (NBAS)TenperatureTurbidity

ORGANIC9

.6 Cool, 4°C 7 days 250 alS Cool, 4°C 7 days 250 «6 Cool. 4°C 7 days 250 at6 Cool, 4"C Tdays 250 alc Cool. 4°C « !»«« 1r«» «'«niy Cool, 4'C 28«Jays 250 al" Cool. 4°C 2B««av» «> al>6 Cool, 4CC, add tine 7 days 250 at

acetate plusNaOH to pH >°

G Cool, 4°C /nalyze (mediately 250 Bl'r Cool, 4°C *« •>«« ' »c None Required Analyze Innediately 100 Bl)c Cool, 4 *8 hours 500 Bl

Purgeable Kalocarbons 6, Teflon Cool, 4°C 14 days S x *0 mlEPA 601,624 lined septum O.OOBX NtjS 5

i .urgeable Aromatict C, Teflon Cool, 4°C 14 days 3 x 40 mls EPA 602,624 lined septun HC1 to pH «2S

0.008X HtjSjOj5Base/Neutral and Acid G, Teflon Cool, 4°C 7 days until 1 IExtractables (GC/MS) . lined cap 0.008X **£fr extraction. 40 daysEPA 625 after extraction

TOO (Dioxin) G, Teflon Cool, 4°C 7 days until 1 IEPA 613 lined cap 0.008X Na2S20,s extraction, 40 days

after extractionPolynuclear Aromatic G, Teflon Cool, 4°C 7 days until 11Hydrocarbons lined cap 0.008X N«2$203S extraction, 40 daysEPA 625 store in dark after extraction

PCBs G, Teflon Cool, 4°C 7 days until 1 IEPA 608 lined cap extraction, 40 days

after extractionPesticides G, Teflon Cool, 4°C 7 daya until 1 IEPA 608 lined cap pH 5-910 extraction, 40 days

after extraction

RADIOLOGICAL

Alpha, Beta and Radium P.G HHO, to pH <2 6 months 1 Gal

AR307I39 FI6URE4

SAMPLE PRESERVATION SUMMARY: SW-846 THIRD EDITIONRecommended Aaount of

Parameter Container1 Preservative Holding Time Sample Required

VOLATILE ORGANICSS010. 8020, 8240

Concentrated Waste Samples G, Teflon Nona 14 days 500 gcsp

Liquid Samples B, Teflon Cool, 4°C 14 days 2 x 40 mlNo Residual Chlorine lined septus 4 drops Cone. Ha

Residual Chlorine G, Teflon Collect saapit in a 14 days 2 x 40 allined septus 250 Bl soil VOA

container preservedwith 4 drops of 10XKajSjO, Nix andtransfer to 40 Blvial preserved with4 drops Cone. Ha,Cool, 4°C

Soil/Sediments and Sludges a. Teflon Cool, 4°C 14 days 250 glined cap

SEMI-VOLATILE ORGANICS ,8080, 8720, 8280

Concentrated Waste Samples G, Teflon None 14 days until 250 glined cap extraction, 40 days

after extractionLiquid Samples 6, Teflon Cool, 4°C 14 days until 500 mlMa Residual Chlorine lined cap extraction, 40 days

after extractionResidual Chlorine 6, Teflon Cool, 4°C 14 days until 500 mt

lined cap add 3 ml 1C* extraction, 40 daysNa2*2°3 P**" sfttr e*tr8Ct<ongallon

Soils/Sediments and Sludges 8. Teflon Cool, 4°C 14 days until 500 glined cap extraction, 40 days

sfter extraction

INORGANICS

Chromius VI P.8 Cool. 4°C 24 hours 250 BlMercury7 P.8 KNO, to pH <2 28 days 250 mlMetals, except above7 P.O HNO, to pN <2 6 months 1 I

SAMPLE PRESERVATION NOTATIONS1 Polyethylene (P> or Glass (B).2 Sample preservation should be performed inasdtately upon sample collection. For composite samples, each aliquot should be

preserved st the tins of collection. When use of en automated sampler makes it impossible ta preserve each aliquot, the samplemay be preserved by maintaining 4°C until compositing and sample splitting is completed.

3 When any sample is to be shipped by comaon carrier or sent through the United States mail, it oust comply uitfc the Departmentof Transportation Hazardous Materials Regulations (40 CRF Part 172). The person offering such material for transportation itresponsible for ensuring such compliance.

4 Samples should be analyzed as soon ss possible after collection. The time* listed are the maximum tines that samples may btheld before analysis and still considered valid. Samples may be held for longer periods only if the permittee or monitoHnrlaboratory has data on flit to show that the specif ie types of samples under study art stable for the longer tint and hatreceived a variance from tha Regional Administrator under Paragraph 136.3(3). Some samples may- not be stable for the maxima*time period listed in tha table. A permittee, or monitoring laboratory, is obligated to hold tha sample for a shorter time i-knowledge exists to shou this is necessary to maintain sample stability.Should only be used in tha presence of residual chlorine.

8 Maximum holding tins is 24 hours when sulMde is present.Samples should be ft Itered immediately on-sita before adding preservative for dissolved metala. For mercury analysis on drii*«mwaters, the samples must be collected in Glass (8) only.

8 Guidance applies to samples to be analyzed by GC, LC, or GC/NS for specific compounds.9 Sample receiving no pN adjustment must be analyzed within seven days of sampling.10 The pN adjustment may be performed upon receipt at the laboratory and may be omitted if simples are extracted within 72 hour*

of collection. For the analysis of sldrin, add 0.008X Na-SjO,.AR307UO FIGURE*PRESSW.UAT/C « M wf V f I t U

3.2 SAMPLE PACKING AND SHIPPING

I. APPLICATION

This procedure 1s applicable to the packing of samples for shipment to alaboratory for chemical analysis.


A. LABORATORY AND TURNAROUND

Water samples will be submitted to:Chester LabNetA Division of Chester Environmental Group4990 Grand AvenuePittsburgh, Pennsylvania 15225

Analyses should be requested at normal turnaround.Sediment samples should be delivered to:

Free-Col Laboratories, Inc.P.O. Box 557, Cotton RoadMeadvllle, Pennsylvania 16335

Analysis should be requested at normal turnaround.B. SPECIAL SHIPPING CONSIDERATIONS

Sediment samples shall be delivered by Aquatic Systems Corporationto Free-Col Immediately after they are collected.

C. OTHER REQUIREMENTS

NoneIII. PROCEDURE

1. Prepare shipping containers for shipment. An Insulated container,such as a cooler or styrofoam box, should be used.

Tape any drains shut.Fill the bottom of the container with vermlcullte, packingfoam, or bubble pack.

2. Seal glass sample containers 1n separate plastic bags or bubble-packbag.

3. Arrange the containers 1n each shipping carton so that they do nottouch. Place packing material between the samples as appropriate.

FIP-OU2 & OU5 -21- 6/29/93

AR3071M

4. If 1ce is required to preserve the samples, cubes should berepackaged in double ziplock bags and placed on and around the .^Jcontainers.

5. Fill the remaining space with packing material.6. . Complete the chaln-of-custody form (as shown 1n Figure 5):

a. CEC project numberb. Self-explanatoryc. Your signature and those of the rest of the sampling teamd. Self explanatorye. Suites of analyses requested, In specific terms. Examples:

TCL VOCsRCRA MetalspH, Specific ConductanceN1, Fe, Mn.

Avoid vague descriptions like "VOCs" or "metals."f. See "Sample Packing and Shipping"g. Date of sample collectionh. Time of sample collection1. Sample number as specified 1n Sampling Proceduresj. Check "AQUEOUS" for watery liquids, "NON-AQUEOUS" for all

othersk. Total number of bottles/jars1. "X" under desired analysesm. Special handing, etc. ,n. Your signature \***o.,p. Date and time you turned over the samples to someone else or

placed them under custody seals.q. Signature of the Individual receiving the samples.r. Self-explanatory.Note; The signatures of every person who has control of the samplesshould appear on the Chaln-of-Custody. If another person (evenanother CEC employee) takes responsibility for packing or shippingthe samples after you have completed the chaln-of-custody form, thatperson should sign as receiving and subsequently relinquishing thesamples.

7. Separate the copies of the forms. Seal the white copy within alarge plastic bag and tape it to the Inside lid of the cooler.Deliver the pink copy to the project manager.

3. Close and fasten the lid of the shipping container.9. Tape the container closed. Place the container In a cardboard

shipping carton, If necessary.10. Complete custody seals and place them on all seams of the shipping

container, or opposite sides of-any Hdded container.

FIP-OU2 1 OU5 -22- 6/29/93

AR307IU2

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AR307IU3

11. Complete a Federal Express air bill (or other carrier If necessaryor specified In PROJECT-SPECIFIC REQUIREMENTS). In addition to ,Jfully completing name, address, and phone number of sender andlaboratory:

Include project number as Internal Billing Information.Check box to bill sender (be sure CEC account number Is filledin).

Check box to send the package Priority Overnight.Retain the pink Sender's Copy

Fill out an air bill for each cooler, or fill out one air bill and:a. Write the number of packages on the air bill in the

appropriate section.b. Number each carton clearly (e.g. 1 of 3, 2 of 3, 3 of 3).

12. Securely attach the air bill to the cooler. Do not cover addresslabel or custody seals.

13. Relinquish the containers to the carrier.IV. EQUIPMENT

Insulated shipping containersPacking material (foam packing, bubble pack, vermiculite)Plastic bags with water-tight sealChaln-of-custody formsStrapping tapeClear postal tapePermanent markersDOT hazardous shipping labels (if required)Air blll(s)


If you have any questions when shipping medium- and high-hazardsamples, call the carrier and ask for the restricted articlessection. They have specialists trained in the shipment of hazardousmaterials who can answer all of your questions.Be certain to seal ice bags and sample containers tightly. Thecarrier will generally refuse to accept or deliver any leakingcontainers, and has no way of knowing whether a leak 1$ an unsealedice bag or a contaminated sample.

FIP-OU2 & OU5 -24- 6/29/93

AR307IH

VI. REFERENCE

Title 49, Code of Federal Regulations, Subtitle B, Parts 100-177.

FIP-OU2 & OU5 -25- 6/29/93

AR307U5

3.3 GROUNDHATER SAMPLING

I. APPLICATION

The procedure is applicable to the sampling of monitoring and residentialwater wells.


A. SAMPLING SCHEDULE AND ANALYSIS

1. Mine Void Wells (1 round):MWV1 MWV6MWV2 MWV7MWV3 MWV3MWV4MWV5

Samples will be analyzed for Low Level VOCs using "SuperfundAnalytical Methods for Low Concentration Water for OrganicAnalysis, Method OLC02.0, 6/91."

2. Homewood Aquifer Monitoring Wells:First Round:

UMW2MWH2 UMW3MWH3 UMW4MWH4 UMW5UMW1

Samples will be analyzed for Low Level VOCs using "SuperfundAnalytical Methods for Low Concentration Water for OrganicAnalysis, Method OLC02.0, 6/91," and pentachlorophenol and

•* * ^ ^ .:*%*rtaAV.5»s*a« WJw*«.y£AW.r.«wyiV.v<v. .ViV« vJv ^bi s (Z ethyl hexyl ) phthal ate

Second Round;UMW2 UMW5UMW3 MWH4

Samples will be analyzed for low level TCL volatile organiccompounds only.

FIP-OU2 & OU5 -26- 6/29/93

AR307U6

Special Consideration; Monitoring wells UMW2, UMW3, UMH5 andMWH4 will have duplicate samples analyzed for VOCs during bothsampling events.

3. Connoquenesslng and Burgoon Aquifer Monitoring Wells (1 round)MWU3 BW3HWB2 CW1DMW2 CW2BW1 CW3BW2

Samples will be analyzed for low level VOCs,pentachlorophenol, and bis(2-ethylhexyl)phthalate, and leadand mercury.

4. Residential Wells (quarterly)Breese Matson ElchmanDininger MontgomeryKreig Slazor

Samples will be analyzed for TCL volatiles using EPA MethodOLC02.0.Special Consideration; The sampling will be performed by P1neTownship personnel. Assistance, including proper sampling andcustody procedures, will be provided to the Township, asnecessary. The Initial round of residential well samplingwill be performed concurrently with monitoring well samplingto provide on-site assistance to the Township, 1f necessary.

B. SAMPLE NUMBERS

Samples should be designed by well number or resident's name,followed by the date In parenthesis. Example: MW-8 (11/22/91).

C. CONSIDERATION FOR FREE PRODUCT

No free product is expected.D. FILTRATION

AHquots for metals analyses should be filtered.E. QUALITY-ASSURANCE SAMPLES

Mine Void. Connoouenessino. Burgeon and Residential Wells; Collectone field blank, one trip blank, and one duplicate sample whilesampling the monitoring wells.

FIP-OU2 & OU5 -27- 6/29/93

AR307IU7

Homewood Wells; Collect one field blank and one trip blank whilesampling the monitoring wells. Monitoring wells UMW2, UMW3, UMW5, ,and MWH4 will have duplicate samples taken. ^—'

F. OTHER REQUIREMENTS

None

III. PROCEDURE FOR MONITORING WELLS

A. INITIAL CHECK

1. Remove the well cap and check for vapors using an organicvapor monitor.

2. Measure the water level from the top of the riser pipe at thepre-marked reference point.

B. PURGING• *

Prior to sampling, each well will be purged to remove stagnant waterwithin the well and obtain a representative sample. Each well willbe purged using the following procedure:1. Calculate the purge volume using the data presented In the

table following this section and the criterion in SectionII.B.

2. Purge the required volume by submersible pump or adecontaminated bailer. Note that a 3.1-Inch I.D., 3-footbailer holds 1.2 gallons and a 1.6-Inch I.D., 3-foot bailerholds 0.3 gallons. Flow rates from a submersible pump can bechecked with a bucket and stopwatch.

C. SAMPLE COLLECTION

1. Collect water from the well using a decontaminated samplebailer.

2. Transfer the sample directly Into sample bottles. Fill VOAvials first. If Indicated In Section II.D., filter samples inaccordance with the appropriate SOP.

3. Measure the temperature, pH, and specific conductance of thesample.

4. Replace the well cap and lock the cover.5. Decontaminate the bailer as specified below.6. Pack and ship the samples as the SOP, "Sample Packing and

Shipping."FIP-OU2 i OU5 -28- 6/29/93 ^

AR307U8

IV. PROCEDURE FOR RESIDENTIAL WELLS

A. INITIAL CHECK

Obtain information on well construction.B. PURGING

1. Run the faucet or other outlet prior to any holding tank ortreatment unit. At some wells, it may not be possible toobtain a sample prior to a holding tank. In these cases,adequate purging will be required to empty the holding tank,as well as to evacuate the well. Wells that are hand operatedwith no storage or treatment will be purged by hand. In allcases, wells will be purged for at least 15 minutes, andsample bottles will be filled directly from the faucet or tap.

C. SAMPLE COLLECTION

1. Samples of Influent will be collected prior to treatment, ifpossible.

2. Transfer the sample directly into VOA vials prior to anytreatment system.

3. Measure the temperature, pH, and specific conductance of theexcess sample.

4. Shut off valve.5. Pack and ship the samples in accordance with Section 3.2.

V. DECONTAMINATION

All sampling equipment - such as bailers, barrel filter, and buckets -willbe decontaminated as follows between each well:1. Wash thoroughly with a simple detergent, such as trisodium

phosphate, and potable water.2. Rinse thoroughly with distilled or deionized water.

VI. DOCUMENTATION


1. Complete a chaln-of-custody form for each shipping containerof samples.

FIP-OU2 & OU5 -29- 6/29/93

AR307U9

2. All field measurements and observations will be noted on aSampling Data Sheet using indelible ink. Entries Include:

Site nameField personnelDate and time of sampling eventWeather conditionsStatic Water LevelPurge volume and methodField measurements, such as pH, specific conductance,temperature, dissolved oxygen, free product thicknessObservations, such as color, odor, clarityAdditional comments as needed, such as any problemsoccurring during purging or sampling, observation ofwell damage, or no lock on well


1. The white copy of the chaln-of-custody form should accompanythe samples. The pink copy should bexlelivered to the projectmanager.

2. Field observations and the Field Data Sheet should beincorporated Into a trip report for transmlttal to the projectmanager and Project File.

VII. PRECAUTIONS AND COMMON PROBLEMS

A. Observe all procedures in the site Health and Safety Plan.B. Unless wells can be purged dry, samples should be collected

Immediately after the purge.C. Wells which exhibit poor yields may need to be purged the day before

sampling. However, this should be done only when necessary.D. Note that well purging Is not the same as well development, although

these may be done concurrently unless prohibited in Project-SpecificRequirements.

VIII. EQUIPMENT AND SUPPLIES

Submersible pump and adequate amount of hoseGeneratorBailer (4-inch and/or 2-Inch as appropriate) constructed ofstainless steel, teflon, or other non-reactive materialRopeNltrlle glovesDecontamination bucketTrisodium PhosphatePaper towelsBailer Brush

FIP-OU2 & OU5 -30- 6/29/93

AR307I50

Distilled or deionized waterpH/conductiv1ty/temperature/dissolved-oxygen meter withcalibration solutionsBarrel filter, filter paper, air pumpTape measure or Interface probeSample bottleSample tagsZiplock bagsPreservatives (as needed)

FIP-OU2 & OU5 -31- 6/29/93

AR307I5I

I F e e tof

StandingWater

123 .4567a91015

1 2 025 .303540455055606570

1 7 580859095100105110115120

CASING INSIDE DIAMETER1-1/4" I 2' 1 4" 1 6"

(Gallons per Well Volume)0.10.20.20.30.40.40.50.60.60.71.01.31.62.02.32.52.93.23.53.84.24.54.85.15.55.86.16.46.77.17.4

1 7.7

0.20.40.50.70.91.01.21.41.51.72.53.34.14.95.86.67.43.29.09.310.711.512.313.113.914.715.516.417.218.018.819.5

0.71.72.02.73.34.04.65.35.96.69.81*. 116.319.622.926.229.432.735.939.242.545.749.052.355.558.862.165.368.571.875.178.4

1.53.04.55.97.48.910.311.813.314.722.129.435.344.151.453.366.973.580.383.295.5102.9110.2117.5124.9132.2139.6146.9154.3161.6168.9176.3

FIGURE 6

AR307I52

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AR307I53

3.4 FILTRATION

I. APPLICATION

This procedure 1s applicable to the filtration of water samples using abarrel filter.


Groundwater samples for metals analysis will be filtered.III. PROCEDURE

1. Pour enough water Into the top of the decontaminated barrel filterto fill the required bottle(s).

2. Check that the 0-ring 1s seated properly In top of the unit.3. Place the sediment screen over the opening. Make sure it is seated

properly. *4. Place a 0.45-m1cron filter paper over the screen.5. Place the base of the barrel filter on the main body unit and

secure.6. Turn the barrel filter right-side-up and attach the tubing and tire

pump to the top.7. Place the sample bottle under the filter outlet.8. Give the tire pump compressions until water begins to flow Into the

bottle. Additional compressions may be necessary if a large volumeof water is required.

9. Fill the sample bottle(s). Be sure to leave enough room to addpreservative to the sample.

10. Empty and decontaminate the barrel filter and components asdiscussed below.

11. DISCARD THE FILTER PAPER. Do not reuse the filter paper.IV. DECONTAMINATION

All portions of the barrel filter which come Into contact with the sample(container, screen, and base) should be decontaminated between samplelocations. Decontamination procedures are as follows:1. Wash the Inside of the barrel filter, the screen, and the base with

potable water and a mild detergent such as trlsodium phosphate. Use

FIP-OU2 8i OU5 -34- 6/29/93

AR307I51*

a small brush or paper towel to reach corners and the groove Inwhich the 0-ring rests.

2. Rinse the unit and screen thoroughly with distilled or deIonizedwater.

V. DOCUMENTATION

Filtration records should be noted on the sample Cha1n-of-Custody,recorded in a field log book, and Included in the final documentation ofthe sampling event.

VI. PRECAUTIONS AND COMMON PROBLEMS

Sediment-laden water may clog the filter. It may be necessary to replacethe filter paper one or more times to filter the required volume.

FIP-OU2 & OU5 -35- 6/29/93

AR307I55

3.5 BIOASSAY SEDIMENT SAMPLE COLLECTION

I. APPLICATION ^

This procedure 1s applicable to collection of sediment samples from thewetland and off-site pond for Chronic Bioassay Testing.


A. NUMBERING SYSTEM

Four samples, two from the wetland and two from the off-site pond,will be collected.The following sample location numbers will be used:Off-Site Pond;

BS1BS2

Wetland:

BS3BS4

B. Samples will be designated by sediment sample number, followed bydate in parenthesis. The time that the samples were collected will \^be recorded on the sample bottle and Chain-of-Custody. Example:

BS1 (11-22-93)

C. LOCATIONS

Sediment sample locations are shown on Figure 2.D. TESTING PROCEDURE

The chronic tests will be conducted using Ceriodaphnia dubla testorganisms and fathead minnows per procedures outlined in Short-TermMethods for Estimating the Chronix Toxiclty of Effluents andReceiving Waters to Fresh Water Organisms, EPA 600/4-89/001, secondedition. Five serial dilutions (100%, 50%, 25%, 12.5% and 6.25%)and a Laboratory Water Control (LWC) will be analyzed for eachcomposited sample.Sediment pore water will be extracted In accordance with theprocedures outlined in "Sediment Toxiclty Assessment" (1992), editedby G. Alien Burton, Jr. All sediment samples will be centrifuged atapproximately 5,650 rpm for 20 minutes and filtered through a 0.20ura filter.

FIP-OU2 4 OU5 -36- 6/29/93

AR307I56

III. PROCEDURE

A. SAMPLE COLLECTION

The negative reference control location for the bioassaysamples will be the off-site pond (Figure 2). Two sedimentsamples will be collected at the control area. Sufficientsediment will be collected to produce 10 L of pore water fromeach location.Two sediment samples wiljj j ljcj ^the bioassay tests.

Bioassay sediment samples will be collected using stainlesssteel, plastic, or plastic-coated Implements. Bioassaysediment samples will be collected from similar hydro!ogleregimes at the control location. The sediment samples

™1 be placed In |lf 5-gallon buckets wTCn?eal1n'g"TTds"'and plastic sample bag liners.Bioassay sediment samples will be Immediately labeledaccording to project, location, date, time, and sample number.

Sediment samples will be maintained at a temperature of 4° C.The analytical laboratory performing the bioassay testing(Free-Col Laboratories, Inc.) will be responsible for thepreparation of the sediment samples to extract pore water foruse in the chronic bioassay tests.

IV. DOCUMENTATION


1. Complete a chaln-of-custody form for each shipping containerof samples.

2. All field measurements and observations will be noted in afield notebook. Entries Include:

Site nameField personnelDate and time of sampling eventWeather conditions

FIP-OU2 & OU5 -37- 6/29/93

AR307I57

Static water levelSediment sample depth ,

V. EQUIPMENT AND SUPPLIES

Sample containers and coolersShovelsTape measureBound and page-numbered field notebook

FIP-OU2 & OU5 -38- 6/29/93

AR307I58

3.6 BIOACCUHULATION EARTHWORK SAMPLE COLLECTION

I. APPLICATION

This procedure 1s applicable to collection of earthworm samples from thewetland and control wetland for evaluation of accumulation of Aroclor 1254In earthworm tissues.


A. SAMPLING SCHEDULE

Four composite samples will be collected during a one-day fieldvisit.

B. SAMPLE NUMBERS

Samples will be designated by composite sample number followed bydate in parenthesis. The time that the samples were collected willbe recorded on the sample bottle and Chain/of-Custody. Example:

Wetland Earthworm Composite 1 (11-22-93)C. COMPOSITE PROCEDURE

Earthworm samples will be prepared and analyzed by the analyticallaboratory In accordance with EPA method OB 10/90, "Extraction andAnalysis of Organlcs in Biological Tissue, as published by the EPA'sEnvironmental Services Division, Region IV Analytical SupportBranch, Athens, Georgia.

III. PROCEDURE

A. FIELD COLLECTION PROCEDURES

Field sampling will be conducted at two locations (wetland andreference locations). The reference area will be locatedupgradlent from the site but will be In a similar hydrologicsetting (depth to local water table, soil moisture). Thereference location is shown on Figure 8.Field collection will be made using the necessary equipment,shovels, etc. for earthworm collection. Earthworms will beplaced in pre-cleaned, 1-1 Her glass jars with vented lids,within coolers containing ice. Jars will be filled to a 10-centimeter depth with moist corn meal. All coolers and samplejars will be properly labeled as to sampling location.The field collection of worms may Initially require thatspecimens of different sizes from multiple species becollected because the dominant species and size ranges presentat both locations may not be readily apparent from preliminary

FIP-OU2 & OU5 -39- 6/29/93

AR307I59

REFERENCES :U.S.G.S. 7.5* TOPOGRAHIC MAP. GROVE CITY. PA. QUADRANGLE. DATED 1961, PHOTOREVISED 1981.SCALE : 1"=2000'

Civil & Environmental Consultants, Inc.PotterPtazaXI • 7MHoMay DtKre • PHttbufoJi.PtMt»yt»anla 1S220

(412) 121-3402 • (SOO)MS-2U4 • Fll (412) MI-

REFERENCE SITE LOCATION PLANOSBORNE LANDFILL SITE

OU2 & OU5 REMEDIAL INVESTIGATIONFIELD INVESTIGATION PLAN

DWN.BY;S.METZI APPROVED BY:CHKD. BY:

SCALE: DATE:r-2000' 1/15/93 91187 FIGURE 8

«nju/ Ibu

observations. Species to be analyzed will be determined afterall collections have been made. Those specimens selected willbe retained for samples, and the other organisms will bereturned live to the locations they were collected from.The same species will be selected from site and controllocations for analysis for PCBs and Aroclor 1254.Two separate composite samples will be obtained at eachlocation (four samples). Each sample will be a composite offive to seven Individuals of comparable size and weight .forthat species.

B. PRE-TREATMENT OF ORGANISMS PRIOR TO DELIVERY TO THE ANALYTICALLABORATORY

The three to five earthworm specimens selected to comprise asample will be placed in a pre-cleaned, 1-liter glass jar (orother suitable container) which has a vented lid and 1s filledto a 10-centimeter depth with moistened corn meal. Sampleorganisms will remain In ASC's custody until delivery to theanalytical laboratory.Earthworms will be kept In cornmeal-filled jars at 20° Celclusat least 48 hours until sacrificial testing of two worms perjar demonstrates that the gut contents of the worms have beenreplaced with cornmeal. Earthworms will be rinsed three timeswith distilled water (at 20° Celsius), packed 1n fresh,moistened corn meal, and Immediately shipped In Ice-packedcoolers to the analytical laboratory.

C. DOCUMENTATION/SAMPLE DELIVERY TO ANALYTICAL LABORATORY FORPROCESSING AND ANALYSIS

A chaln-of-custody form will be completed for transfer of thesamples from the field to the analytical laboratory and alldestinations In-between. The samples will be delivereddirectly to the laboratory by ASC personnel.The analytical laboratory will be responsible for theprocessing of samples for analysis. Standard laboratoryprocedures for decontamination of equipment will be used priorto processing, after each sample 1s processed, and beforestorage of equipment.One duplicate sample from the site will be prepared foranalysis by the analytical laboratory. Therefore, fivesamples will be analyzed for concentrations of Aroclor 1254 inthis study. *

FIP-OU2 & OU5 -41- 6/29/93

AR307I6I

IV. DOCUMENTATION


1. Complete a chain-of-custody form for each shipping containerof samples.

2. All field measurements and observations will be noted on aSampling Data Sheet. Entries Include:

Site nameField personnelDate and time of sampling eventWeather conditionsStatic water level in excavations, if anySoil depth sampled

V. EQUIPMENT AND SUPPLIES

Sample containers and coolers ,ShovelsTape measureBound and page-numbered field notebookCornmealDistilled water

FIP-OU2 & OU5 -42- 6/29/93

AR307I62

4.0 EQUIPMENT USE PROCEDURES

4.1 HNU PHOTOIONIZATION DETECTOR

I. APPLICATION

This procedure 1s applicable to operation of the HNU Model 101photoionization detector for detecting volatile organics found in theambient air. The Instrument serves as a total hydrocarbon analyzer,although it does not detect methane.


A. USAGE

The HNU will be used on the site to monitor the organic vaporconcentration In the breathing zone during all drilling activitiesand to screen all soil samples and boreholes.

B. LAMP REQUIRED

10.2 eV

III. PROCEDURE

The following procedures are used 1n operating the HNU:1. Connect the probe cable plug to the 12-pin keyed socket on the

readout assembly panel. Carefully match the alignment slot In theplug to the key in the connector. Screw down the probe connectoruntil a distinct snap and lock 1s felt.

2. Screw the probe extension into the probe end cap. The probe may beused without the extension, if desired.

3. Turn the function switch to the BATT (battery check) position. Theneedle on the meter will go to the green zone if the battery isfully charged. If the needle 1s below the green arc, or if the LowBattery Indicator comes on, the battery must be recharged before theanalyzer 1s used.

4. Turn the function switch to the STANDBY position. Turn the zeroadjustment until the meter needle 1s at zero.

5. Turn the function switch to the appropriate operating position.Start with the 0 - 200 position and then switch to the sensitiveranges. The UV light source should be on, confirmed by BRIEFLYlooking Into the probe to observe a purple glow from the lamp.

6. Hold the probe so that the extension is at the point where themeasurement Is to be made. . The Instrument measures the

FIP-OU2 i OU5 -43- 6/29/93

AR307I63

Quality Assurance/Quality Control ProgramsPage 44

concentration by drawing the gas in at the end of the extension,through the lonlzatlon chamber, and out the handle end of the probe.

7. Take the reading or readings as desire, taking into account that aircurrents or drafts in the vicinity of the probe tip may causefluctuation in readings. Change the ranges as required.

IV. CALIBRATION

A. FREQUENCY

The calibration of the HNU will be checked dally using a cylindercontaining isobutylene.

B. PROCEDURE

At the factory, the Model 101 Is calibrated'to benzene with the spanset at 9.8. A measurement is then made using Isobutylene. TheIsobutylene reading and the span setting (9.8) are recorded on thecalibration report.In service, the HNU 101 calibration can be checked and readjusted(If necessary) using Isobutylene as follows:1. Connect the HNU to the cylinder regulator with a short piece

of tubing. The calibration gas in the cylinder consists of amixture of Isobutylene and zero air. Isobutylene 1s nontoxlcand safe to use in confined areas. There are no listedexposure levels at any concentration. The regulator sets andcontrols the flow rate at a present factory value of about 250cc/min.It 1s Important that the tubing be clean since contaminatedtubing will affect the calibration reading. Do not use thecylinder below about 30 pslg as readings below that level candeviate up to 10% from the rated value. Safely discard thedisposable cylinder when empty. Do not refill this cylinder.It 1s against the law to transport refilled cylinders.

2. With the SPAN setting and the function switch at the samepositions as listed In the Applications Data Sheet orCalibration Report (normally 9.3 and 0 - 200, respectively),open the valve on the cylinder until a steady reading 1sobtained.

3. If the reading 1s the same as the recorded data, the analyzercalibration for the original species of Interest 1s stillcorrect.

FIP-OU2 & OU5 -44- 6/29/93

AR307I61*


4. If the reading has changed, adjust the SPAN setting until thereading 1s the same.

5. Shut off the cylinder as soon as the reading Is established.6. Record and maintain this new SPAN setting. Recalibrate the

analyzer on the species of Interest as soon as possible.7. Whenever the analyzer is recalibrated, it is to be Immediately

checked with the Isobutylene and the reading recorded. Thiscan then be used for later checking In the field.

C. DOCUMENTATION

Documentation of calibration should be kept In a field log book ora calibration data sheet. At a minimum documentation shouldInclude: date, field personnel, probe type, and readings before andafter calibration.

V. MAINTENANCE

A. The HNU should be kept out of the rain and generally free ofmoisture. It is not water-proof. Water entering the probe orInstrument body may render it inaccurate. The body case may beremoved to allow removal of water or dust with a clean soft cloth.

B. The probe tip must be kept clean and obstruction-free to allow airflow. Remove the tip from the probe and clear it with a pipecleaner.

VI. DECONTAMINATION

Wipe all external portions of the HNU with a damp clean cloth. Wipe drywith a clean cloth or allow to air dry.In some circumstances (such as wet or highly contaminated conditions) itmay be pertinent to encase the Instrument in plastic to decrease thepotential for contamination. This protective covering must contain holesfor both Inflow and outflow of air. The plastic can be wiped off, removedfrom the Instrument, and discarded with personal protective equipment atthe end of the job.

VII. DOCUMENTATION


HNU screening of ambient air, soil samples, and boreholes will befully documented in a field log book and/or on boring logs.

FIP-OU2 & OU5 -45- 6/29/93

AR307I65


JCalibration will be documented in a field log book or a calibrationlog sheet.


Dated and initialed copies of the field data should be given to theproject manager and placed In the project file.

VIII. PRECAUTIONS AND COMMON PROBLEMS

1. The HNU should not be used In rainy conditions unless great care Istaken to prevent the instrument from getting wet.

2. Materials with an 1on1zat1on potential greater that the probe energywill not be measured. For Instance, with a 10.2 eV probe, thefollowing substances are among those which, will not be detected:

Methane (12.98 eV)Hydrogen (10.46 eV)Hydrogen Cyanide (13.91 eV)Carbon Dioxide (13.79 eV)

Refer to the Site Health and Safety Plan for the proper probe.3. The repeatability of the meter reading 1s ± 1% of the full scale

deflection (e.g. on the 0 - 200 ppm scale, the uncertainty is ±9.2ppra). Therefore, at low concentrations near the detection limit,the error could be quite large.

IX. REFERENCE

HNU Systems Model PI101 Photoion1zat1on Analyzer Instrument Manual,Newton, MA 12/85.

FIP-OU2 i OU5 -46- 6/29/93

AR307I66


4.2 HATER ANALYZER(PH,CONDUCTIVITY, TEMPERATURE, DISSOLVED OXYGEN METER)

I. APPLICATION

This procedure applies to measurement of pH, conductivity, temperature,and dissolved oxygen of water using the ICM Model 51100 Water Analyzer.


Temperature, pH, and specific conductance of all water samples should bemeasured at the time of collection.

III. PROCEDUREA. GENERAL OPERATION

1. Assemble - Plug the probe into the meter. (It only fits one way.)Make sure it 1s fully secure. You should hear two "clicks".

2. Remove pH Boot - A small polyethylene capsule covers the end of thePh electrode. It contains a 10% KC1 ph«4 solution which preservesthe Integrity of the electrode and Its calibrated values. This must

«y be removed before pH measurements can be made.3. Rinse the pH electrode - Some of the KC1 solution may have

crystallized on or around the electrode. Rinse with clean water.4. Place the probe in water/solution to be measured. The water should

be deep enough to cover the exposed end of the pH electrode.5. Press ON/OFF key - The display should read "Water Analyzer." If no

keys are pressed, there 1s a 20 second pause before measurements aredisplayed. Press:

ENTER - Immediate display of measurementsMODE - to select a new operating mode

6. Display - The analyzer displays temperature (°C), pH, conductivity(uS or mS), and dissolved oxygen (ppm). Units can be changed inSETUP INSTRUMENT Mode. The center of the top line of the displaywill contain either a "c" or "n", denoting compensated or notcompensated, respectively. In "c" mode pH and conductivity arecompensated for temperature and dissolved oxygen level fortemperature, salinity, and atmospheric pressure. To cfiange between"c* and "n", use MODE options.

FIP-OU2 & OU5 -47- 6/29/93

AR307I67


7. Reading-Storage Option - Pressing STORE while the analyzer isdisplaying readings will cause the current reading to be stored Inmemory. The number assigned to the logged reading will flash Indisplay for 3 seconds. Stored readings may be recalled with theREVIEW READINGS mode or erased with the CLEAR READINGS mode.

B. MODES OF OPERATION

The analyzer contains seven modes of operation. These are called upto display by pressing the MODE key and using the arrow keys to scanthrough the available modes. Press ENTER to call up the desiredmode.1. SETUP INSTRUMENT - Used to change display units. Contains

the following prompts. Within each prompt, use the arrow keystoggle units or yes/no. Press ENTER, to make selection.

Erase All Cal - DO NOT USEUnits for Temp DisplayUnits for Oxygen Display

2. CALIBRATION SET - Allows barometric pressure value to bechanged and prompts for calibration standard solutions to bechanged. In general, this mode 1s not used.

3. CALIBRATION - See Section III of this SOP.

4. REVIEW READINGS - Allows you to read previously storedmeasurements. Use arrow keys to select the number of thestored reading. Press ENTER to display the reading.

5. CLEAR READINGS - Clears all stored readings.6. COMPENSATION ON - Normal operating mode. If in "off" mode,

press ENTER to change to "on."7. COMPENSATION OFF - Not normally used. Press ENTER to change

from "on" to "off."C. RECHARGING BATTERY

The Water Analyzer 1s equipped with a rechargeable battery. Thebattery should provide about 10 hours of continuous operation. A"low Battery" signal will appear when approximately 1 hour of use Isleft. Recharge time 1s 15 hours. DO NOT fully-discharge thebattery before recharging 1t. (It 1s not a NiCad battery). Adirect plug-In charger 1s provided. Also, a cigarette lighteradapter 1s provided for charging. DO NOT. use this adapter in

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extreme temperatures or start the vehicle while the analyzer Isplugged in.

IV. CALIBRATION

A. FREQUENCY

The dissolved oxygen and pH portions of the probe need periodiccalibration. It Is recommended that the dissolved oxygen portion ofthe probe be calibrated at the beginning of each days' use. Storageof the pH electrode 1n the "boot* solution will decrease thefrequency with which 1t Is required. The probe should be calibratedfor pH before each day of operation. The conductivity portion of theprobe has less stringent requirements. The manufacturer statesthat, If working with solutions less than 5,000 micromhos, you willprobably never need to calibrate the conductivity probe. However,conductivity calibration should be checked prior to use of the probeto determine the need for recallbration.

B. PROCEDURE

In the CALIBRATION mode the following Information 1s prompted forone at a time. Press ENTER if you desire to SKIP to the next

- prompt:Barometric PressureNo Oxygen CalAir Sat Ox CalCalib pH 7.00Calib pH 4.00/loCalib pH 10.00/hiCalib Cond 73.9 uSCalib Cond 718 uSCalib Cond 6.67 mSCalib cond 58.6 mS

Press ENTER until the desired calibration prompt is displayed. Forall but the first prompt, the probe is placed in the appropriatecalibration solution, allowed to stabilize (1 to 5 minutes, watchdisplay), and the STORE key pressed to store as a calibration value.The information will be processed and the next prompt willautomatically be displayed.Calibration for dissolved oxygen requires entering the currentbarometric pressure (check T.V. or radio) and -adjusting foraltitude. The displayed barometric pressure Is changed in theCALIBRATION SET MODE.

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C. DOCUMENTATION

Documentation of calibration should be kept in a field log book andcalibration data sheet. At a minimum, documentation should Include:date, field personnel, calibration type (pH, conductivity, ordissolved oxygen), calibration solutions used, and readings beforeand after calibration.

V. MAINTENANCE

Oxvaen Sensor - It may be necessary to replace the oxygen membrane andpolish the gold cathode. Extra membranes and an abrasive paper areIncluded in the kit.Conductivity Sensor - Should corrosion build-up occur, clean using a mildabrasive and a soft toothbrush.oH electrode - STORE IN BOOT filled with 10% KC1 in pH 4 buffer.

DO NOT STORE IN DISTILLED WATER.

DO NOT STORE DRY. If allowed to dry, soak in warm KC1solution for 8-12 hours.

VI. DECONTAMINATION

1. Gently wipe the entire probe with a soft cloth and a mild detergent.It may be necessary to use a soft toothbrush to clean around the pHportion of the probe.

2. Rinse the entire probe thoroughly with distilled or deionized water.VII. DOCUMENTATION


Record pH, conductivity, temperature, and dissolved oxygen readingsfor each sample in a field log book or water-sample data sheet.Record all calibration Information in a field log book or acalibration data sheet.


Dated and Initialed copies of the field data should be~given to theproject manager and placed In the project file.

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VIII. PRECAUTIONS AND PROBLEMS

The WATER ANALYZER does not hold a full charge in temperatures belowfreezing. It may be necessary to use the cigarette lighter adapter foroperation in cold weather conditions.

IX. REFERENCES

Operations Manual

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<J4.3 LEL/02 METER

A. Introduction and Overview; The MlnlGard II Gas Indicator Isdesigned to simultaneously monitor combustible gas and oxygenconcentrations in workplace atmospheres and confined spaces. TheInstrument uses low-powered combustible gas sensors andelectrochemical oxygen sensors. At the site, it will be used tomonitor the test borings, primarily borings encountering the deepmine workings.

B. Method: After the LEL/02 meter has been turned on and reset, It canbe carried anywhere to monitor the atmosphere for both oxygen andcombustibles. When the combustible gas concentration exceeds thefactory-set limit of 25% of the lower explosive limit (LEL), anaudible alarm and visual LEL alarm will be activated. The oxygenalarm will be activated when the oxygen concentration exceeds 23% ordrops below 19.5%.1. Calibration

Turn the meter on by pressing the "ON/OFF" button.Allow the Instrument a 15-minute warm-up prior tocalibration. Allow the meter to stabilize at thetemperature the meter is to be used. ,Press the "FUNCTION" button until "% OXY" appears on thedisplay. Expose the Instrument to fresh air until thedisplay reading stabilizes, then set the display to20.8% by adjusting the "SP OX" control.

To adjust the "SP OX" control, loosen the calibrationcover screws and pivot the cover to expose thecalibration adjustments. Adjust the "SP OX" controluntil the display Indicates "20.8." For additionalInformation concerning the location of the calibrationcover, see the Instruction Manual. If the Instrumentcannot be adjusted to 20.8% in fresh air, the.sensormust be replaced.Depress "FUNCTION" button until % LEL 1s displayed.Adjust "COMB Z" control until a zero reading isobtained.Position sampling/calibration adapter over the sensoropenings at the top of the Instrument and finger-tightento seal. Do not have aspirator bulk and tubing attachedto the adapter.

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Attach the flow control to the calibration gas tank.Attach the tubing, furnished with the calibration kit,between the flow control and the unthreadedsampling/calibration adapter connection.Open flow control valve on gas tank to pass gas throughthe Instrument. When the combustible displaystabilizes, the reading for .75% pentane-in-air shouldbe between 48% and 52%.If the calibration check reading 1s not within 48% and52%, set the display readings to 50% by adjusting the"COMB SP" control located under the calibration cover.Close flow control Valve.Remove sampling/calibration adapter from Instrument.Recheck zero reading in fresh air and repeat process iffresh air reading Is not equal to zero.Remove flow control from calibration gas tank.Close calibration cover and tighten screws.

2. Operation; The following procedures are used 1n operating themeter:

Turn the meter on by pressing the "ON/OFF" buttonfirmly. Visual alarms and buzzer will activate. Themeter will stabilize In 10 seconds.

Press the "RESET" button firmly to cancel alarms. If"BATT" shows on the display, press the "ON/OFF" buttonto turn the Indicator off. Install a fully chargedbattery pack.In fresh air, the percent LEL display should read "000"and the percent 02 display should read 20.8 when the"FUNCTION" button is pressed. If reading other than"000" and "20.8" is displayed, see Section 7.2.1 forcalibration.Select the preferred readout for percent 0", or percentLEL by pressing the "FUNCTION" button. If either the 02or LEL preset limits are exceeded, an appropriate alarm

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will activate. Cancel the alarm by pressing "RESET*when the gas concentration returns to the normal range.When monitoring 1s completed, turn the meter off bypressing the "ON/OFF" button.

C. Precautions; Under no circumstances should the meter be used exceptby qualified, trained personnel, and not until the Instructionsaccompanying the meter and following warnings have been read andunderstood:

The meter 1s designed to measure combustible gas or vaporcontent in air. It will not Indicate the combustible gascontent In an Inert gas background, atmospheres containingless than 10% oxygen, furnace stack or in a reducingatmosphere. Further, this Instrument should not be used wherethe oxygen concentration exceeds that of fresh air (oxygenenriched atmosphere). An explosion may result.Recharging must be done in a non-hazardous location, known tobe free of combustible gases or vapors.Certain materials such as silicone, silicates and organic leadtend to poison the combustible gas sensor, thereby givingerroneously low readings. Calibration checks should be madefrequently if such materials are suspected to be present inthe tested atmosphere.The combustible gas indicator detects only combustible gases(and vapors) in the air. It will not indicate the presence ofcombustible airborne mists or dusts such as lubricating oils,coal dust or grain dust.Pressurized or low pressure samples will give erroneous oxygenpercent readings. For atmospheric sampling at higher or loweraltitudes, the oxygen system should be calibrated at theelevation where sampling is to take place.Add gases, such as carbon dioxide, will shorten the servicelife of the oxygen sensor.When sampling with accessory sampling lines, the shortestpossible length of sampling line should be used to minimizethe number of times the aspirator bulk must be squeezed toobtain a valid Indication.When sampling over liquids, take care that end of samplingline does not touch surface of liquid..

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Do not push on center of oxygen sensor. Damage to the sensormay result.Obstruction of the sensor grid holes in the case will causeerroneously low readings. These holes must be kept open(clean).Combustible gas readings, either negative or greater than 10%LEL, may Indicate an explosive concentration of gas beyond theaccurate response range of the combustible gas sensor.When an atmosphere contaminated with leaded gasoline Istested, the lead produces a solid product of combustion which,upon repeated exposure, may develop a coating upon thedetector element, resulting in a loss of sensitivity.Therefore, more frequent calibration .checks must be performed.

D. References:Mine Safety Appliances, Minigard II, Combustible Gas and OxygenIndicator Instruction ManualMine Safety Appliances, Calibration Test System Instruction Manual

OU5-FIP/16D

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APPENDIX B

CEC CORPORATE QUALITY ASSURANCE PROGRAM

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CIVIL & ENVIRONMENTAL CONSULTANTS, INC.

QUALITY ASSURANCE PROGRAM MANUAL

JUNE 1989

REVISED APRIL 1990

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TABLE OF CONTENTS

Pace

1.0 INTRODUCTION 1

1 . 1 Purpose 11.2 Project Specification Programs 11.3 Review and Updating 11.4 Distribution of Manual 2

2.0 ORGANIZATION

2.1 Corporate 32.2 Projects 3

3.0 STAFF 5

3.1 President 53.2 Principals , 53.3 Project Manager ' 53.4 Review Team Leader 53.5 Staff 5

4.0 PROJECT ACTIVITIES 7

4.1 Preparation of a Proposal and Project Initiation 74.2 Acquisition of Data 34.3 Analysis of Data 84.4 Professional Product 34.5 Independent Review 9

5.0 CORPORATE ACTIVITIES 11

5.1 Professional Development 115.2 Technical Training 115.3 Report Review Program 11

6.0 AUDITING THE QUALITY ASSURANCE PROGRAM 12

6.1 Responsibility 126.2 Scheduling 126.3 Audit Procedure 126.4 Audit Report 136.5 Response 136.6 Audit Records 13

7.0 NON-CONFORMING ITEMS 14

7.1 Reporting Non-Confo nuances 147.2 Data 147.3 Response to Non-Conformance Report . 14

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Table of Contents (continued)ii

Page

8.0 CORRECTIVE ACTION 15

8.1 Procedure by Project Organization 158.2 Procedure by Quality Assurance Officer 158.3 Corrective Action Log 15

FIGURESFigure 2-1 - Project Operations Management Structure 4

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Civil & Environmental Consultants, Inc.Quality Assurance Program Manual Page 1

1.0 INTRODUCTION

Civil & Environmental Consultants, Inc. (CEC), as a professional, consultinggeoscience firm, Is dedicated to providing high quality, professional engineeringand geoscience services to private and public clients. Services will be offeredonly when properly educated and managed staff are available to meet clients'technical requirements, time schedule, and budget. Our management will createa professional environment suitable for the professional growth of the staff.In order to achieve this goal of providing high quality service, CEC willmaintain a quality assurance program (QAP) that addresses all aspects of Usprofessional, technical and support activities. It 1s the objective of thisprogram to maintain the quality of all company activities, particularly thequality of service to clients, at a consistently high level. This program 1$subject to continuing review, and modifications are made as required to reflectchanges in company organization or operation, or to clarify or Improve theprogram.1.1 PURPOSEThe purpose of CEC's QAP is to define an Integrated -program for assuringtechnical quality and consistency in services and delivarables provided by CEC.The components of the program include:

An organization with established lines of responsibility, authority, andaccountability;Staff familiar with their responsibilities, and the objectives andprocedures of the program;Specified procedures for operating the program;Methods to document the QA activities; andActivities to audit the program and correct the deficiencies identified.

The services provided by CEC cover many disciplines, and must respond to thevarying needs of Us clients. The purpose of this program Is not to specifymethods of professional practice, but to provide a framework for achieving theobjective of high quality technical work by formalizing QA procedures.1.2 PROJECT SPECIFIC PROGRAMS

The QAP program outlined in this manual Is applicable to the activities of CECon all types of projects. Project-specific quality assurance plans may barequired for individual projects where more detailed specification ofinvestigation and analysis techniques, documentation, and auditing of projectactivities is required. Before Implementation of a project-specific qualityassurance plan, the plan will be reviewed by a CEC principal not directlyinvolved with the project for consistency with contractual agreements and thefirm-wide program included in this manual. The review will be documented by asign-off on the review stamp by the reviewing principal. This copy of the planwill be a permanent part of the project file. -1.3 REVIEW AND UPDATING

This manual will be reviewed and periodically updated in accordance with therequirements of evolving quality assurance technology. This manual will bereviewed annually by the Corporate Quality Assurance Manager or his designee.Annual review is Intended to mean that the interval between any two successive

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Civil & Environmental Consultants, Inc. ,••,•.,;,.Quality Assurance Program Manual ; Page 2

reviews shall not be more than one year. Reviews shall be documented by amemorandum signed by the reviewer, which Includes a statement that the review hasbeen completed.1.4 DISTRIBUTION OF MANUAL

All employees of CEC are issued a copy of this QAP and are expected to read andunderstand Us contents. This procedure Is consistent with CEC's policy ofhaving all of Us employees responsible for quality assurance. Employees willbe issued copies of all modifications that are produced as a result of annualreviews.

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Civil i Environmental Consultants, Inc.Quality Assurance Program Manual Page 3

2.0 ORGANIZATION ^

2.1 CORPORATE

The general organization of CEC showing the chain of responsibility in theestablishment of policies to the professional and technical staff assigned toproject and service activities is presented in Figure 2-1. The overallresponsibility for quality assurance is held by the President of CEC, Dr. JamesM. Roberts. Dr. Roberts Is the corporate Quality Assurance Manager, and hisduties Include the coordinating of all company quality assurance activities,monitoring the QAP and any project-specific quality assurance plans, and advisingand assisting the Principals and Project Managers in the conduct of theiractivities. Because quality assurance 1s an Integral part of company operations,the day-to-day implementation of the program In project activities and In supportservices is the responsibility of all CEC employees.2.2 PROJECTS

Services to clients are on a project basis. Each project 1s assigned to aPrincipal-in-Charge who is responsible for all aspects of the project. Theproject is started by the assignment of a Project Manager who is responsible tothe assigned Principal for completion of the work, Including contacts with theclient. Depending on the type of services involved, Project Managerresponsibility may be assigned to an officer of the firm; a senior projectengineer, geologist, or scientist; or a project engineer, geologist, orscientist.Professional and technical staff are assigned as needed to assist inaccomplishing the services required by the project. Support services usuallyavailable to the Project Manager in-house Include library, secretarial, typing,drafting, reproduction, and accounting. Other services, such as laboratorytesting and exploratory drilling, are obtained on a subcontract basis, whenrequired, or through a standing contract or agreement for services.The ultimate responsibility for quality assurance on a project basis rests withthe Principal-in-Charge. It Is the Principal's responsibility to ensure that theproject procedures outlined in Section 4.0 of this program are Implemented. Inparticular, it is the responsibility of the Principal to arrange for Independentreview (both personnel and scheduling) of all deliverables. It will be theprimary responsibility of the Project Manager to ensure that calculations,analyses, and data collection activities are performed and checked in accordancewith specified procedures.

AR307I82

PROJECT OPERATIONS

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3.0 STAFF

The responsibility for quality assurance within CEC rests with every staffmember. The quality assurance duties and responsibilities of all CEC personnelare outlined briefly in the following items:3.1 PRESIDENT

The President of CEC, James M. Roberts, 1s the corporate Quality AssuranceManager, and Is responsible for Implementation of the Quality Assurance Program.He is responsible for the development, revision and monitoring of the QAP withthe assistance of the other CEC Principals. His other duties Include developing,implementing and monitoring practice, enhancement strategies, professionaldevelopment programs, and deliverable review activities. He 1s continuouslyresearching and developing quality assurance concepts as applied to professionalservices. Principals and Project Managers receive quality assurance directionsfrom the President.3.2 PRINCIPALS

A Principal is a corporate officer appointed by the President for theprofessional practice and administrative management of all work performed onprojects and tasks assigned to him. A Principal is concerned with professionalpractice, administration, and management. For administrative Items, a Principalis responsible for implementing the QAP within his areas of responsibility. Whenacting as the Principal-in-Charge on a project, the Principal has primaryresponsibility for ensuring that the project 1s performed in accordance with bothcorporate and project specific quality assurance programs and plans.3.3 PROJECT MANAGER

A Project Manager is a senior staff member who 1s assigned to each projectgenerally at Us inception. He is responsible to the Principal-In-Charge for allaspects involved in completion of the services on the project, includingtechnical, management, client contact, and planning and Implementation of theQAP, including implementation of a project-specific quality assurance plan, ifrequired.3.4 REVIEW TEAM LEADER

A staff member will be assigned as Review Team Leader (RTL) on all projects.Depending on the requirements of the project, the RTL may act alone as theindependent reviewer; or, for larger projects, the RTL will organize and compilethe comments of a team of reviewers. In this capacity, he advises and assiststhe Principal-In-Charge and Project Manager in planning and implementing thequality assurance program for the project. He is responsible for conductingquality assurance reviews according to the procedures and schedules, applicableto the project, including audits of subcontractors, vendors, or consultants,where such is required.3.5 STAFF

All staff members, whether with professional, technical, or administrativeduties, or whether in project or service assignments, have quality assurance

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Civil & Environmental Consultants, Inc. ;Quality Assurance Program Manual Page 6

responsibilities. These responsibilities include: (1) being familiar with therequirements of the QAP as presented in this Manual, and with those of anyproject-specific quality assurance plan or procedures manual applicable to hisassignment; (2) conducting his specific assignment according to the applicablerequirements of the QAP pertaining to the project; (3) participating 1n assignedtraining and orientation programs; and (4) Initiating a non-conformance andcorrective action report for all non-conformances discovered.

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4.0 PROJECT ACTIVITIES

Initiating and completing a project consists of four types of activities, asfollows: (1) preparation of a proposal and project Initiation; (2) acquisitionof the required data; (3) analysis of the data and development of designs,drawings, opinions, recommendations, and conclusions, and review; and (4)statement of opinions, recommendations and conclusions generally presented in areport, or submlttal of plans and specifications. All four activities arenormally involved In most projects, although the relative emphasis on each willvary considerably.4.1 PREPARATION OF A PROPOSAL AND PROJECT INITIATION

Submission of an oral or written proposal Is generally the first step in securingmost projects. Prior to preparing a proposal, CEC principals will evaluate thecapability of CEC to perform the project, if awarded to CEC. This will Includean evaluation of staff availability and expertise to perform the technicalaspects of the project. A proposal presents the scope of services, the timeschedule, and the price in sufficient detail to define tha desired objectives ofthe client. Other information, such as personnel resumes or project experiencesummaries, 1s included if considered desirable or required by the client.Because most proposals present costs of performing professional services, andmany proposals present preliminary technical evaluations of data or conceptualdesigns, all proposals will be reviewed by a principal other than the Principal-in-Charge on the project. The extent of review will vary with projectrequirements, but will be performed and documented by sign-off on the reviewstamp on a copy of each proposal. This copy of the proposal will become apermanent part of the project file.Before any services are provided, a contractual agreement 1s entered Into betweenCEC and the client. Only officers of CEC have authority to enter intocontractual agreements with clients. Because of the extreme variety of practice,contractual agreements may vary from formally executed contracts to proposalsaccepted and signed by a responsible client representative, verbal authorizationbased on formal proposals, or letters of Intent. If there are significantchanges occurring during the performance of the services, the contractualagreement 1s amended accordingly.Each project 1s assigned an Identification number. A project file is initiatedat the start of the project; maintained during the entire project; and kept,abstracted, or disposed of according to CEC policies. Separate original andaccounting files are also maintained. In the case of large and complex projects,there is an identifiable master file which contains all significant information,including the location and content of secondary project files, such asspecialized discipline files and site file.The Initial effort on the project may be the preparation of a work plan, if thescope of work was not sufficiently detailed in the proposal. The work plan istailored to the size and complexity of the project. The plan is based on thecontractual agreement, and may be amplified as necessary to show additionaldetails on phase or task descriptions, time schedules,' and budgets. Thecompleted work plan, as approved by the Principal-in-Charge and Project Manager,serves project personnel as the basic guide for providing services on theproject. A revised work plan is prepared, approved, and disseminated in the same

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Civil & Environmental Consultants, Inc.Quality Assurance Program Manual : Page 8

V_/manner as the original work plan, whenever significant changes are made in theorganization or conduct of the project or in the project scope. If a writtenwork plan is developed, it is reviewed by the RTL, who will review projectdellverables generated later in the project.4.2 ACQUISITION OF DATA

Data acquisition proceeds as outlined in the proposal or work plan. Dataacquisition usually consists of one or more of the following: literature search(supplemented by personal communications, as appropriate), field Investigations,and laboratory Investigations. Data Includes relevant observations,measurements, results of field and laboratory tests, and all qualitative andquantitative Information obtained by trained technicians and professionals. Dataare acquired according to methods and procedures which will obtain results thatare objective, repeat able, and of known accuracy. In general, CEC utilizes datacollection methods specified by ASTM, EPA, or other organizations publishingstandard methods. The methods utilized will be documented in field logs.4.3 ANALYSIS OF DATA

All data analyses and interpretations are based on logical, systematicprocedures. If appropriate to the project, background considerations andtechnical concepts utilized in each analysis are recorded as the analysis isperformed, in order that the analytical process may be reconstructed by aknowledgeable reviewer. Only computer programs certified or cross-checked witha known solution are used in connection with project calculations and analyses.Computer Input will be checked by an Independent staff member prior to use ofanalytical results. All manual calculations will be checked by staff familiarwith the theory and methods utilized and the staff will Initial originalcalculation sheets to document the review.4.4 PROFESSIONAL PRODUCT

Development of designs, opinions, conclusions and recommendations is the primarypurpose of CEC project activities. All opinions, criteria, designs,specifications, drawings, recommendations, and conclusions developed are thedirect responsibility of a Principal-In-Charge who 1s responsible for the qualityof the project work. Each Principal must assure himself that the professionalsunder his responsibility have the required capabilities to analyze the data anddevelop opinions, recommendations, and conclusions. The skill and knowledge ofCEC professionals are continuously evaluated and reviewed.The Project Manager has the overall responsibility for the presentation ofdesigns, statements of opinions, recommendations, and conclusions to the client.This 1s done in written communications consisting of reports, memoranda, letters,specifications, and/or drawings. The format, style, and complexity of thesewritten communications vary, depending upon such factors as the contractualagreement, the nature of the project and the wishes of the client. At anappropriate stage, or stages, in the project activity, Indicated results,conclusions, and recommendations are discussed with the client, both to keep himinformed and to obtain his input, whenever deemed appropriate. Opinions,recommendations, and conclusions are sometimes given to the client orally or bymeans of Informal notes and sketches. Opinions, recommendations, and conclusions

AR307I87


which are given orally are either confirmed in writing or adequately documentedin the project file.All reports, specifications and drawings will be subject to project andindependent review. Project review consists of review of all documents producedby the Project Manager and Principal-in-Charge. Following project review, thedeliverables will be submitted for independent review, as presented in Section4.5.

4.5 INDEPENDENT REVIEW

Independent review 1s an Integral part of all professional services rendered byCEC, and 1s conducted In dally practice. It consists of requiring that one ormore peers of the professionals who develop the designs, opinions,recommendations, and conclusions review their adequacy. The corporate QualityAssurance Manager assures himself that Independent review Is made and documented,and that the RTL and other reviewers have the necessary knowledge and skill toperform the review and are not directly involved in the activity reviewed. Therequirements and procedures for the performance, documentation, monitoring andauditing of the independent review activities follow. On large and complexprojects, or projects judged to entail above average risks, independent reviewmay be supplemented by a formal design review. These reviews may be conductedby the RTL alone, or by teams composed of experts in the services to be providedon the project and are made at specific milestones during the project work.4.5.1 Initiation and Verification of Independent Review——The Principal-In-Charge for a project shall assure that: (1) an RTL 1s assignedto the project; (2) the scope of the Independent review to be conducted by eachassigned reviewer is specified; (3) Independent reviews are conducted asspecified; (4) the results of Independent reviews are documented; and (5) anydifferences between originators and reviewers are resolved and the resultsdocumented. The frequency and number of reviews conducted during the projectwork will depend on the complexity and duration of the project and the number oftechnical fields Involved. Independent reviews shall be completed for allprojects prior to submission of the results of the work or technicalrecommendations to the client via a letter or report, whether in draft or finalform. An independent review shall be made on each letter or report, exceptingas noted in this subsection.4.5.2 Qualifications of Reviewer

An RTL or other reviewer shall possess the technical qualifications, practicalexperience, and professional judgement considered by the Principal-In-Charge, orhis designee, as being adequate to conduct the review. The reviewers shall nothave been involved with the substantive technical approach or production of thework to be reviewed. For projects of limited scope and compVexlty, thePrincipal-in-Charge may further designate that a technical review by the RTLalone shall constitute independent review. Such designations and the results ofthe technical review shall be documented.

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Civil i Environmental Consultants, Inc. d> ,Quality Assurance Program Manual Page 10

4.5.3 Scope of Review

The independent review Includes a critical evaluation of the basis and validityof all significant conclusions, opinions, assumptions, evaluations,recommendations, designs, and other items that are required as an end result ofthe project services. It emphasizes establishing the validity of the technicalapproach and other procedures used to form an opinion of the suitability of theend result. The Independent review does not necessarily Include a complete checkof detailed calculations, but does Include verification that a review or checkingof calculations has been adequate. Upon completion of an Independent review, thereviewer shall discuss his comments with the author/originator and shall attemptto resolve any significant Issues. Any unresolved Issues shall be referred tothe Principal-In-Charge for resolution prior to completion of the review process.4.5.4 Independent Review Not Required

The Principal-1n-Charge may find that a project does not require Independentreview. Projects or reports in this category are those for which Independentreview is Impractical; for example, preparation and testimony as an expertwitness; individual consultation in which an Individual has special expertise.Further, an Independent review 1s not required for the submission of testresults, boring logs, construction observations or similar Information, providedthe data have been reviewed by a responsible individual and the transmittalletter contains no technical recommendations. This finding shall be documentedby the Principal-In-Charge by Identifying the project as a project where no

i , independent review i s required.4.5.4 Documentation

The results of each Independent review shall be documented by the reviewer so asto provide a permanent record of the review in the project files. The record ofthe review shall Identify the reviewer, the scope of the review, and the opinionof the revlewer(s) (use of rubber stamp). Verification that reviewer commentsare correctly implemented into the final draft 1s the responsibility of thePrincipal-In-Charge. The permanent record documenting this verification will bemaintained in the project file (final copy showing actions in response toreview).

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5.0 CORPORATE ACTIVITIES

CEC maintains a professional development program as a standing policy of thefirm. The purpose of this program is to provide motivation and assistance towardthe maintenance of a high degree of skill and knowledge among the professionalsof the firm. This is achieved through a series of programs directed towardimprovement of practice methodology and development of the relevant experienceand education of employees. This program 1s administered by the Vice Presidentof Personnel.5.1 PROFESSIONAL DEVELOPMENT

Professional development programs are encouraged by CEC. These programs mayinclude seminars, continuing education activities, sponsorship of professionalsociety participation, and new employee training. These activities are conductedunder the direction of the Vice President of Personnel. Professional developmentactivities will generally be implemented on an employee-by-employee basisconsidering the usefulness of the activity with respect to the employeesdevelopment within CEC and the anticipated need for the skills being developed.Additionally, CEC will provide in-house loss prevention training to all staffusing ASFE/Terra Insurance materials.5.2 TECHNICAL TRAINING

Technical training will be provided to employees via on-the-job training. Thistraining will consist of observing a task, performing the task with supervision,and performing the task without direct supervision but with scrutiny of results.During the task observation phase, the employee observes an experienced personperforming the task. This observation period gives the employee time to becomefamiliar with task procedures, including technical protocols and documentationprocedures. This period gives employees opportunities to ask questions relatingto tasks.After observing the task, the employee is given hands-on experience by performingtasks under the supervision of an experienced staff member. The supervisor onlyoffers assistance 1f asked, or if an error is observed. This phase of trainingcontinues until the employee performs the task without the supervisor'sassistance.The employee will next be required to perform the task without a supervisorpresent. At the conclusion of the task, the supervisor will review the taskproducts for errors and completeness. If no errors are present, the on-the-jobtraining for that task will be completed.5.3 REPORT REVIEW PROGRAM

CEC will participate in ASFE's report review program which will provide CEC withindependent review of Us work products. The results of these reviews will becirculated so that recommended modifications to CEC reports will be implementedfirm-wide.

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Civil 4 Environmental Consultants, Inc. *!•Quality Assurance Program Manual Page 12

6.0 AUDITING THE QUALITY ASSURANCE PROGRAM

This section describes requirements and guidance for performing Internal andexternal audits to verify compliance with the elements of the QAP. Theobjectives of the audit are:

To determine that a QAP has been developed and documented in accordancewith specified requirements;To verify by examination and evaluation of objective evidence that thedocumented program has been Implemented;To assess the effectiveness of the QAP;To identify non-conformance; andTo verify correction of identified deficiencies.

6.1 RESPONSIBILITY

The President of CEC who acts as the corporate Quality Assurance Manager, or hisdesignated representative, audits the QAP in accordance with the requirements ofthis procedure and reports the audit findings to the corporate officers.6.2 SCHEDULING

A general audit of the QAP will be made approximately every 12 months, unlessotherwise stated in a specific procedure. Regularly scheduled audits may besupplemented by audits for one of the following reasons:

When significant changes are made 1n the QAP;When it is necessary to verify that corrective action has been taken on anon-conformance reported in a previous audit; andWhen a systematic, independent assessment of program effectiveness 1sconsidered necessary.

6.3 AUDIT PROCEDURE

Checklists will be used to ensure depth and continuity of audits. The auditchecklist is intended for use as a guide and will not restrict the auditinvestigation when findings raise further questions that are not specificallyincluded in the checklist. Selected elements of the QAP shall be audited to thedepth necessary to determine whether they are being implemented effectively.Conditions requiring immediate corrective action shall be reported immediatelyto the Principal-In-Charge and, if appropriate, others. . .. •

At the conclusion of the audit, a post-audit conference shall be held with thePrincipal-1n-Charge and Project Manager, if appropriate,, or his designatedrepresentative, to present audit findings and clarify misunderstandings. Auditfindings shall be concisely stated by the auditor on the List of Findings forPost Audit Conference. The findings will be acknowledged by the Principal-1n-

AR307I9I


Charge or Project Manager or his designated representative by signing the audit \Jreport.6.4 AUDIT REPORT

An audit report will be prepared by the Audit Leader and signed by the applicablePrincipal-in-Charge. The report will Include the following:

Description of the audit scope;Identification of the auditors;Persons contacted during audit and post-audit activities;A summary of audit results, including an evaluation statement regardingthe effectiveness of the QAP elements which were audited;Details of findings and program deficiencies will be reported on an AuditFindings Report (APR). Each finding and program deficiency shall beidentified and described in sufficient detail to assure that correctiveaction can be effectively carried out by the project organization; andRecommendations for correcting the findings or improving the QAP.

6.5 RESPONSE

6.5.1 Bv Pro.iect Organization

The Principal-in-Charge or Project Manager or his designated representative shallrespond to the AFR by preparing a Corrective Action report. The response shallclearly state the corrective action for each finding, including action to preventrecurrence and the date the corrective action will be completed.6.5.2 Bv Quality Assurance Manager

Follow-up action shall be performed by the Quality Assurance Manager or hisdesignated representative to:

Evaluate the adequacy of the response;Assure that corrective action 1s identified and scheduled for each non-conformance;Confirm that corrective action is accomplished as scheduled; andFollow-up action may be accomplished through written communication, re-audit, or other appropriate means.

6.6 AUDIT RECORDS

Records shall be generated and retained for all audits. Records shall includeaudit reports, written replies, the record of completion of corrective actions, ^and documents associated with the conduct of audits which support audit findingsand corrective actions as appropriate.

AR307I92


7.0 NON-CONFORMING ITEMS

7.1 REPORTING NON-CONFORHANCES

The Audit Finding Report provides a means for informing management of all non-conformances, and provides a documented history of each non-conformance andcorrective action. Any employee may be the originator of a non-conformancereport. A non-conformance 1s defined as a deficiency in procedure ordocumentation which renders the quality of an item unacceptable or Indeterminate.Following 1s the procedure used in reporting and processing a non-conformance:

The originator submits the report, Including a brief description of thenon-conformance (observation/finding), the action which he proposes forcorrection of the non-conformance (recommendations), and, If appropriate,proposed corrective action to prevent recurrence of the non-conformance(corrective action reply). If the non-conformance was discovered duringa quality assurance audit, the report 1s prepared by the auditor, andreference is made to the audit report.

f

The originator submits the report to the Project Manager and thePrincipal-In-Charge.

7.2 DATA

7.2.1 Non-ConformingData that are in non-conformance due to lack of adequate documentation, checking,review, or deviation from specified procedures need not be segregated, but maybe used provided acceptable corrective action Is taken.7.2.2 Rejected Data

Data that are not amenable to corrective action cannot be made to conformto the requirements of established procedures, are rejected due to out-of-cali brat ion equipment, or data which In the judgment of theEngineer/Geologist are suspect and cannot be verified, will be marked soas to signify rejection.The decision to reject the data Is the responsibility of theEngineer/Geologist/Scientist in charge of that phase of the work afterconsultation with the Project Manager. The decision to reject the datawill be documented by the Engineer/Geologist/Scientist in charge by aconcise memorandum to the Project Manager describing the problem and thereasons for the rejection.

7.3 RESPONSE TO NON-CONFORHANCE REPORT

All non-conformance reports shall be in accordance with the procedures presentedin Section 8.0, Corrective Action.

AR307I93


8.0 CORRECTIVE ACTION

When a condition adverse to quality is detected, it shall be reported to theProject Manager and the Principal-in-Charge, in accordance with the proceduresestablished in Section 7.0, Non-Conforming Items. The response to the non-conformance report shall be as hereinafter described.8.1 PROCEDURE BY PROJECT ORGANIZATION

The Project Manager or his designated representative shall respond to the AuditFinding Report by preparing a memorandum of response. The response shall becompleted within 20 days from the date of the audit report.8.2 PROCEDURE BY QUALITY ASSURANCE OFFICER

Follow-up action shall be performed by the Audit Leader responsible for the auditfindings to:

Evaluate the adequacy of the response; -Assure that corrective action is identified and scheduled for each non-conformance;

Confirm that corrective action is accomplished as scheduled; andFollow-up action may be accomplished through written communication, re-audit, or other appropriate means.

8.3 CORRECTIVE ACTION LOG

The Audit Leader shall maintain a Corrective Action Log. When all the correctiveactions have been verified, a completed copy of the log shall be sent to theProject Manager signifying a satisfactory closeout of the audit or otheridentified non-conformances.

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APPENDIX C

CHESTER LABNET QA/QC PROGRAM

AR307I95

QA/QCQuality Assurance/Quality Control Program

Presented by

CHESTER LabNetA Division of Chester Environmental Group

P.O. Box 9356, Pittsburgh, PA 15225-0356412269-5708

AR307I96

TABLE OF CONTENTSEaoa

1.0 INTRODUCTION 1-1

2.0 OBJECTIVES 2 • 1

3.0 ORGANIZATION AND RESPONSIBILITY 3-1

3.1 DIVISION 3-1

3.1.1 Organization 3-13.1.2 Responsibility 3-1

3.2 LABORATORY 3-3

3.2.1 Organization 3-33.2.2 Responsibility 3 - 3

4.0 SAMPLE CUSTODY 4 -1f4.1 CUSTODY AND DOCUMENTATION IN THE FIELD 4 - 1

4.2 SAMF1E CUSTODY IN THE LABORATORY 4-6

4.2.1 Sample Receipt in the Laboratory 4 • 64.2.2 Shipment Inspection 4-64.2.3 Reconciliation with Chain-of-Custody Document 4-84.2.4 Resolution of Shipment Irregularities 4-94.2.5 Sample Log-In 4-10

4.2.5.1 Entry in Master Log 4-104.2.5.2 Job Traveller 4-114.2.5.3 Sample and Sub-Sample Numbering 4-134.2.5.4 Information Distribution and Job Filing 4-13

4.2.6 Custody Transfer within the Laboratory 4-154.2.7 Sample Disposal 4-154.2.8 Custody Transfer for Prepared Samples 4-19

5.0 ANALYTICAL PROCEDURES 5 -1

5.1 COORDINATION OF ACTIVITIES 5 -1

5.2 PREPARATION OF SAMPLE CONTAINERS 5-1

5.3 INSTRUMENT MAINTENANCE 5-3

5.4 PREPARATION OF STANDARDS 5 - 4

5.5 DETERMINATION OF DETECTION AND QUANTITATION LIMIT . - 5-10

5.5.1 Instrument Detection Limit 5-105.5.2 Method Detection Limit ' 5-115.5.3 Quantitation Limit ' 5-13

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TABLE OF CONTENTS(Continued)

•"'""5.5.4 Conversion of Detection Limits to Minimum

Detectable Concentration 5-145.5.5 Documentation of Detection Limits 5-145.5.6 Application of Limits in Data Reporting 5-15

5.6 INSTRUMENT AND EQUIPMENT CALIBRATION 5-15

5.6.1 Initial Calibration 5-155.6.2 Continuing Calibration 5-185.6.3 Calibration Frequency 5-19

5.7 A 1ALYT1CALMETHODS 5-20

5.8 ANALYSIS OF QUALTTY CONTROL SAMPLES 5-21t5.6.1 Blanks 5-21

5.8.1.1 Reagent Blank 5-215.8.1.2 Method Blank 5-21

5.6.2 Spiked Blank 5-225.8.3 Spiked Sample 5-235.8.4 Sample Duplicate 5-245.8.5 External Quality Control Audit 5-255.8.6 Record Keeping on Analysis of QC Samples 5-25

5.9 LGEOFSIJRROGATES 5-26

5.10 ESTASUSHMENTrOFACCEPTANCECRrrERIA . 5-27

5.11 DEVELOPMENT OF NEW OR MODIFIED METHODS 5-30

6.0 DATA HANDLING 6-1

6.1 DATAFECORDING 6-1

6.1.1 Notebooks 6-16.1 .2 Record Keeping in Sample Preparation 6 - 26.1 .3 Record Keeping in Instrumented Analysis 6 - 36.1 .4 Record Keeping in Noninstrumented Analysis 6 - 7

6,2 DATAREDUCT10N 6-7

6 . 3 DATA VALIDATION 6 - 9

6.4 DATA COMPILATION " 6-11

6.5 FINAL REVIEW 6-11

,AR307I98

TABLE OF CONTENTS(Continued) , y j

7.0 CORRECTIVE ACTION 7 -1

7.1 IDENTIFICATION OF POTENTIAL PROBLEMS 7 -1

7.2 PROBLEMS AND ACTIONS 7-2

7.2.1 Continuing Calibration Outside Acceptance Range 7 - 27.2.2 Calibration Standards Exceeding the Permitted

Holding Time 7 - 27.2.3 Laboratory Method Blanks Exceed Method Detection

Limit but Are Below Quantitation Limit 7 - 37.2.4 Laboratory Method Blank Exceeds the Quantitation

Limit 7-37.2.5 Laboratory Control Standard Exhibits Recoveries

Outside the Acceptance Criteria 7 - 47.2.6 Surrogates and Sample Spikes Exhfoft Recoveries

Outside the Acceptance Limits 7 • 47.2.7 Control Chart Exhibits a Regular Trend 7 - 47.2.8 Poor Performance on an internal System Audit or

an External Performance Evaluation 7 - 5

111 AR307I99

FIGURES• Page

3 -1 DIVISION ORGANIZATION CHART 3 - 2

3-2 LABOFttTORYOFlGANIZATION CHART 3-4

4 -1 FIELD CHAIN-OF-CUSTODY 4 - 3

4 - 2 SAMPLE SHIPMENT CHECKLIST 4.7

4-3 SAMPLE MASTER LOG PAGE 4-12

4-4 JOB TRAVELLER 4-14«

4 - 5 INTERNAL SAMPLE TRANSFER 4-16

4-6 SAMPLE DISPOSAL RECORD 4-18

4-7 PREPARED SAMPLE CUSTODY TRANSFER ' 4-20

5-1 ANALYTiCALREQUESTFORM 5-2

5 - 2 INVALID DATA NOTIFICATION 5 - 5

5-3 STANDARD PREPARATION LOG 5-9

6-1 ORGANIC EXTRACTION 6-4

6 - 2 METALS PREPARATION 6 - 5

lv AR307200

TABLES

4 - 1 CONTAINERS. PRESERVATIVES. AND HOLDING TIMES 4 - 4

5-1 STANDARDS AND SOLUTIONS HOLDING TIMES 5-6

5-2 CALIBRATIONS FREQUENCIES 5-19

5-3 SURRCGATECCMPOJNDSANDACCEFTABLERECOVERIES 5-26

AR30720!

1.0 INTRODUCTION

The Analytical Division of Chester Environmental Group, Inc., Chester LabNet, iscommitted to excellence in chemical analysis. All data generated by the ChesterLabNet Division must be technically sound, property documented, legally defensible,and supported by defined and verified confidence limits. The Division consists ofChesterLab, Neville Island, PA; Keystone Lab-Monroeville, PA; Keystone Lab-Houston, TX; and Keystone/NEA, Tigard, OR.

This document is designed to serve as a guideline to Chester LabNet as a whole.Specifically, this document defines the divisional objectives, organization, functionalactivities, and QA/QC programs that routinely apply to the entire division. Thisdocument is supplemented by sets of Standard Operating Procedures that areunique to the separate laboratories. This document delineates the standardpractices within Chester LabNet; for specific projects, addenda will be preparedresponding to the project needs.

749M17/KW2 1-1 AK307202

2.0 OBJECTIVES

The Quality Assurance Program at Chester LabNat is principally aimed at producingresults of verifiable high quality. Towards this goal, the Program addresses severalareas:

1. Detection of problems through statistical measures ofacceptability and confidence

2. Implementation of corrective action

3. Documentation procedures designed to produce legallydefensible results

4. Establishment of training programs to assure that eachperson is thoroughly familiar with tha methods,procedures, and documentation of his area of activity

5. Development of a review and validation process to verifythat all data produced by the Division are within theguidelines defined in this Manual and the associatedStandard Operating Procedures.

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5/88 M AR307203

, 3.0 ORGANIZATION AND RESPONSIBILITY

Before delving into the the procedural aspects of this Manual, it is necessary to definethe organizational structure of the Division so that reporting and responsibility levelscan be outlined.

3.1 DIVISION

3.1.1 Organization

The Divisional organization is schematically shown in Figure 3-1.

3.1.2 Responsibility f

While the functions of Divisional personnel are principally administrative,certain responsibilities relative to the Quality Assurance Plan do exist.

The Division Operations Manager is responsible for assuring that the\~J Laboratory Directors, the Technical Director, and the Laboratory Information

System Manager are thoroughly familiar with the Divisional Quality AssuranceManual and good laboratory practices. It is also the responsibility of theOperations Manager or his designee to approve all changes and revisions in theDivisional Quality Assurance Manual.

The Information System Manager is responsible for assuring that allreports generated by the system are correct and complete, and for verifying thatall necessary back-up data are available. It should be emphasized that reportsare generated at two different levels. For projects that are entirely internal to asingle Laboratory, the reports are generated, approved and verified in thatLaboratory. Reports on projects that involve several laboratories requireintegration of data. The assignment of the responsible laboratory, andcoordination of the integration of data for reports involving several laboratoriesis the responsibility of the Information System Manager. Coordination anddistribution of samples on projects that necessitate employing more than one

, facility will also be performed by the Information System Manager.

3., RR30720U

Division Organization Chart

TechnicalDirector

OfficeSupport

mmm

mm

OperationsManager

mmm

mmm

mmm

mmm

mm

mm

*

Marketing/Sales

InformationManagement

Lab DirectorHouston, TX

Lab DirectorPitb. urgh, PA

Lab DirectorMonroeville, PA

Lab DirectorPortland, OR

AR307205

The Technical Director serves the role of establishing appropriate protocols—J within the individual laboratories and assuring that the Division quality

assurance program is being followed. In cases of deviations from establishedprocedures, the approval of the Technical Director must be obtained. TheTechnical Director will also review and approve all new methodologiesestablished in any of the laboratories. It is the responsibility of the TechnicalDirector to assure that all work performed by the Division meets technicallysound criteria.

The role of the Laboratory Directors will be discussed in the next Section.

3.2 LABORATORY

3.2.1 Organization

Figure 3-2 illustrates generically the organization of each Laboratory within theDivision.

^ 3.2.2 Responsibility

The Laboratory Director is responsible for assuring that all SectionManagers are thoroughly familiar with the Divisional Quality Assurance Manualand good laboratory practices, and that all laboratory personnel meet therequisite qualifications for their positions within the laboratory. TheLaboratory Director, or his designee, must review and approve all outgoingreports. The Laboratory Director is also responsible for effective dailymanagement of the laboratory and its staff, and for communication and liaisonwith the client.

The Section Manager is responsible for the production of quality resultswithin the Section. To achieve this, the Section Manager must be thoroughlyfamiliar with the Divisional Quality Assurance Manual and the associated

*

Standard Operating Procedures for his Section. He is also responsible forfamiliarizing the Section personnel with the Quality Assurance Manual and the

REV.O5/88 3-3 AR307206

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REV.O5/88

AR307207

, Standard Operating Procedures, overseeing that required protocols are followed,—' reviewing the results, and approving release of the data to the Data Management

Group. The Section Manager, in coordination with the Sample and DataManagement Section and the Project Manager, if a special project Is involved, isresponsible for the scheduling of work in the Section and conforming to requiredholding times. The Section Manager, in conjunction with the Quality AssuranceManager, is responsible for providing the necessary training to the Sectionpersonnel.

The Group Leaders and analysts in the Inorganic Section, the Organic Section,and in Special Projects are responsible for performing all analyses as required,paying attention to the required QC analyses demanded by the analytical method ortechnique. In order to provide proper analysis, they must be familiar with theQuality Assurance Manual and the associated Stan'dard Operating Procedures.They are also responsible for initiating system or method corrective action,should they become aware of a malfunction. Initiation of corrective actionrequires appropriate notification, as discussed later in this Manual.

The Sample end Data Management Section Manager is responsible for thecoordination of the activities of the Sample Management Group and the DataManagement Group. It is his responsibility to assure that the group leaders arethoroughly familiar with the Quality Assurance Manual. He is also responsiblefor interacting with clients in case of discrepancies or irregularities in thesample shipment. In addition, he is responsible for maintaining and updating theschedules within the Department.

The Sample Management Group Leader is responsible for the followingfunctions: sample receipt, storage, distribution of the information through theLaboratory, sample custody, and sample disposal. It is his responsibility tonotify the Section Manager should there be any discrepancies or irregularitiesin the shipment of samples.

The Data Management Group Leader is responsible for maintaining thestatus of the work within the Laboratory, coordinating the compilation of thedata, and preparation of reports for review and approval. It is also his

REV.O5/88 3-5

AR307208

responsibility to alert the Section Manager if there are apparent problems inmeeting schedules or holding times.

The QA/QC Manager is responsible for assuring that the QA/QC requirements ofthe Quality Assurance Manual and its associated Standard Operating Proceduresand addenda are strictly adhered. He is responsible for review and validation ofdata, alerting the Sections should the need for corrective action exist, performinginternal audits as specified by the Manual, introduction of performanceevaluation samples on a periodic basis, and maintenance of the QC records. He isalso responsible for preparing project specific QA/QC plans, and interfacing withclients on matters pertaining to data quality.

The QA/QC Manager functions independently of the laboratory staff. In order toachieve independence from the pressures of daily production in the laboratoryand maintain the necessary objectivity, the QA/QC Manager reports both to theLaboratory Director and the Divisional Technical Director.

The Project Manager is a special position assigned by the Laboratory Directorfor specific projects. Projects may require a specifically assigned managerbecause of unusual duration of the project, complexity of the analyticaltechniques or reporting requirements, and coordination of activities in severallaboratories. The responsibility of the Project Manager to the specific projecttranscends that of the Laboratory Director. It is the Project Manager'sresponsibility to assure that work on the project is performed in accordancewith project specified protocols, following project specific QC requirements.Acceptance of results on analyses for the project is subject to approval by theProject Manager.

REV.O5/83 3-6

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4.0 SAMPLE CUSTODY

To provide for legal defensibility of ail work performed at a given site, it is essential tobe able to provide documentation tracing the samples from collection, to the labora-tory, and through the analytical procedures. Chester LabNet performs both samplingfunctions and analytical functions; however, the Division can only guarantee that thisManual is followed from the point of origin only for samples that are both collected andanalyzed by Chester LabNet.

Maintaining sample custody consists of two distinct aspects: maintenance of thesamples in the field, and maintenance of the samples from the time of receipt in thelaboratory. These two aspects are discussed separately in the following sections.Inasmuch as sampling is not necessarily performed by our personnel, the custody anddocumentation in the field are included here as a recommendation.

4.1 CUSTODY AND DOCUMENTATION IN THE FIELD

The field sample custodian, which, depending upon the project, may be the sampleror another person in the same sampling group is considered to have custody of thesamples at all time during the field operations, until the samples are shipped to stor-age or to the laboratory. Upon collection of a sample in the field, the sampler tags thesample with its site and type (water, soil, sludge, etc.) identification. The sampler alsoindicates on the tag the date and time of sampling. After cleaning the exterior of thesample container, the field sampler transfers the container with the tag to the fieldsample custodian.

Throughout this document, the term sample is used to indicate a quantity of one typeof material collected at one time, at a single location. Thus, a water sample may beshipped to the laboratory in several containers, depending upon the required testingand sample preservation dictated by the project. Each container is identified as a sub-sample, but it is not classified as a unique sample.

The field sample custodian compares the identification of the individual sample withthe sampling plan, and enters all pertinent information on the chain-of-custody docu-ment and on the label of the sub-sample container. The information that must beincluded consists of the following:REV.O5/88 AR3072IO

a. Project identificationb. Sample identification (such as station number and location) ~/c. Date of samplingd. Time of samplinge. Name of samplerf. Parameters for which the sample is to be analyzedg. Number of containersh. Sample matrix (ground water, surface water, wastewater, soil,sediment, sludge, unknown waste, etc.)i. Added preservatives in each sample containerj. Ice chest numberk. Chain of custody number

A sample field chain-of-custody is shown in Figure 4-1.

The field sample custodian is then responsible for packaging the sample(s) for shipping,adding ice if the samples require chilling, signing and dating the chain of custodydocument, placing the chain of custody document in a water-proof envelope and attachingthe envelope to the inside of the ice chest lid. x—

If the samples are to be shipped by a common carrier, then the field sample custodianmust also place custody seal on the ice chest

Simultaneously with filling the chain of custody document, the field sample custodianalso records the information in the field logbook. In filling the chain of custody documentand the field logbook, any corrections that need to be made must be done so that theoriginal incorrect entry is legible. Hence, the incorrect entry is lined out. and thechange is initialed and dated by the field sample custodian.

Table 4-1 lists the required types of containers, preservatives, and holding times foreach type of analyte. It is the responsibility of the field sample custodian to assure thateach sample or sub-sample are packaged correctly. The samples are considered

•>

formally to be in the custody of the field sample custodian until they are officiallytransferred to the carrier, and the transfer is documented on shipping records, or untilthe samples are transferred to the laboratory in person.

^

2w° 4-2 AR30721I

4-3 HR3072I*

TABLE 4-1CONTAINERS, PRESERVATIVES, AND HOLDING TIMES ^J

ANALYSIS CONTAINER1 PRESERVATIVE HOLDING TIME2

Volatile organics G Coolto4°C 14 d

Semivolatile organics G Coolto4°C 7 d to extraction,40 d for extract.

Organochlorine pesticides G Coolto4°C 7 d to extraction,40 d for extract.

Herbicides G Cool to 4°C 7 d to extraction,40 d for extract

Organophsophorus pesticides G Cool to 4°C ' 7 d to extraction,40 d for extract

Cartaamates G Cod to 4°C 7 d to extraction,40 d for extract

Triazines G Coolto40C 7 d to extraction.40 d for extract i

Metals (except mercury) P HNOa 6 m

Mercury P HN03 28 d

Hexavalent chromium P Coolto40C 24 h

Acidity, Alkalinity P,G Coolto40C 14 d

Ammonia. COD, total P,G H2S04, Cod to 4°C 28 dphosphorus

BCD P.G Coolto4°C 48 h

Chloride, Ruoride P None 28 d

Color P,G Cool to 40C 48 h

Cyanide P,G NaOH, Cool to 4°C 14 d

Hardness P HNCg 6 m

pH P,G None • NoneW

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AR3072I3

TABLE 4-1CONTAINERS, PRESERVATIVES, AND HOLDING TIMES

(CONTINUED)

ANALYSIS CONTAINER1 PRESERVATIVE HOLDING TIME2

Nitrogen, Kjeldahl and G H2S04, Cool to 4°C 28 dTotal organic, Phenols

Nitrate, Nitrite P,G H2S04, Cool to 4°C 48 h

On and Grease G H2S04, Cool to 4°C 28 d

Ortho-phosphate P,G Coolto4°C 48 hDissolved oxygen G None None

»Residue, Total, Filterable, P,G Cool to 4 0 7d

Nonfilterable and Volatile

Residue. Settleable P.G Coolto4°C 48 h

Silica P Cool to 40C 28 d

Sulfate, Specific Conductance P, G Cool to 4°C 28 dSulfide P,G Zinc acetate + NaOH, 7d

Coolto4°CSulfite P,G None None

Surfactants, Turbidity P,G Coolto4<>C 48 h

Temperature P,G None None1 ) P • Polyethylene

G. Glass2 ) h « hours

d-daysm « monthsNone means that analysis must be done immediately

REV.O5/88 4-5

RR3072IU

4.2 SAMPLE CUSTODY IN THE LABORATORY

The laboratory operation, as it pertains to the sample custody, consists of severalfunctions. Specifically, these are: sample receipt, inspection of the samples,reconciliation of the information on the sample label and the chain-of-custody, alertingthe project manager or the Sample and Data Management Section Manager of anyinconsistencies in the shipment, logging in of the samples, placing the samples inappropriate storage areas, distribution of the information to the laboratory analyticalsections, transferring of the custody of the samples to the analysts, recovery of thesamples at tha completion of the analysis, and discarding of the samples after theappropriate laboratory holding time has expired.

These operations are the responsibility of the Sample Management Group. The precisesteps are itemized below.

4.2.1 Sample Receipt In tha Laboratory

Samples will be received in the laboratory either by commercial carrier, thepostal service, or hand-carried. Personnel of the Sample Management Group signfor the receipt of each shipment of samples, and retain a copy of the shippingdocuments. The personnel receiving the sample shipment will open a sampleshipment checklist, a copy of which is shown in Figure 4-2, at the time ofreceiving tha shipment.

If. for any reason, the shipping container is not expected to be openedimmediately, then the seals on the container must remain intact.

4.2.2 Shipment Inspection

It is expected that a shipment received in the laboratory will be opened andinspected immediately upon receipt Prior to opening the shipping container, thecustody seals will be inspected to assure that no tampering has been done with thesample containers. The state of the custody seals will be noted by the personinspecting the shipment of the sample shipment checklist.

REV.O5/88 «* AR3072I5

CHESTER LABNET[] Houston f] Monroeville [] Neville Island [] Portland

i sample shipment checklistCLIENT:_____________________ DATE SHIPPED:CLIENT CONTACT:______________ DATE RECEIVED:TELEPHONE NO.:_______________ SHIPPED VIA:_CHECKED BY:________________________________

NUMBER OF SHIPPING CONTAINERS (COOLERS. BOXES. ETC.):.CONTAINER ID CUSTODY TAPE

PRESENT?(Y/N)

INTACT?(Y/N)

TEMPERATUREC

NO. OF SAMPLECONTAINERS

#

AGREE WITHCOC? (Y/N)

IRREGULARTTES

SAMPLE ID SUB SAMPLE ID IRREGULARITY

CHECKER SIGNATURE: DATE:

RESOLUTION OF IRREGULARITIES WITH CLIENTCLIENT REPRESENTATIVE: KEYSTONE REPRESENTATIVE:TELEPHONE NO.:WRITTEN FOLLOWUPDECISION:

DATE TIME<Y/N1 DATE

.REV.O5/88

SIGNATUREBlftllDC >!_O

SAMPLE SHIPMENT CHECKLIST

4"7 RR3072I6

After the seals are inspected, the ice chest is placed in a fume hood and opened.The temperature of the int€ or of tha ice chest is measured and recorded. Tomeasure the temperature, the lid is quickly opened and a thermometer is insertedinto the ice chest, and the lid is closed again for five minutes. At the end of fiveminutes, the lid is quickly opened and the temperature read rapidly. Thetemperature is recorded on the sample shipment checklist.

While the ice chest is still in the fume hood, the chain of custody document isremoved from the inside of the lid, and the individual sample containers areremoved from the ice chest. The sample or sub-sample containers are countedand reconciled with the number of such containers indicated on the chain-of-custody. If the number of retrieved sample containers is less than that indicatedon the chain-of-custody, the packing materials inside the ice chest are furtherchecked to make sure that no sample container has Seen accidentally left in theice chest

Each individual sample or sub-sample container is visually inspected todetermine that no breakage, cracking, external corrosion, or leakage hasoccurred. If none have occurred, the individual sample containers may beremoved from the fume hood and placed on a workbench to complete theinspection. If, on the other hand, there is indication that breakage, cracking,corrosion, or leakage has occurred, the inspection of the sample containers willbe completed while the containers are kept in the fume hood.

Tha integrity of the individual sample or sub-sample containers is recorded onthe sample shipment checklist.

4.2.3 Reconciliation with Chain-of-Custody Document '

Once the integrity of tha sample containers has been determined, tha samplecontainers are reconciled against the records on tha chain-of-custody. This isdona by checking tha sample identification on the chain-of-custody and on thasample container label. In addition, tha analyta identifications are checked toensure that they are correct.

REV.O5/83 4-8

Any discrepancy is noted on the chain-of-custody, signed, and dated. The—/ discrepancies are also entered on the sample shipment checklist. At this point,

the sample shipment inspection is complete. The sample shipment checklist issigned and dated by the person performing the inspection. If there are nodiscrepancies, and the shipment is complete as evidenced by the inspection, theshipment of samples is ready to be logged in. If there are discrepancies orinconsistencies, the sample shipment checklist is submitted to the Manager of theSample and Data Management Section, or his designee, and the logging in processis delayed until the discrepancies are resolved.

4.2.4 Resolution of Shipment Irregularities

If any irregularities are noted during the sample shipment inspection, they arerecorded on the sample shipment checklist, and the'checklist is submitted to theManager of the Sample and Data Management Section or his designee. TheManager of the Sample and Data Management Section, or his designee, will contactthe client's representative to determine the fate of the sample shipment. Therecords of the conversation with the client's representative are entered on thesample shipment checklist, including name of contact, time and date of theconversation, and the resolution of the irregularities.

There are several possibilities for the resolution of the irregularities. Theseare:

1. Return the sample shipment to sender2. Destroy the entire shipment of samples3. Log in and process those samples that are intact.

The sample shipment checklist containing the comments regarding resolution ofany irregularities is returned to the Sample Management Group, the personnel ofwhich will act according to the annotated agreement with the client.

*To maintain the custody of the samples, the shipment of samples during thisperiod is either locked up in a secure area or is in view of the SampleManagement Group personnel.

REV.O5/88 4-9 AR3072I8

4.2.5 Sample Log In

Once the sample shipment has been inspected and any irregularities resolved, thesample shipment is ready to be logged in. For laboratory purposes, a singlesample shipment from a specific client constitutes a singla job. The shipmentmay contain ona or many samples, and may have arrived in a single shippingcontainer or in many shipping containers.

For the tog-in process, the Sample Management Group person performing thalogging in needs the field chaln-of-custody and the sample shipment checklist,both with whatever corrections required to be made during tha inspection andresolution steps. Tha log-in process consists of four steps which are detailedbelow:

4.2.5.1 Entry in Master Log

Tha Master Log is a hardbound book in which all jobs received in thalaboratory are chronologically recorded. Tha following information isentered in the Master Log:

1. Job Number2. Data of Receipt3. Date of Logging-in4. Name of Client5. Number of Samples (not sub-samples)8. Due Data7. Completion Data8. Data of Sample Return to Client9. Data of Sample Disposal as Waste

The job number consists of a letter followed by a seven digit number. Thainitial letter code identifies the laboratory (H - Houston, M -Monroevilla, C • California). The four digits following tha latter identifythe year and tha month of the sample shipment logging-in. and the lastthree digits ara chronological within the month. Thus, M8709005 is a

REV.O5/88 4-10

job number issued by the Monroeville Laboratory for the fifth job loggedin during September 1987.

A sample page of the Master Log is shown in Figure 4-3. At the time ofentering the job in the Master Log, the job number is manually writtenon the Field Chain-of-Custody and on the Sample Shipment Checklist Thejob number remains the identification of the job in the laboratory and onthe job records.

4.2.5.2 Job Traveller

In addition to opening an entry in the Master Log, a Job Traveller isissued for every job in the laboratory. The Job Traveller is a computergenerated document that gives all the pertinent details regarding theindividual samples in the job.

For each sample in the job, a unique number is assigned. The uniquenumber consists of the job number followed by three digits, which aresequential within the job. A sub-sample is further identified by a letterfollowing the sample number. Thus, M8709005027C identifies sub-sample C of the 27th sample of job number M8709005.

The sub-sample letter code is used to identify the purpose or thepreservative of the sub-sample. The following codes will be used

A Unpreserved sample for volatiles by GC/MSB Preserved sample for volatiles by GC/MSC Preserved sample for volatiles by GC/MSD Unpreserved sample for volatiles by GCE Preserved sample for volatiles by GCF Unpreserved sample in glass container for organicsG Nitric acid preserved sample in plastic for metalsH Sodium hydroxide preserved sample in glassI Add preserved sample in glass

REV. 05/88 4-11

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REV.O5/88 4*12

AR30722I

On the job traveller, each sample is assigned a unique laboratory number.This number is entered on the traveller, as well as the original sampleidentification off the field chain of custody, the date of sampling, thesample matrix, and the parameters for which the sample or sub-sampleare to be analyzed. In addition, the traveller heading contains informationpertaining to the job as a whole: the client identification, projectcontacts, date of logging in, and due date. The traveller also indicateswhere the sample or sub-sample is stored (refrigerator I.D., shelfnumber, etc.).

A sample of a Job Traveller is shown in Figure 4-4.

4.2.5.3 Sample and Sub-Sample Numbering

When the computerized logging-in process is complete, the operatorentering the information proofs the input and verifies that all theinformation is correct. The complete sample or sub-sample

. identifications are entered on labels. The operator then places the correctlabel on each container of each sample, and verifies once more that theinformation has been correctly recorded.

The labelled sample containers are then placed in the appropriate storagearea as designated on the traveller.

4.2.5.4 Information Distribution and Job Filing

The Job Traveller is the working document for each job. The SampleManagement Group personnel makes a copy of each traveller for eachsection or group in the laboratory, as well as the Data Management Groupand the QA/QC Section. The copies are distributed to the group and sectionmanagers as required. The original traveller is used to open a file for thejob in which the laboratory copy of the field chain-of-custody and thesample shipment checklist are placed. The file is identified by the jobnumber. As the work on the job is completed, the file wilt be used tostore all laboratory records regarding the job.

<~sREV.O5/88 4-13

AR307222

FIGURE 4-4

(Need a LIMS generated dummy traveller)

4'14 AR307223

The file for the job is placed in the laboratory central active job filingsystem.

The sample log-in process is extremely critical for the properfunctioning of the laboratory. " must be performed rapidly andaccurately, so that holding times will not be violated, and so that thecorrect analyses will be performed on the appropriate samples.

4.2.6 Custody Transfer Within the Laboratory

Because the laboratory is considered a secure facility, samples will be consideredas being in the custody of the laboratory from the time that sample receipt isrecorded.

^All samples will be maintained at the locations designated on the traveller untilthe section responsible for the sample preparation for analysis is ready to startwork on the samples. The section representative will then proceed to recover thesamples from their designated storage area. The person retrieving the sampleswill fill in a transfer form, a sample of which is shown in Figure 4-5, andsubmit the form to the personnel of the Sample Management Group, while keepinga copy of the form.

When the sample preparation is completed, and residual samples are returned totheir original storage location as had been indicated on the Job Traveller, thesample preparation group will return the copy of the transfer form to theSample Management Group, indicating on the form which samples, if any, havebeen completely used up. The Sample Management Group will file these formswith the job file.

4.2.7 Sample Disposal

From the laboratory perspective, samples are disposed of when either they arereturned to their origination point (the client) or are eliminated as waste.

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Samples that are returned to their point of origination will be accompanied by achain-of-custody document, and the laboratory will be acting as though it were afield unit. The Sample Management Group will complete a chain-of-custodydocument as described under field custody in Section 4.1 , and ship the samples asdescribed in Section 4.1, unless documented client instructions provideinformation to the laboratory for a different mode of returning the samples.Copies of these documents will be placed in the job file by the SampleManagement Group, and the date of sample disposal will be entered in the MasterLog.

Samples that are being disposed of as waste will be recorded by the SampleManagement Group on a special form, a sample of which is shown in Figure 4-6.When the disposal is complete, the person disposing the samples will sign anddate the form, and enter the date in the Master Log and the form in the job file.

Before samples are disposed of as waste, the Sample Management personnel willreview the analytical data and the history of the samples, so that appropriateprecautions may be taken. Those samples which were found to be innocuous willDe disposed of either as ordinary trash or, if aqueous, by pouring down the drain.

In disposing the samples, as waste, great care must be exercised. Special drumswill be maintained for such disposal and the drums will be clearly marked toidentify the type of waste that may be placed in each drum. For aqueous wastestwo drums will be maintained, the first for acidic waste and the second foralkaline waste. These two types of waste must not be mixed because the acid-basereaction may be too violent, and because the water samples may contain materialsthat are incompatible with the prevailing pH of the drum (for example, cyanidewaste cannot be added to an acid drum because of the generation of hydrocyanicacid).

Two additional drums wilt be maintained for disposal of organic liquid waste andfor disposal of solid samples in which hazardous materials were identified.Samples of solvents, or laboratory waste solvents will be placed 1n the organicliquid waste drum. Solid samples that have been found to contain hazardous

REV.O.5/88 «•" RR307226

SAMPLE DISPOSAL RECORD

TRAVELLER NO. ______ DISPOSAL DATE

SAMPLE ID SAMPLEMATRIX

HAZARD

FLAMMABLE

CORROSIVEACID

CORROSIVEBASE

REACTIVE

3xo

DISPOSALMUNICIPALSEWER

MUNICIPALWASTE

Osocs»

•) IDENTIFY DRUM DISPOSED BY ___

FIGURE 4-6

2/88° *-i» AR307227

materials, except for strong oxidizing agents, will be placed in the drum for solidwaste. Wipes of spills and contaminated sample containers and laboratory warethat are to be disposed, as well as other laboratory waste that may be consideredhazardous (such as used syringes) will be placed in the solid waste drum.

For each drum, a log will be maintained identifying in general terms the type andquantity of material that have been placed in the drum. This log will facilitatepreparing the manifest for shipping the waste for ultimate disposal.

The drums will be disposed through a contracted firm dealing in the disposal ofhazardous waste no less frequently than once per month. While the waste iscollected in the laboratory, a special area will be set aside for the storage of thedrums.

t4.2.8 Custody Transfer for Prepared Samples

When the sample preparation group completes the preparation of a batch of, samples, and if the prepared samples (extracts, digests, distillates, etc.) are to

be transferred to the analytical group, the sample preparation group completes atransfer form, shown in Rgure 4-7. The transfer form is transmitted with theprepared samples to the analytical group, and a copy of the form is given to theSample Management Group to be placed in the job file.

REV.O5/88 *-16* rx ~

^307228

PREPARED SAMPLE CUSTODY TRANSFER

QC BATCH ID ___________ DATE OF TRANSFERDIGESTATES: ICPEXTRACTS: B/N/A ____ GFAA

OTHER1DISTILLATES: CN

TPH ___ p ——OTHER* —— OTHER"

TRAVELLERNUMBER

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REV.O FIGURE 4-75/88 4-20

307229

5.0 ANALYTICAL PROCEDURES

In order to produce meaningful results, both sampling and analytical procedures must besound and complimentary to each other. While close coordination of activities betweenthe laboratory and field services is highly advisable in order to produce a high qualityproduct, the laboratory services will frequently involve analyses of samples collectedthrough organizations other than Chester. Thus, the application of strict proceduresregarding the transfer of samples from the field to the. laboratory is not always possible.

5.1 COORDINATION OF ACTIVITIES

Analytical services are requested through several sources. For projects of long durationor of such magnitude as to warrant it, an analytical project manager is assigned. Theproject manager acts as liaison between the client and the laboratory on all matterspertaining to the project. In other cases, requests for analytical services originate withthe laboratory sates representatives, sample control personnel, or other key technicalpersons in the laboratory. Regardless of the means through which a request has beenmade, the person receiving the request will enter a description of the requested work onan Analytical Request Form, shown in Figure 5-1, and tha information will be enteredinto the Laboratory Information System as proposed work. When the proposed projectbecomes a definite task for the laboratory, the Sample Management Group will activatethe project and distribute the information together with tha anticipated schedule, so thatthe laboratory sections that will be involved in the analysis are aware of the upcomingwork.

All further coordination and scheduling of the work will be issued through the SampleManagement Group.

5.2 PREPARATION OF SAMPLE CONTAINERS

For clients and projects that require the laboratory to supply with containers forsamples, the Sample Control Group will be responsible for preparing the containers,labelling them, and shipping them to the client. It is the responsibility of the projectmanagers to inform the Sample Control Group of the need for containers. Such

S'° 5., flR307230

ANALYTICAL REQUEST FORM

Request Taken By: Request Date:

Client: Project Manager:Client Contact: Telephone:Address:

Start Date:

Telephone:

NO. OFSAMPLES

MATRIX ANALYTICAL PARAMETERSf

TURNAROUNDTIME, DAYS

APPLICATION: QNPDES QSDWA Q RCRA Q Superfund Q OtherSpecial Instructions:

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FIGURE 5-1REV.O5/88 5^DOftir>^.

notification must be received by the Sample Control Group at least three working daysprior to the time for which the sample containers are required.

For aqueous field samples, new pre-cieaned sample bottles with Teflon lined screw capswill be used. The containers will be prepared with the appropriate preservatives, andwill be labelled with information regarding the anatytes that are to be determined on thesample.

For solid samples, a variety of containers may be used. For soils, brass sleeves arefrequently employed. The brass sleeves will be recycled after thorough cleaning andbaking in the laboratory. When the samples are to be collected in polyethylene or glass,appropriate new and pre-cleaned containers will be used.

Table 4-1 lists the appropriate containers and preservatives 'for aqueous samples.

5.3 INSTRUMENT MAINTENANCE

Maintenance of the instruments in the laboratory in good working order is of paramountimportance. Instrument maintenance consists of two major aspects, the first is routinepreventive maintenance, and the second is repair due to malfunction.

For all instruments, the manufacturer's recommended schedule of preventivemaintenance will be closely adhered to. It is the responsibility of the Section Manager ineach section of the laboratory to assure that the time required for preventivemaintenance is set aside and planned on. Records of this maintenance will be kept in theinstrument log, including information concerning replacement parts, readjustments,and calibrations, which may affect the performance of tha instrument relative to itsperformance just prior to maintenance. Verification of instrument response, andrecalibration if necessary, must be performed immediately after the completion of suchmaintenance, before any sample analysis is taken up.

Instrument repair will bo performed as necessary either by a service call or throughlaboratory personnel. It is the responsibility of the analyst to verify that theinstruments are performing within preestablished criteria, and investigate and cause tocorrect any malfunctions. Instrument malfunction cannot always be detected throughroutine use; the running of verification samples throughout the course of an analyticalREV.O

5/88 M AR307232

run will be used to further certify that the instrumental response and behavior waswithin accepted norm.

Should an instrument be serviced, the analyst will verify that the instrument isperforming within the required acceptance criteria before analyzing any samples. If theinstrument after maintenance is not within these criteria, the instrument will berecalibrated.

Records of all instrument maintenance and repair will be kept in the instrument tog.These records will Include information regarding the cause of the malfunction, thecorrective action that has been taken, record of verification of performance after themalfunction has been corrected, and identification of the samples that may have beenaffected by the malfunction. The Section Manager, or his designee, will be responsible toassure that the maintenance fogs are properly kept and filled, and that notification ofinvalid data is given to the Data Management Group, if the data from the invalid runs hasalready been released by the Section. Figure 5-2 shows the form that is used to notifythe Data Management Group that certain data are invalid.

5.4 PREPARATION OF STANDARDS

All analytical methods at some point must be validated by the use of calibrationstandards. A calibration standard is made by the appropriate dilution of .a puresubstance, the purity of which is traceable to NBS standard. Because of the highsensitivity of many analytical instruments, the calibration standard Is an extremelydilute version of the pure compound. Because of the high dilution required, in order tobe within the linear range of the instrument, the preparation of the calibration standardis frequently made by serial dilution rather than in a single step. In order to providestandard solutions at sufficiently tow concentration, a miniscule amount of the puresubstance will be required, the measurement of which is subject to extreme error.Thus, it is preferable to deal with potential dilution errors, rather than with the largeerror associated with the measurement of a very small amount of the pure substance.

*•The initial oure standard is usually obtained either as a pure material or already insolution prepared as a certified solution of a given concentration of the pure compound orcompounds. In preparing the stock solution of the calibration standard, great care mustbe exercised in measuring weights and volumes as accurately as possible, since all the

INVALID DATA NOTIFICATION

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FIGURE 5-2REV.O5/88

AR307231*

analyses following the calibration will be based on the accuracy of the calibration, andthe accuracy of the ultimate data cannot be any better than that of the calibration curve.Table 5-1 summarizes the valid lifetime of primary and secondary standards used inmany tests. These lifetimes should be taken as a guide only. It is the analyst'sresponsibility to assure that all standards used by him are within the standard solutionholding time, and to prepare fresh standard solutions whenever necessary. In preparingworking solutions, or using working solutions, the analyst must check for signs ofdeterioration, such as the formation of cloudiness and precipitation, discoloration. Thestandard must also be periodically compared with previous runs of standards, and withindependently prepared standards to assure that response factors fall within anhistorically accepted range.

TABLE 5-1STANDARDS AND SOLUTIONS HOLDIN& TIMES

MATERIAL _________HOLDING TIME__________t

PURE STOCK WORKINGCOMPOUND SOLUTION SOLUTION

Volatile organic compoundsfor GC or GC/MS analysis 1 Yr @ -10°C 2 Mo @ -10°C 1 Wk @ -10°C

Semrvolatile organic compoundsfor GC or GC/MS analysis 1Yr@4°C lYr@4°C 6Mo@-io°C

Semivolatile organic compoundsfor HPLC analysis 1 Yr @ 4°C 1 Yr @ 4°C 6 Mo @ 4°C

Pesticides (Cl, P. N) and herbicides 1 Yr @ 4°C 1 Yr @ 4°C 6 Mo @ -10°C

Polychlorinated dioxins and furans 1 Yr @ 4°C 1 Yr <g> 4°C 6 Mo @ 4°CMetals for ICP analysis Indef. @ RT 1 Yr @ RT 6 Mo @ RT

Metals for GFAA analysis Indef. @RT 1Yr@RT 6Mo@RT

Mercury Indef. @RT 6Mo@RT 1D@RT

Hexavalent chromium Indef. @RT 1Yr@RT 1YJ@RT

REV.Os/88 s-e AR307235

For anions and other parameters, the holding times of standard solutions should bechecked in the appropriate method.

All standards and standard solutions of organic compounds will be maintained in glasscontainers, and will be protected from light. The position of the meniscus in eachcontainer wiil be marked after each time that the container is opened, so that changes dueto evaporation can be detected.

Metals working solutions and stock solutions will be kept in polyethylene containers atroom temperature. The position of the meniscus will be marked each time a solution isused to insure that concentration changes due to evaporation are detected. Before usingany standard solution, the analyst will examine it for signs of precipitation and changesin color. If precipitation has occurred, the solution will be discarded and a new standardprepared. Discoloration frequently is only a warning sign, but will not affect theresults. If a solution is discolored, the analyst will compare the results withhistorically established response factors, to assure that the solution is still within theoperating range of tha method, and within experimental error of its originalconcentration.

The preparation of standards is very exacting. To facilitate the operation of preparingstandards, a separate area Is set in the laboratory equipped with a small hood andanalytical balance. A freezer in the same room is used to store all primary standards.and no other samples or extracts. In this fashion, the contamination of standards bysamples, and vice versa, is minimized.

For each stock standard solution that is prepared, accurate records will be kept in aspecial logbook used only for the maintenance of standards data. The followinginformation will be entered In the logbook at the time of stock standard preparation:

a. Date of preparationb. Application for which the standard is being prepared (i.e.,

identification of the method)c. For each compound, the supplier of the primary standard, the

batch number, and the amount taken

d The solvent identification (compound, supplier, tatch number)

REV.O

5/88 5-BR307236

e. The final volume of the stock standard ;

f. The identification number assigned to the stock standardpreparation

g. The name of the analyst preparing the standard

A typical page of the logbook is shown in Figure 5-3.

the identification number that is assigned to the stock standard is alphanumericconsisting of the date preparation and a method code. Thus. 090587MS625 will be theidentification number of a standard prepared for semivolatiles by GC/MS on September5, 1987.

In preparing the diluted working standards, it is the analyst's responsibility to makesure that the stock standard is of valid vintage. The preparation of all working standardsis also recorded in the logbook. The following information is recorded in the logbook:

a. Date of preparationb. Identification number of the stock standard solutionc. Volume of stock standard solution takend Final volume of the diluted standard solutione. Concentration of each parameter in the diluted standardf. Identification number for the diluted standardg. Name of the analyst preparing the diluted standards.

The working standards will also be identified by an alphanumeric system consisting ofdate, method, and nominal concentration. Thus, 090587MS625C10 would be theidentification of a working standard prepared on September 5, 1987. for semivolatilesby GC/MS, and in which the nominal concentration of the components is 10 ng/uL in theworking solution. The ppb or ppm designation is intentionally not employed because itusually refers to the concentration of the compounds in water. Since our activitiesinvolve identification and quantitation in all matrices, it is preferred to identify theconcentration in the calibration solution per se.

The working standards for organic analysis will be stored in a freezer in the work area.No other samples or extracts will be stored in the same freezer. The working standardsfor metals will be stored in the work area in a cabinet or shelf designated for standardsonly. These need not be refrigerated. For other parameters, the working standards will

REV-0 mn*~s/88 s-8 AR307237

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1 i ' - • # * • ' •be maintained in either a' refrigerator or at room temperature in the work area, but atspecifically designated cabinets or shelves, where no other materials are being stored.

5.5 DETERMINATION OF DETECTION AND QUANTITATIONLIMITS

For many projects, knowledge of detection limits is essential in order to be able tobracket analytical results that are obtained. Several such limits exist, and differentexperts define these limits differently. For this reason, the definition and determinationby which Chester abides is given below.

5.5.1 Instrument Detection Limit

In simple terms, the instrument detection limit is the smallest quantity ofmaterial that the instrument can detect. It has been defined in the past as acertain value of the signal-to-noise ratio. Many modem instruments, however,are designed to self compensate for noise, so that the measurement of the signal-to-noise ratio is not a simple matter.

For the purposes of work at the Chester Laboratories, the instrument detectionlimit is d Ined as three times the standard deviation from the mean of sevenreplicate measurements of a tow concentration standard that produces a. definite,measurable signal. The signal may be an area count, a peak height en absorbancereading, or electric measures (such as voltage, current, resistance). The natureof the signal is dictated by the instrument and detector that are used. Theinstrument detection limit is calculated from the following equation:

Where, IDL « Instrument detection limit, in weight units (ng, mg)for those parameters where the signal depends on anabsolute quantity (such as chromatographic methods),and in concentration units for those parameters thatare concentration dependent

S « Standard deviation of the seven replicate readings, inunits of the reading (i.e., auia. count, peak height, etc.)

REV.O5/88 5-10

RF •» Response factor, in units of signal reading/unitweight, or concentration, depending upon the units usedfor IDL.

The calculation of the response factor is shown in Section 5.8, where calibrationprocedures are discussed. The calculation of the standard deviation is shownbelow.

V- nS(x|ii!_~ D

where, xj - The value of the i'th reading of the set of replicatesXm - The mean value of the replicatesn * The number of replicate measurements

The mean, Xm. is determined as follows:

In order for the results to be useful, the standard chosen to obtain the detectionlimit should be such that the mean of its readings. Xm, is slightly greater than3S. This may require some trial and error initially when a new instrument isinstalled.

The instrument detection limit will be determined on a quarterly basis, andwhenever the instrument has undergone extensive maintenance. Records ofperforming the determination of the instrument detection limit will be kept inthe instrument tog, and the values of the instrument detection limit will beupdated in the working SOP'S at each time that tha instrument detection limitsare determined.

5.5.2 Method Detection Limit

The method detection limit is obtained in a manner very similar to that of theinstrument detection limit. The principal difference is that in determining the

REV.O AR3072l*05/83 5-11

method detection limit (MDL), the analytes are subjected to the entire analyticalprotocol for the specific method that is being employed. Ideally, the methoddetection limit should be determined for every matrix that is being analyzed.Unfortunately, obtaining reproducible, well characterized matrices for mediaother than water is not yet feasible. Hence, method detection limits will bedetermined for water only.

To determine the method detection limit, seven replicates of laboratory purewater are each spiked with a known amount of the analyte. The amount that isbeing added is the same for all seven replicates, and should be 2 - 3 timesgreater than the previously determined instrument detection limit. The sevenreplicates are subjected to the same analytical procedures as a sample would be,and the concentrations of the analytes of interest are measured. The methoddetection limit, as was the instrument detection limit,' is defined as three timesthe standard deviation of the seven readings. The calculation of the methoddetection limit should be done in units of weight of the analyte. In this fashion,such variables as injection volume in chromatographic techniques or pathlengthin spectrophotometric techniques are eliminated.

The equations that apply to the calculations of method detection limits areidentical to those used for the instrument detection limit

where MDL - Method detection limit, in units of weight (ng, ug) forthose methods that depend upon an absolute quantity,and in concentration units for those methods thatdepend upon concentration

Sm « The standard deviation of the seven readings from themean, in units of signal size (area, height, etc.)

RF « The response factor of the instrument to the analyte,in units of signal size/unit weight or concentration,depending upon the MDL units.

The standard deviation is determined just as before from the equation:

REV.O5/88 5-12AR3072U

where yi =• the instrumental reading for the i'th sample that hasgone through the entire preparation procedure

Ym * Tha mean value of the replicate readings

n - Tha number of replicates that have been run.

The mean value is determined as follows:

i-1

As a minimum, tha method detection limit will be determined for all analytesassociated with the method on a semiannual basis. It will be determinedquarterly for a selected list of analytes. which are normally used in spikingsamples. During the quarterly determinations, the method detection limits foranalytes that are not specifically analyzed at that time will ba determined byapplying established ratios to tha anaiytes that are normally used for spiking.

The quarterly determination of method detection limits will also ba performedwhenever tha instrument undergoes major repair or modification, if thameasurement of the instrument detection limit shows a significant departurefrom the previously determined instrument detection limit. If tha instrumentdetection limit has remained substantially unchanged after tha repair or themodification, there is no need to run the method detection limit again.

Tha method detection limits must also be determined whenever tha samplepreparation mode is modified.

5.5.3 Quantitation Limits . -

Tha quantitation limit is determined at the same time as tha method detectionlimit and from tha same runs. The quantitation limit (QL) is defined as five

times the standard deviation that has been measured in determining the methoddetection limit. Thus,

RFwhere the symbols have the same meaning as before.

5.5.4 Conversion of Detection Limits to Minimum DetectableConcentration

The conversion of the detection limit (MDL and QL) to a minimum detectableconcentration in a sample is done as follows:

where DLS * Detection limit in sample in units of weight per unitweight or per unit volume

DL B Either the MDL or the QL as defined in the precedingsections

vj « Volume of prepared sample taken for analysis (such asthe volume of extract injected into a GC), in mL

v j « The volume of the prepared sample (such as the finalvolume of an extract), in mL

S « The sample size that was taken to produce the preparedsample of volume vj. Sample size is normallymeasured In liters for aqueous samples and in grams,dry weight, for solid samples.

5.5.5 Documentation of Detection Limits

Whenever instrument detection limits, method detection limits, and quantitationlimits are determined, the results will be copied to the QA/QC Section. Theresults must identify the type of detection limits, and include both the value interms of weight (absolute quantity) and concentration. In reporting theconcentration units, standard sample sizes and aliquots will be reported.

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5.5.8 Application of Limits In Data ReportingJ

In reporting data, tha following rulas pertaining to detection limits shall apply:

a. Experimental data which are equal to or greater than the value ofDLS that has been calculated on the basis of QL will ba reportedwith the concentrations found, without any qualifiers.

b. Experimental data which are equal to or greater than the value of DLS,calculated on the basis of MDL, but are less than tha value ofDLS, calculated on the basis of QL. may ba reported, with thequalifier that tha concentrations are estimated below detectionlimits.

c. Experimental results below tha value of DLS. calculated on thebasis of the MDL. will ba reported as not detected at the DLSvalue.

*Exceptions to these rulas will ba applied only for contracts and projects whichspecify their detection limits, and whosa detection limits exceed the value of QLAlso exceptions will ba applied when a prepared sample requires very highdilution in order to have tha analyte of tha highest concentration within thalinear range of tha method. In the latter case, tha client will be so notified, sothat decisions can ba reached if tha client needs additional dilutions measured

5.6 INSTRUMENT AND EQUIPMENT CALIBRATION

Instrument and equipment calibration must ba rigorously and routinely performed inorder to provide reasonable assurance that the data generated are valid and acceptable.

Two principal types of calibration are performed. Tha first is an initial calibration.which consist of determining tha linear range of tha instrument and its response factor.Tha second is a verification calibration, which serves, during tha course of runningsamples, to ascertain that tha instrument calibration has not drifted unacceptably. Thafrequencies of performing tha different types of calibrations are shown in Table 5-2.

5.6.1 Initial Calibration

All instrumental methods of analysis are subjected to an initial calibration,consisting of tha measurements of responses to five different standard solutions

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i of the analytes of interest. The standard solution of the lowest concentrationshould have a concentration of the analytes of interest approximately 2 - 3 timesthe concentration that corresponds to the Instrument Detection Limit; and thestandard solution of the highest concentration should have a concentration of theanalytes of interest at or near the upper end of the linear range of the method.

In performing the analyses of the standards to determine the response factor andthe linear range, the standard solution is prepared as mentioned in Section 5.4,and surrogates and internal standards are added to it when appropriate. Theidentification of the working standard solution and the date of performing the runare entered on the records of the run by the analyst.

When the five runs are completed, the responses are. fitted to a straight line ofthe form

y « ax -t-b

Where y - the measured responsex « the known amount of the analytea • the response factorb - the y-intercept.

In addition to determining the values of a and b, the correlation coefficient isdetermined. The latter is a measure of how closely the five points were to thestraight line. The correlation coefficient Is determined from the followingequation:

1.1 i-1 U1n n n/ n

-v/ n£V i-1

where r • Correlation coefficientxi « The known amount of the analyte in the ith standard runyi. The measured response to the to the i'th standardn - The number of standards run to obtain the calibration curve.

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In order for tha calibration curve to ba valid, tha correlation coefficient must be0.995 or higher, and tha ratio b/a must ba no greater than tha method detectionlimit (MDL). If the correlation coefficient is not mat, it usually implies thateither tha lowest or the highest concentration of standard is outside tha linearrange. To correct for this, tha analyst should rerun the highest standard, andalso run a high standard somewhat more dilute than tha initially used highestconcentration. Similarly, tha analyst should examine tha effect of increasingslightly the concentration of tha lowest standard.

If the ratio b/a criterion is not mat, tha problem may be with contamination inthe system or change in tha noise level of the instrument. To correct for this, thainstrument detection limit should ba first checked. If it has in fact changed, tharatio should ba compared to tha newly determined noise level, in order to sea ifthe criterion is met.

While, as much as possible, certifiable standards ara used in tha preparation ofsolutions for calibration, it is always possible that tha manufacturer has made amistake. To circumvent tha possibility of erring dua to a mistake in thamanufactured primary standard, a check sample will ba analyzed whenever aninitial calibration curve is constructed. The check sample will consist of asolution of tha analytes of interest and at known concentration, but obtained andprepared by a different source than tha manufacturer of tha calibrationstandards. When the anaryta concentrations in the check sample are calculated,they should differ by no mora than 20% from tha known concentration. If thadiscrepancy is greater than 20%, a determination of the source of inaccuracywill ba performed.

Once tha initial calibration curve has been determined and verified, a table isprepared with tha response factors for all tha analytes. Tha table also includesthe identifications of all tha standards used In generating tha data, and the data ofrunning tha initial calibration. A copy of tha table is submitted by the analyst totha QA/QC Section, and another copy is maintained in tha work area for ready

»reference on a dairy basis.

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5.6.2 Continuing Calibration

Continuing calibrations, sometimes also called verification calibrations, serve toinsure that the instrument, during the course of running samples, is remainingsufficiently stable so that the response factor calculated in the initial calibrationremains valid.

In performing a continuing calibration, the analyst analyzes a midrange standard,containing all the analytes of interest and internal standards and surrogatecompounds if applicable. The response factor is determined for each analyte bydividing the signal by the known concentration of the anafyte. If the responsefactor is within 10% of the originally determined response factor, theinstrument is considered to be within calibration, and analysis may continuewithout performing the initial calibration procedure again. If the responsefactor is determined to be outside the acceptance range, the instrument will berecalibrated by using the initial calibration process. Samples that have beenanalyzed since the last acceptable calibration will also require to be reanalyzed,after the instrument has been recalibrated.

In recording the information on continuing calibrations, the analyst will enterthe identification of the initial calibration to which the continuing calibrationrefers back, and a list of the samples that have been analyzed since the previousacceptable continuing calibration. A copy of this information will be submitted tothe QA/QC Section so that the data associated with the calibration can be validated.Another copy or copies will be submitted to the Data Management Section forInclusion in the file of the project from which samples have been analyzed whilethe specific continuing calibration was in force.

At no time should the response factor be corrected on the basis of the continuingcalibration. Until such time as it is necessary to reestablish the initialcalibration, the response factors determined in the initial calibration will beadhered to.

AR3072II7

5.6.3 Calibration Frequency

Instruments have widely variable stabilities, requiring variable frequencies ofcalibration. Table 5-2 summarizes tha frequancies of such calibrations. Itshould ba emphasized that these frequencies are based on instruments that areperforming normally. It is or should ba obvious that after change in instrumentparameters or after repair, tha initial calibration must ba repeated, and thacycle started over again. Thus, tha frequencies included in tha table areminimum requirements.

TABLE 5-2CALIBRATIONS FREQUENCIES

INSTRUMENT APPLICATION INITIAL CALIBRATION CONTINUING CALIBRATION*

GC/MS Volatiles Once per Every twelve hours and at theWeek end of a sequence of runs, if the

instrument is about to ba idle.GC/MS Sami- Cnca par Every twelve hours and at tha

Volatites Week end of a sequence of runs, if theinstrument is about to ba idle.

GC Volatiles Every Three After every eight runs, and atby Purge- Days tha end of a sequence of runs.and-Trap

GD Extracts Every Three After every eight runs, and atDays tha end of a sequence of runs.

HPLC Extracts Every threa After every eight runs, and atDays tha end of a sequence of runs.

1C Solutions Every Threa After every eight runs, and atDays the end of a sequence of runs.

Autoanalyzer Solutions Daily After every tan runs, and at theend of a sequence of runs.

ICP Digests Daily After every ten runs, and at theend of a sequence of runs.

M Digests Daily After every ten runs, and at theend of a Sequence of runs.

Mercury Digests DaUy After every ten runs, and at theAnalyzer . end of a sequence of runs.

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TABLE 5-2

CALIBRATIONS FREQUENCIES(CONTINUED)

INSTRUMENT APPLICATION INITIAL CALIBRATION CONTINUING CALIBRATION

TOC Analyzer Solutions Daily After every eight runs, and atthe end of a sequence of runs.

TOX Analyzer Solutions Daily After every eight runs, and atthe end of a sequence of runs.

IR Solutions for Daily Every ten runs, and at the endO&G or TPH of a sequence of runs.

UV/Vis Solutions Daily Every ten runs, and at the endSpectrophotometer of a sequence of runs.Fluorometer Solutions Daily * Every ten runs, and at the end

of a sequence of runs.

pH Meter Aqueous Daily1 Every ten runs, and at the endSolutions of a sequence of runs.

Analytical Solids Annual2 Daily2\ / Balance

Thermometers Temperature Quarterly3 Not applicableMeasurement

1) pH calibration requires the use of only three standards.

2) Analytical balances are calibrated and serviced annually by representatives of themanufacturer.Their calibration is checked daily before any weighings are done againsta certified class S weight. Deviations from the true weight are recorded and applied toweighings when appropriate.

3) Thermometers are calibrated quarterly against an NBS certified thermometer, and anyrequired corrections are applied to measurements.

5.7 ANALYTICAL METHODS

Whenever possible, the analytical methods that will be employed are either EPA, NIOSH,AOAC, or ASTM. The abbreviated methods are included in the Standard OperatingProcedures, and complete copies of the methods are maintained in each laboratory. Theywill not be reproduced here.

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f . 5.8 ANALYSIS OF QUALITY CONTROL SAMPLESV—/

Routine quality control samples are analyzed to assure that the operation is withincontrol as established for the laboratory on the basis of historical data. The routinequality control consists of blanks, spiked blanks, spiked sample, duplicate sample, andexternal check sample analyses. These are discussed separately in the followingsections.

5.8.1 Blanks

Four types of blanks may be associated with any batch of samples. These are:reagent blank, method blank, trip blank, and field blank. The latter two typesare considered by the laboratory as ordinary samples, and are not therefore panof the internal laboratory QC, although they are very much part of the programQC. Thus, trip and field blanks will not be discussed here.

5.8.1.1 Reagent Blank

Reagent blanks are set aside whenever the reagents are used forpreparation of samples. The reagent blank is the reagent or group ofreagents that is normally used for sample preparation, without goingthrough any of the preparation steps. This reagent blank is normally notanalyzed, unless the method blank, discussed in Section 5.8.1.2, showsthe presence of contamination which may have arisen from the reagents.The reagent blank will be labelled with the QC batch identification,followed by the letter R. It will be set aside until all the samples of the QCbatch have been analyzed. At that point, if the method blank wasacceptable, the reagent blank may be discarded.

5.8.1.2 Method Blank

The method blank is a preparation carried through the entire preparatorysteps, except that the reagents do not come in contact with a sample.Rather, laboratory reagent water is used in lieu of a real sample. Ideally,

i. the method blank would be prepared using a matrix that is similar to the

5*8 .rs~5-21 AR307250

matrix of tha samples that are being prepared. Since a reference matrixv ^is not available for matrices other than water, water is the only matrix

used as a method blank.

In preparing tha method blank, water is spiked with surrogates andinternal standards if appropriate for tha method, and tha water sample iscarried through tha entire analytical procedure. The method blank isprepared with every batch of samples that is being prepared at the sametime, provided tha batch is no greater than twenty samples. For batcheswhich are greater than twenty samples, a method blank will be preparedfor every sub-batch of twenty samples. In addition, a method blank isprepared whenever the lot number of any of tha reagents is changed. Thepreparation log will then indicate which samples are associated with thenew lot number of reagents.

Tha method blank is analyzed before any samples are analyzed, and thadata of tha analysis are reviewed. If no analytes are found above thamethod detection limit, analyses of tha prepared samples may baundertaken. If analytes are found above tha method detection limit, butbelow tha quantitation limit, the associated prepared samples may baanalyzed, but tha results will ba corrected by the blank.

If analytes are found above tha quantitation limit, analyses of thaassociated samples will not ba undertaken until the contamination sourceis identified and isolated. At this stage tha reagent blank will ba analyzed.If it is found that tha reagent blank shows the contamination, tha sampleswill ba reprepared using a new lot of reagents.

5.8.2 Spiked Blank

The spiked blank, or laboratory control standard, serves as a measure ofaccuracy of the analytical procedure in tha laboratory. The. spiked blank isprepared by adding prescribed amounts of specific analytes to laboratory reagentwater, prior to preparation of the water for analysis. For inorganic parameters,

SS'° 5-22 AR30725I

a spiked blank is prepared for each batch of twenty or fewer samples that areprepared at the same time. Water is spiked for every analyte of interest, for theinorganic parameters.

For organic parameters, a spiked blank is prepared for every batch of samplesthat is subjected to sample preparation at the same time. The spike contains onlyselected anatytes, which are specified in the pertinent methods of analysis in theStandard Operating Procedures.

Preparation of the spiking mixture is done in the same manner as thepreparation of standard solutions for calibration. The spiking mixture is thenassigned an identifying code, which is recorded at the time of preparing thespiked blank.

The spiked blank is carried through the entire analytical procedure, and theconcentrations of the spiked analytes determined. These values are accumulatedby the QA/QC Section to update acceptance criteria and to validate a set of runs.The spiked blank forms the backbone of the determination of the reprodudbilityof data in the laboratory, since it is based on a well-characterized matrix(water) and is designed to be essentially free of matrix effects. If the spikedblank does not meet the established acceptance criteria, it is assumed that samplepreparation or analysis have been faulty, and the batch of samples associatedwith the spiked blank will be reprepared and reanalyzed.

5.8.3 Sofked Sample

Spiked samples serve to identify if the sample matrix provides certain effectswhich preclude the ability to recover analytes through the prescribed method.Thus, the spiked sample is used only to determine matrix effects.

One sample per batch of twenty or fewer samples, of the same apparent matrix,will be spiked with a spiking solution, in the same manner as the spiked blank.The spiked sample will be processed through the analytical scheme, and therecovery of the spiked anatytes will be determined.

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In utilizing tha information, great care should be taken because deviations fromacceptability may ba due to procedure or to matrix effects. Generally, if thespiked blank associated with tha batch exhibits acceptable recoveries, it isassumed that tha sample preparation and analysis have been performed correctly.It is possible, however, that for some reason tha specific spiked sample has beenhandled differently. Hence, a repeat preparation will ba used to demonstrate iftha analysis or preparation has been faulty. If tha repeat analysis shows thasame anomaly, it will ba assumed that some matrix effects exist which preventthe sample from behaving in the expected manner.

Since sample spiking is performed before the sample is initially analyzed, it ispossible that for some parameters tha innate level in tha sample is so high thattha spiked amount is insignificant Under those circumstances, tha anaryta spikerecovery will not ba calculated, but analysis of a spiked sample will not berepeated.

In selecting a sample for spiking, every effort will ba made to choose a fieldsample, and not one of tha field or trip blanks. This can be accomplished only ifthe identity of the blanks b known in advance. If tha samples are submittedentirely as blind samples, then tha selection of the sample to ba spiked will barandom.

5.8.4 Sample Duplicate

Sample duplicates are run to assess precision of tha laboratory work. Onesample in a batch of twenty or fewer samples, of tha same apparent matrix, isprepared and analyzed in duplicate.

Tha purpose of this analysis is to obtain data on the precision of tha analyticalprocedures that are being followed. Clearly, duplicate analyses will provideprecision data only for anatytes detected in tha samples. Thus, development ofhistorical background for some less commonly found analytes may requireconsiderable time.

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As in the case of the spiked sample analysis, the choice of sample for duplicateanalysis will be limited to actual field samples, excluding blanks, unless theidentity of the blanks is not known, in which case the selection will be random.

If the results of the duplicate analyses are not within accepted criteria, theanalysis of the batch of samples with which the duplicate samples have beenassociated will be repeated.

5.8.5 External Quality Control Audit

An external quality control audit will be performed periodically by submittingfor analysis known standard materials from a source other than that from whichthe calibration standards are prepared. These quality control audit samples willbe submitted for analysis by the QA/QC Section, and (hey will be analyzed by thesame procedures as are used for the analyses of samples.

The external quality control audit will be performed on a quarterly basis. Ifthere are projects in the laboratory which have these audit samples submitted bythe project, and where the results are made known to the laboratory, then theQA/QC Section wilt not submit the external quality control audit samples forthose parameters which are included in the project audit samples.

5.8.6 Record Keeping en Analysis of QC Samples

The results of the analyses of the QC samples may pertain to more than oneproject, since the sample preparation area batches samples from potentiallyseveral sources to provide for efficient operation. Hence, the retrieval of the QCdata may be necessary for several different projects. The QC data, however, isidentified by the batching identification provided upon the preparation of thesamples. Hence, the retrieval of the data can be readily achieved by identificationof the preparation batch number.

For every batch of samples, the identification of the batch will be entered at thepreparation stage on the appropriate forms. Sufficient number of copies of theforms wilt be made to file with every project associated with the batch. The

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5/88 ** AR307251*

results of tha analysis of tha QC samples will ba filed sequentially by the QC batch "number and will ba retrieved through tha batch number system whenever it isnecessary to retrieve these data.

On a routine basis, tha QC approval of an analyzed batch will ba based on theacceptance of tha QC samples associated with tha batch. Once determined by theQC Department to ba within acceptable limits, tha entire batch of samples will bereleased and tha analytical data for each sample recorded with the appropriateproject.

5.9 USE OF SURROGATES

Tha use of surrogates in organic analysis serves as an .additional measure of theacceptability of tha results. The significant advantage of tha use of surrogates is inmeasuring recovery against an historically established acceptance range in thaperformance of each analysis. Thus, tha data do not depend solely on tha spiked blank toassess tha quality of each run.

Surrogates are compounds that ara expected to behava analytically in a mannar similarto tha target analytes. Tha surrogates are added into tha sample before tha preparationstage is initiated, and their recovery is a measure of tha efficiency of tha extraction. Thafollowing surrogates hava been used at the Monroeviila Laboratory and are recommendedfor usa throughout tha laboratory system.

TABLE 5-3SURROGATE COMPOUNDS AND ACCEPTABLE RECOVERIES

EPA METHOD COMPOUND RECOVERY RANGE

501/601/8010 Bromochloromethane 70 - 1202-Bromo-l-chloropropana 70 - 1201,4-Dichlorobutane 70 - 120

502/602/8020 Benzotrifluorida . 80 - 120

604/8040 2-Fluorophanol 21-1002.4.6-Tribromophanol . 10 - 123

5.26 AR307255

TABLE 5-3(Continued)

SURROGATE COMPOUNDS AND ACCEPTABLE RECOVERIES

EPA METHOD COMPOUND RECOVERY RANGE605/8050 1-Naphthylamine 10 • 94606/8060 Dibutylchlorendate 24 - 154608/8080 Dibutylchlorendate 24 - 154

2,4,5,6-Tetrachloro-m-xylene 25 - 125609/8090 2-Fluorobiphenyl 43 - 116

610/8310 Benzo(e)pyrene 43-116Decafluorobiphenyl 40-140

611/8110 Isodrin ' 33-141

612/8120 Dibutylchlorendate 24 - 154615/8150 2,4-DB 40 - 140

. For GC/MS, standard EPA surrogate compounds will be used for all analyses.

5.10 ESTABLISHMENT OF ACCEPTANCE CRITERIA

Establishment of acceptance criteria is necessary in order to be able to determineregularly whether or not quantitative data generated by the laboratory are within thecontrol limits. The principal criteria that are used to measure the quality of the data areaccuracy and precision.

The initial determination of acceptance criteria hinges upon repetitive measurements ofprepared spiked solutions, and determination of spike recovery. Twenty samples oflaboratory reagent water are spiked with the analytes of interest at a concentration ofapproximately twice the quantitation limit. Where applicable, the water is also spikedwith surrogates and internal standards. The samples are then prepared for analysisfollowing precisely the appropriate protocol, and the concentrations of the analytes are

«determined. From these values, the mean and the standard deviation for the recovery ofeach analyte are determined. The deviation of. the mean from the known spiked amount is

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a measure of the accuracy of tha method. The standard deviation of tha series ofmeasurements is a measure of tha precision of the method. Tha percent recovery iscalculated as follows:

R-100 X

where R » Percent recovery of the anatytaCm * The measured concentration of the analyte

Ci - Tha native concentration of the analyte in the sample (Ci - 0 forblank spike)

Cs =» The amount of analyta spiked into the sample.

Tha accepted recoveries of tha analytes must ba within three* standard deviations of themean. It should ba emphasized that recoveries are dependent upon both tha method ofsample preparation and tha sample matrix. Thus, recoveries from soil ara not expectedto ba within tha acceptance limits as determined for water. Similarly, extraction bysonication may not show tha same recovery as would an extraction via a Soxhletextractor. Thus, acceptance criteria must ba determined matrix by matrix, and methodby method.

Frequently, samples ara spiked at tha time of sample preparation, without knowing ifthe anatytes that ara being spiked into tha sample ara present or not, and withoutknowing if these analytes are at levels that would make tha spike amount insignificantTha analyst is cautioned that recoveries of spikes should not ba calculated if tha amountin tha sample is overwhelming tha spike. For most applications, if tha ratio C$/Ci is notequal to or greater than 5, tha spike recovery should not ba calculated, since thauncertainty in tha native concentration is sufficient to causa greater uncertainties in thespike recovery.

The acceptable precision range is defined in a similar manner. Tha precision is ameasure of tha deviations from tha mean of repetitive measuraments. Thus, standarddeviation will be used as a measure of precision. More frequently, tha relative percentdeviation will br used because at best, measurements ara performed in duplicate. Therelative percent deviation is determined by tha equation

REV.O5/88 «• AR307257

%RPD« 100 X X!! ' *2

where xi « high value for the analyteX2 •= low value for the analytexm - mean value for the analyte - —10* 2

The results of the determination of recoveries and relative percent deviations will beplotted, indicating the upper and lower limits of acceptance, and the upper and lowerwarning limits. Future data will be considered acceptable if recoveries of spikes andrelative deviations of duplicates fall within the acceptance criteria. The control chartswill be updated regularly, generally requiring 20 data points to obtain a valid controlchart. The QC Section will maintain the control charts and update them regularly, whensufficient data are collected. Whenever the control charts are updated and the acceptancelimits modified, the QC Section will issue the new limits to the analytical section of thelaboratory in which the analyses are performed. It is the responsibility of the sectionmanagers to assure that data within their section are within the acceptance limits. Ifthey are not, corrective action will be initiated immediately by the section manager ofthe appropriate section.

If five successive measurements, while falling within the control limits, appear on thesame side of the mean, the analyst will stop to investigate if the trend indicates that achange in methodology has occurred. Such successive points may indicate a pattern, andit would be necessary to institute a return to preexisting conditions to avoid thepossibility that out of control situations may arise.

It is not feasible, in organic analysis, to obtain control Charts for every analyte. Thus,while initial control charts are constructed for all the parameters that are beinganalyzed, continuous verification of the control is obtained through the use of surrogatecompounds and the spiked blank analysis. All other analytes in the organic analysis willbe assumed to be within control if their relative response to the internal standards andsurrogates have remained constant.

»

While accuracy and precision form the backbone of the acceptability of quantitative data,qualitative identification is more difficult to cast into quantitative measures. In organic

REV.Os/88 5-29 AR307258

analysis, the principal criterion for chromatographic analysis is tha retention time, orrelative retention tima. Relative retention time is used with those methods employinginternal standards. It is the more reliable maasure because it is less dependent on suchphysical parameters as tha length of tha column. In all cases, tha retention tima for eachanalyte, or the relative retention time for tha analyte, will be based on tha data obtainedfrom the nearest standard.

To determine tha acceptance windows for retention times, tha continuing calibration datawill ba employed. For each compound, tha retention times obtained in performing thacontinuing calibrations during tha period of one week will ba averaged and their standarddeviation determined. The acceptance window will consist of threa standard deviationsfrom the mean retention tima for each compound. Tha retention tima acceptance windowwill ba redetermined whenever tha chromatographic column is changed or thechromatographic conditions altered. It is tha responsibility of tha analyst to maintainthe records for retention tima criteria. Copies of tha established acceptance windowswill ba submitted by the analyst to tha QC Section for reference in reviewing work.In mass spectrometric analysis, in addition to tha retention tima, tha mass spectralmatch of tha compound to the standard will be used to verify its identity.

In inorganic analysis, tha determination of a positive signal, after correcting for knownpotential interferences will constitute a positive identification.

5.11 DEVELOPMENT OF NEW OR MODIFIED METHODS

There are occasions when it is necessary in tha laboratory either to devise a newapproach to analysis or modify an existing method. The former may be needed foranalytes for which proven methods do not axist. or if they do, the/ ara not applicable totha matrix being handled. The latter case is frequently tha situation that arises becauseof unusual matrix interferences. It Is not tha intent of this manual to prescribeanalytical approaches to analytes for which methods do not yet exist. However, in orderthat tha laboratory may use tha methods with any reliance on tha data, tha new methodmust ba subjected to tha repetitive analyses of a spiked matrix in order to ascertain thaprecision and accuracy of the method. No method will ba employed by tha laboratorywithout tha establishment of precision, accuracy; and detection limits.

- 05/88 5-30 AR307259

When a method is being modified, or a new method is being devised and tested, foranalytes for which an existing approved method is available, the new or modified methodwill be subjected to equivalency testing. In performing the equivalency testing, theanatytes will be subjected to seven replicate analyses in parallel by the existing methodand the new method. To be acceptable, the new method must produce results that arestatistically equivalent, or are better than the old method. In addition, sufficientreplicate analyses will be performed to assure that acceptance criteria may beestablished. The new or modified method will then be written, the method with thesupporting data and documentation will be reviewed by the Section Manager for thesection in which the analyses will be performed and by the QA/QC Manager. Aftercorrection and amendments are inserted, the QA/QC Section Manager will transmit theinformation and the new method to the Technical Director for approval. When approvedby the Technical Director, the method may become part of the repertoire of thelaboratory.

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6.0 DATA HANDLING

The data produced by the various sections of tha laboratory are ultimately tha productwhich the laboratory offers. Henca, not only is it necessary to produce results withaccuracy and precision, but it is also necessary to ba able to maintain tha traceability oftha data and the association of sets of data with each other. Tha responsibilities to thaproduction of accurate and precise data are with the individual analysts. They ara, afterall, the producers of tha data. No amount of supervision and validation can correct formistakes or omissions occurring at the bench. At best, supervision and validation cancull tha unsupported data. Traceability of tha data, however, pertains to tha manner inwhich the records are kept within the laboratory as a whole. Because of this, recordkeeping in the laboratory, will be addressed first. This will be followed by a briefdiscussion of data reduction, data validation, data review and release, and finallyreporting.

6.1 DATA RECORDING

Tha modes of maintaining data in tha various sections differ with tha methods of analysis.Certain aspects of record keeping have been addressed in tha section pertaining to thasample logging and distribution of tha information through tha laboratory. The travellerand tha sample transfer forms (whether for prepared samples or for raw samples)constitute the first step in tha generation of data for any set of samples. Samples in thalaboratory, however, ara analyzed in batches. On large jobs, a batch may constitute justa portion of tha total number of samples in tha job. For small job. a batch may consist ofsamples from several travellers handled together. Thus, tha maintenance of records intha laboratory must also provide for cross-referencing batches and travellers.

6.1.1 Notebooks

Certain records are maintained in notebooks by the analysts. These records maypertain to methods that ara entirely manual, such as many of tha methods in wetclhemical testing, or they may ba used to record unusual observations during theperformance of preparation and analyses of instrumented techniques. Thesenotebooks become a permanent record of laboratory work, and they must batraceable.

rev. 05/88 s-1 AR30726I

i Bound hardcover notebooks, with prenumbered 'ages, will be numbered andissued by the C "5C section. The QA/QC sectic /ill number the notebook, andrecord in its own notebook log the date of issuance and the laboratory section towhich the notebook has been issued. When the notebook has been filled, it will bereturned to the QA/QC section for permanent archiving.

Users of the notebooks will maintain good laboratory practices in their use. Nopages will be torn out of the notebook; corrections will be done by single line-outerasures, followed by initialling and dating the correction; and each page of thenotebook wit -e signed and dated by the analyst at the time of filling the page.Tk,e use of such materials as tape or liquid paper to make corrections is notpermitted.

*6.1.2 Record Keeping In Sample Preparation

Sample preparation for analysis is generally a manual effort. The records in thisoperation are manually kept All records for routine sample preparation will be

i, kept on standardized forms. The forms will be filled by the person preparing thesamples. The forms will be filled in ink, with no erasures.

If an error occurs, the preparer will line out the erroneous entry once, andenter the correct entry. The preparer will then initial and date the correction.

The following information must be entered:a. The analysis type for which the samples are prepared (usually the

heading of the sheet)b. The date of preparation, and the name of the preparerc. The QC batch identificationd A fisting of the samples being prepared, using the Keystone sample

identificatione. For each sample listed, the quantity of sample taken, including the units

of measurement (for solid samples, use the wet weight) "f . If the method calls for the addition of surrogates, then for each sample the

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surrogate mixture identification and tha quantity, including units, will beentered

v_>g. For any sample that is spiked, tha identification of the spiking mixture

and the quantity, including units, will be entered

h. The identification of the medium of the prepared sample (i.e., tha solventfor organic extraction, tha acid for metal preparation, etc.) and tha lotnumbers of the reagent media

i. Tha final volume of each prepared sample, including unitsj. Any unusual observations. If these are recorded in a notebook, tha

notebook and page numbers must ba entered on tha form.

In addition to filling tha form, the preparer must also tag the prepared samples.As a minimum, tha tag will identify the sample and tha QC batch in which thasample has been prepared. ,

When tha preparation is complete, the form will ba checked for completeness bythe supervisor of tha section, or his designed, and initialed and dated. Thapreparer will make as many copies of the filled form as there ara different jobsin tha batch. The original of tha form will ba maintained in the file of thapreparing section. Tha preparer win then transfer tha prepared samples withtha accompanying copies of the preparation records to tha section responsible forthe analysis of tha prepared samples.

Standard forms for maintaining tha records in tha sample preparation areas areshown in Figures 6-1 and 6-2.

6.1.3 Record Keeping In Instrumented Analysis

Many instrumental methods of analysis produce printed traces, charts, or tables.Some of tha information specified below is entered through a data system beforethe runs ara mada. Clearly, those items of information need not ba reenteredmanually.

For every technique, however, a run log must ba maintained. Tha followinginformation must ba entered in tha run log by the analyst:

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OPGANIC EXTRACTION

DATE BY

QC BATCH NO_________ METHOD (MARK ONE)————————— D EPA 3510 Sep. Funnel

MATRIX D EPA 3520 Continuous———————————— D EPA 3540 Soxhlet

Reagents, Solvents, and Clean-Up Materials: D EPA 3550 SonicationD Other, Specify 'Material Mfr Lot No. Activation

COMMENTS

SAMPLEID

AMOUNT(circle: mL, g)

.

SURROGATESMix ID Vol., uL

SPIKING MIXMix ID Vol.. uL

FINAL SOL'NSolvent Vol., ml

CLEANUP

.

COMMENTnote-page

REV:05/88 FIGURE 6-1

6-4 AR307261*

METALS PREPARATION

DATE BY

QC BATCH NO. METHOD (MARK ONE,MATRIX Q EPA 3005 Aq. for Rama and ICP

——————————————— fl EPA 3010 Aq. for Flame and ICPQ EPA 3020 Aq. for GFAA

Reagents: D EPA 3040 OH. Grease, WaxMaterial Mfr Lot No. EPA 3050 Sad.. Soil, Sludge

Q EPA 7470 Aq. mercuryQ EPA 7471 Mercury in solidsfj Other, Specify _______

COMMENTS

SAMPLEID

AMOUNTCircle: mL, g]

SPIKING MIXMix ID Vol., mL

FINAL SOLUTIONMatrix Vol., mL

COMMENTSnote-page

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FIGURE 6-2

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a. Identification of the analysis (usually this will be the heading of the tog)b. Identification of the instrument

*V - •' •', '*-,'• •c. Date of analysis, and identification of the analystd Identification of the QC batche. Sequential listing of runs (including tuning, initial calibration or

continuing calibration, blanks, spiked blanks, samples, duplicatesamples, spiked samples, etc.). This listing must be accurate andsequential, and the run number (where applicable) must be included

f. Aliquot of prepared sample that is taken for analysis, including unitsg. Any unusual observations. If these are entered in a notebook, they need

only be summarized on the form, and the notebook and page numbersentered for further identification of the comments.

Where printouts for each single run are obtained separately, the printout mustinclude the identification of the method of analysis, date of analysis, identificationof the analyst, identification of the run, identification of the QC batch, and thealiquot of sample that was taken.

Before transferring the data further, the analyst must confirm that the resultsas they appear on the printout are correct. If the results are incorrect, theanalyst will tine them out once and enter the correct value manually. Thesecorrections will be done in ink. When the analyst is finished with the batch ofsamples, including the review of the data, he will initial the run log and transferthe run fog with the data to the Section Supervisor.

The section supervisor wilt review the run log to verify that the sequence of runshas been property followed, as required by the specific method. The sectionsupervisor will also review the QC data pertaining to the batch, and verify thatthe instrument was performing within the required specifications. If any runsappear to have caused problems, the section supervisor wilt make a point ofchecking those data; otherwise, the section supervisor will only spot check theresults on about 20% of the sample runs.

When the section supervisor is satisfied that the data are valid, he will initial therun tog and date it. He will have as many copies made of .the run tog as there are

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jobs represented in the batch that has been analyzed, plus one additional copy fortha QA/QC section. He will then transfer tha samples data to tha data managementgroup, and tha QC data to the QA/QC section. Together with tha data, the sectionsupervisor will transfer the copies of the records from the preparation sectionto the data management section and to tha QA/QC section.

The original run log will be maintained in tha files and records of the sectionresponsible for tha analysis.

For instrumental methods which do not produce the identifying coda of tha run ontha permanent records, such as methods that employ a strip chart as theinstrumental output, tha individual traces will ba identified manually by tha runnumber, and the identification of tha parameters associated with tha run will barecorded manually on the run log.

6.1.4 Record Keeping In Noninstrumented Analyses

Manual analyses have become a rarity in the modem laboratory. Nonetheless,such techniques ara still occasionally employed and tha data generated by thesemethods ara usaabla. Raw data from these analyses will ba kept in hardboundnotebooks. Including all the pertinent information that is normally recorded onprintouts in other technologies. Tha results will be summarized on a summaryform and submitted to data management and to QA/QC section. Tha summary formwill include an identification of tha notebook number and page numbers withinthe notebook that pertain to tha analysis.

6.2 DATA REDUCTION

Reducing the raw data to a presentable form is the responsibility of tha analystperforming tha analysis. In reducing data, tha analyst must take into account whetherthe sample is aqueous or solid, the sample siza, and whether or not tha data ara to bapresented in the form of wet weight or dry weight All final values must ba accompaniedwith tha units of tha value. Tha following equation applies to the calculation forconcentration of an analyte in most analytical techniques employed in tha laboratory.

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5/88 *7 AR307267

C-R?Xv7X As"xDF

where, C «= Concentration of the analyte in the sample, in appropriate units[ng/L (ppt), ug/L (ppb), mg/L (ppm); ng/kg (ppt), ug/kg(ppb), mg/kg (ppm)]

I « Signal size, in units appropriate to the methodRF « The response factor, as defined in Section 5.6.1, in units of signal

size per unit weight of the analyte. This response factor isessentially a mean response factor, determined through regressionof the initial calibration data. If it is not possible to use the meanresponse factor (usually because of instrumental softwarelimitations), then the response factor from the run thatcorresponds to the midpoint of the linear range is used, as long asthis response factor does not differ from the mean by more than10%. The response factor to be used is always taken from theinitial calibration. *

vj « The aliquot size (such as injection amount) of the preparedsample, taken for analysis, in units of mL

ve » The total final volume of the prepared sample (extract volume,digest volume, etc.) in units of mL

AS « The amount of sample taken for preparation. For liquid samples,use mL; for solid samples use the weight in kg. If the results areto be determined on the basis of dry weight, use the following todetermine the sample size:.... . . .. %solidsA8 (dry) . As (wet) x 10Q

DF - Dilution factor. The dilution factor is 1 for samples that areprepared exactly as prescribed in the protocol. If the extract ordigestate require dilution, then the dilution factor differ fromunity. For example if an extract is diluted from 1 mL to 100 mUthe dilution factor becomes 100. If an extract is concentratedfrom 10 mL to 1 mL the dilution factor becomes 0.1.

In many methods, the data reductu. .is computerized, alleviating the need for extensivemanual reduction of the results. Computers, however, are not perfect The analyst mustreview the data, relating it back to the fundamental measurements on which the analysesare based. Thus, in chromatographic techniques, the analyst will compare area counts ofpeaks with those of the corresponding standard, and verify that the data were in factcorrectly reduced. It is also the respnsibility of the analyst to verify the identificationof parameters.

AR307268

It is of tha utmost importance that tha analyst pay close attention to the data beingreduced by him. Data are only spot checked beyond tha analyst. ^

6.3 DATA VALIDATION

Data validation within each analytical section has been discussed previously. Before datafrom an analytical batch may be incorporated into reports, the validation process outsidetha laboratory section that produced tha data consists of a review of tha QC data on thabatch by tha QA/QC section. It is not the responsibility of the QA/QC personnel to checkand verify every value generated and reported by tha laboratory.

In reviewing completed batches, tha QA/QC personnel will check for tha following items,using a checklist to record their observations: fa. Is tha batch completeb. Have all the analyses been performed within holding times, and if not is there an

acceptable explanation for deviations from the holding timesc. Is there a valid continuing calibration associated with tha runs for each

parameter of tha individual samples within the batch ,d. Is tha sequence of runs In which the samples were analyzed proper for tha method

(i.e., are there regular blanks run when necessary, are there standards run formethods requiring periodic standards, are there laboratory blank spikes andmatrix spikes, and laboratory duplicates)

a. If surrogates are required by tha method, are their recoveries within tha controllimits in the spiked blank

f. Is tha recovery of surrogates within control limits in tha samples, and if not, hastha sample preparation and analysis been repeated, and have tha recoveries beenacceptable in tha repeated analysis

g. Is tha recovery of spiked compounds in tha laboratory spiked blank acceptableh. Is tha recovery of spiked compounds in tha spiked sample acceptable and if not,

has there been an acceptable explanation or a repeat of the analysisi. Do duplicate analyses in tha run sequence exhibit precision within the control

limitsj. Is tha documentation in order

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