S F^'AL Tb - semspub.epa.gov > APPf?0!/£D S F^'AL Signature-PA. Remedial F^jcn.^ Section TCN 4204 /IR300U3. It ... NCP National Oil and Hazardous Substances Contingency Plan

TCN 4204-01-QAPjP V& » J DSECTION 1REVISION NO. 0PAGE __ OF __04/SEPT/90_____

ENVIRONMENTAL PROTECTION AGENCYALTERNATIVE REMEDIAL CONTRACTING STRATEGY (ARCS)

REGION IIICONTRACT #68-W8-0092

WORK ASSIGNMENT #92-04-3LQ6

SAMPLING AND ANALYSIS PLANVOLUME I

(QUALITY ASSURANCE PROJECT PLAN)

SEPTEMBER 4, 1990

REMEDIAL INVESTIGATION/FEASIBILITY STUDY

BUTZ LANDFILL(ALSO KNOWN AS NORTH ROAD SITE)

JACKSON TOWNSHIP, MONROE COUNTY, PENNSYLVANIA

TETRA TECH, INC.

Tb> APPf?0!/£D

S F 'AL

Signature-PA. Remedial F jcn. Section

TCN 4204

/IR300U3

ItTETRA TECH. INC. - ^^^POST OFFICE BOX B-5 November 26, 1990r SrSo -S . S> . TCN 4204-01

Mr. Victor JanosikU. S. Environmental Protection AgencyRegion IIIMail Code 3HW21841 Chestnut BuildingPhiladelphia, PA 19107

Dear Vie: /+\ A O • Dcy/i rj iSUBJECT: REVISIONS TO FIELD (L'tMfLIHQ FLjHM, BUTZ LANDFILL, USEPA CONTRACT

NO. 68-W8-0092, WORK ASSIGNMENT NO. 92-04-3LQ6

The following revisions (enclosed) are made to the Quality Assurance Project Plan (QAPjP), in responseto comments submitted September 26,1990 from Diann Sims of the Region III Central Regional Laboratory:

• Replace Section 5.0 in its entirety with the new Section 5.

Minor corrections have been made to the following pages and the revised pages are enclosed:

Table of Contents, pages i (signatures have been added)Table of Contents, pages ii and iiiPages v through ix - add to documentSection 3, page 1Section 3, page 6Section 8, page 25Section 11, page 33Section 12, page 35Sectiqn 15, page 38

In all references to sampling for Target Analyte List parameters, all metals, including mercury, plus cyanideare to be included.

Should you have any questions, please do not hesitate to call.

Sincerely,- . i . /o ,2

^Christopher A Burns, Ph.D.Geologist

JlPEnclosures

cc: James ClarkJames McKenzieSusan JanowiakSteve Pollak

/? P n r* r '? r f»* * * i t t ',', *.:. I '

PA. RemiJ.^: ,"..„,,.•....... f ;:;;—!

ItTETRA TECH. INC. ,, . , .. 1nnnPOST OFF.CE Boxers September 5, 1990NEWARK.D£LAWAREIig7l5 O6 S ,TEUEPKONET 3O2' -73B- 7S5I •

u v , , >Mr. Victor Janosik,r. icor anosi ' / 1 /U. S. Environmental Protection Agency I/ v / /> £>yuRegion III / , {j a i ^ , ?* ' ' (841 Chestnut BuildingPhiladelphia, PA 19107

Dear Mr. Janosik:

SUBJECT: VOLUME I (QUALITY ASSURANCE PROJECT PLAN) OF THE SAMPLINGAND ANALYSIS PLAN FOR THE BUTZ LANDFILL SITE, ARCSCONTRACT #68-W8-0092, WORK ASSIGNMENT #92-04-3LQ6

Enclosed please find Volume I (Quality Assurance Project Plan) of the Sampling and AnalysisPlan (SAP) for Butz Landfill. Volume II (Field Sampling Plan) will be sent shortly underseparate cover.

Should you have any questions, please do not hesitate to call.

Sincerely,

Christopher A. Burns, Ph.D.Work Assignment Manager

J1PEnclosure

cc: Mr. James McKenzieMs. Diane Sims, CRL (2)Mr. James MercerMr. Steve PollakMr. James Clark (letter only)Ms. Susan Janowiak (letter only)

TCN 4204-01-QAPjPSECTION ____1REVISION NO. 0PAGE __ OF ___04/SEPT/90 ____

ENVIRONMENTAL PROTECTION AGENCYALTERNATIVE REMEDIAL CONTRACTING STRATEGY (ARCS)

REGION IIICONTRACT #68-W8-0092

WORK ASSIGNMENT #92-04-3LQ6

SAMPLING AND ANALYSIS PLANVOLUME I

(QUALITY ASSURANCE PROJECT PLAN)

SEPTEMBER 4, 1990

REMEDIAL INVESTIGATION/FEASIBILITY STUDY

BUTZ LANDFILL(ALSO KNOWN AS NORTH ROAD SITE)

JACKSON TOWNSHIP, MONROE COUNTY, PENNSYLVANIA

TETRA TECH, INC.

It SignaturePA. Remedia; i\., ;c;u- Section

TCN 4204

SIGNATURE PAGE

APPROVALS:

J*s Mercer

bL\J &t J, PPM

USEPA Region III Quality AssuranceOfficer

TCN 4204-01-QAPjPS'ECTION ____1_REVISION NO. 0PAGE _JL OF • 5104/SEPT/90____

Christopher Burns DateTetra Tech Work Assignment Manager

A TeNtrra Tech Quality Assurance Officer e

Victor Janosik A^ / r/USEPA Region III Project Officer

FINAL

Signature ' Y-taWljlfi

fTCN 4204-01-QAPjPSECTION 2REVISION NO. 1PAGE 3 OF 5126/NOV/90_____

TABLE OF CONTENTS

Revision

1.0 TITLE PAGE 0 i2.0 TABLE OF CONTENTS 1 ii3.0 PROJECT DESCRIPTION 1 1

3.1 INTRODUCTION 1 13.2 GENERAL BACKGROUND AND SITE INFORMATION 1 3

4.0 PROJECT ORGANIZATION AND RESPONSIBILITIES 0 85.0 QUALITY ASSURANCE OBJECTIVES 1 146.0 SAMPLING PROCEDURES 0 207.0 SAMPLE CUSTODY 0 238.0 CALIBRATION PROCEDURES AND FREQUENCY 1 249.0 ANALYTICAL PROCEDURES 0 2710.0 DATA REDUCTION, VALIDATION, AND REPORTING 0 28

10.1 FIELD AND TECHNICAL DATA 0 2810.2 LABORATORY DATA 0 30

11.0 INTERNAL QC CHECKS 1 3312.0 PERFORMANCE AND SYSTEM AUDITS 1 3513.0 PREVENTATIVE MAINTENANCE 0 3614.0 SPECIFIC PROCEDURES TO BE USED TO ASSESS DATA

PRECISION, ACCURACY, REPRESENTATIVENESS ANDCOMPLETENESS 0 37

15.0 CORRECTIVE ACTIONS 1 3816.0 QUALITY ASSURANCE REPORTS TO MANAGEMENT 0 4317.0 REFERENCES 0 45

APPENDICES;

A. SPECIAL ANALYTICAL SERVICES (SAS) REQUESTSB. PARAMETER DETECTION LIMITSC. ENGINEERING ANALYSIS AND CALCULATION VALIDATION PROCEDURESD. AUDIT PROTOCOLE. ASSESSMENT OF DATA PRECISION, ACCURACY, REPRESENTATIVENESS,

COMPARABILITY, AND COMPLETENESS

/TR300U8

TCN 4204-01-QAPjPSECTION ____2_REVISION NO. .1PAGE _4_ OF '5126/NQV/90_____

LIST OF FIGURES

3-1 Butz Landfill General Location Map 23-2 Local Area Map 4

4-1 Butz Landfill RI/FS Project Organization Chart 94-2 Butz Landfill Quality Assurance Project Organization Chart 10

8-1 Calibration Record of Field Instruments 26

10-1 Data Review Flow Chart 29

15-1 Corrective Action Decision Flow Chart 42

LIST OF TABLESPage

4-1 Personnel Responsibilities for Quality Assurance 11

5-1 Data Quality Levels Summary 165-2 Butz Landfill - Sampling Summary 175-3 Butz Landfill - Data Quality Objectives 185-4 Butz Landfill - Accuracy and Precision Data Quality Objectives

for RAS and SAS Organics 195-5 Butz Landfill - Accuracy and Precision Data Quality Objectives

for RAS and SAS Inorganics 19.45-6 Butz Landfill - Completeness Objectives 19.5

6-1 Butz Landfill - Analytical Parameters, Preservation,and Holding Times 21

8-1 Butz Landfill - Equipment Maintenance & Calibration Protocols 25

10-1 Recommended Documentation for Independent QA Reviewof Data on Organic Substances 31

10-2 Recommended Documentation for Independent QA Reviewof Data on Inorganic Substances 32

15-1 Corrective Actions Checklist 40

iii

TCN 4204-01-QAPjPSECTION 2REVISION NO. 0PAGE _L OF 5104/SEPT/90_____

DISTRIBUTION LIST FOR QAPjP

NO. OF COPIES

Tetra Tech Work Assignment Manager 1Tetra Tech Quality Assurance Officer 1USEPA Region III Remedial Project Manager 1USEPA Region III Quality Assurance Officer 2Tetra Tech Remedial Task Manager 1Tetra Tech Field Task Leader 1USEPA Region III Project Officer 1

iv

A R 3 0 0 I 5 0

TCN 4204-01-QAPjPSECTION 2REVISION NO. 1PAGE 5.1 OF 5126/NOV/90______

ACRONYMS

ALK Alkalinity

AOC Administrative Order on Consent

ARARs Applicable or Relevant and Appropriate Requirements

ARCS Alternative Remedial Contracting Strategy

ATSDR Agency for Toxic Substances Disease Registry

BOD Biological Oxygen Demand

BNA Base Neutral Acids

CAS Chemical Abstract Substance

CD Consent Decree

CERCLA Comprehensive Environmental Response, Compensation, andLiability Act of 1980

COD Chemical Oxygen Demand

COE U.S. Army Corps of Engineers

CR Community Relations

CRDL Contract Required Detection Limit

CRL/CLP Central Regional Laboratory/Contract Laboratory Program

CRP Community Relations Plan

CRQL Contract Required Quantitation Level

DOC Department of Commerce

/1R30QI5!

TCN 4204-01-QAPjPSECTION 2REVISION NO. 1PAGE 5.2 OF 5126/NOV/90_____

DOO Department of Defense

DOE Department of Energy

DO! Department of Interior

DQO Data Quality Objective Levels

ECD Electron Capture Detector

ERA Expedited Removal Actions

ERB USEPA Emergency Response Branch

ERT Environmental Response Team

FEHA Federal Emergency Management Agency

FID Flameionization Detector

FS Feasibility Study

FSP Field Sampling Plan

GCMET Gas Chromatography Mass Electron Transfer

GCMS Gas Chromatography/Mass Spectrometry

HHS Department of Health and Human Services

HRS Hazard Ranking System

HSL Hazardous Substance List

HSP Health and Safety Plan

lAGs Interagency Agreements

IRH Initial Remedial Measures

vin i "•* f', *~\ •"• i P*" f\H l-» o y u i b 2


MS Matrix Spike

MSD Matrix Spike Duplicate

NBS National Bureau of Standards

NCP National Oil and Hazardous Substances Contingency Plan

NOAA National Oceanic and Atmospheric Administration

NPDES National Pollution Discharge Elimination System

NPL National Priorities List

NRC National Response Center

NRT National Response Team

OSC On-Scene Coordinator

O&H Operation and Maintenance

OVA Organic Vapor Analyzer

PA Preliminary Assessment

PADER Pennsylvania Department of Environmental Resources

PID Photoionization Detector

PPH/PPB Parts per mi 11i on/parts per bi11i on

PRP Potentially Responsible Party(ies)

QAO Quality Assurance Officer

QA/QC Quality Assurance/Quality Control

QAPjP Quality Assurance Project Plan

vii

AR3QOI53


RA Remedial Action

RAS Routine Analytical Services

RCRA Resource Conservation and Recovery Act of 1976

RD Remedial Design

RI Remedial Investigation

RI/FS Remedial Investigation/Feasibility Study

ROD Record of Decision

RPO Relative Percent Difference

RPM Remedial Project Manager

RRT Regional Response Team

RSCC Regional Sample Control Center (USEPA)

SARA Superfund Amendments and Reauthorization Act of 1986

SAS Special Analytical Services

SI Site Inspection

SMOAs State Memorandum of Agreements

SOW Statement of Nork

SSO Site Safety Officer

TAL Target Analyte List

TAT USEPA Technical Assistance Team

TCL Target Compound List

viii

A R o G Q i 54

TCN 4204-01-QAPjPSECTION 2REVISION NO. 1PAGE 5.5 OF 5126/NOV/90______

IDS Total Dissolved Solids

TM Task Manager

TOC Total Organic Carbon

TSD Treatment, Storage, and Disposal Facility

TSS Total Suspended Solids

USCG United States Coast Guard

USEPA United States Environmental Protection Agency

VOC Volatile Organic Compound

WAM Work Assignment Manager

IX

A R o U L I j 55

TCN 4204-0I-QAPJPSECTION ____3_REVISION NO. 1PAGE 6 OF • 5126/NQV/90_____

3.0 PROJECT DESCRIPTION

3.1 Introduction

The United States Environmental Protection Agency (USEPA), Region III,utilizing the Alternative Remedial• Contracting Strategy (ARCS), hasauthorized Tetra Tech Inc. (Tetra Tech) to conduct the RemedialInvestigation/Feasibility Study (RI/FS) for the Butz Landfill located inJackson Township, Monroe County, Pennsylvania (Figure 3-1). The RI/FSactivities will be performed under Work Assignment #92-04-3LQ6, datedDecember 16, 1988. All RI/FS activities shall be based on regulations andprocedures for implementing response actions set forth in the National Oiland Hazardous Substances Contingency Plan (NCP) as amended.

This Quality Assurance Project Plan (QAPjP) addresses the major qualityassurance/quality control (QA/QC) considerations and QA/QC guidelines forthe field and analytical activities to support the RI/FS at the ButzLandfill. As the project proceeds, new considerations may need to beaddressed and additional guidelines provided in order to maximize theefficiency and quality of the field work. Appendices included in thisQAPjP are intended to supplement this document, and include the ParameterDetection Limits, Special Analytical Services (SAS) Requests, and AuditProtocols.

fiRSGUf56

BUTZ UKDFILL

FIGURE 3-1GENERAL LOCATION NAPBUTZ LANDFILL

SOURCE: USGS TOPOGRAPHIC MAP MOUNT POCONO QUADRANGLE

TCN 4204-01-QAPJPSECTION 3REVISION NO. 0PAGE 8 OF 5104/SEPT/90____

3.2 General Background and Site Information

The Butz Landfill is approximately 13.42 acres in size and is located onthe south side of Township Road 601 (North Road) in Jackson Township,Monroe County, Pennsylvania (Figure 3-2). The landfill is surrounded onthree sides by undeveloped mature hardwood forests. Land use in thesurrounding area land use is primarily agricultural and recreational. Thepopulation within a three mile radius of the site is approximately 3,300people, which doubles during the tourist seasons of winter and summer.

The Butz Landfill was purchased by the Butz family in March 1963. Landfilloperations began in 1965 and continued until 1973. The landfill wasunpermitted, and accepted household refuse, solid waste, sewagesludge/liquids, and possibly some industrial wastes. The exact quantitiesof waste accepted by the Butz Landfill are unknown.

Based upon citizen complaints, investigation into the landfill operationsbegan in 1971 by the Pennsylvania Department of Environmental Resources(PADER). Water well pollution and leachate seeps were discovered at thistime. In early 1973 PADER ordered the Butz Landfill closed and requiredthe owners to develop a surface water management plan, a ground-watermonitoring plan, and to cover the landfill. The owners complied withPADER's requests and closed the landfill in late 1973.

The cover for the landfill was installed in late 1973, a surface watermanagement plan was implemented, and ground-water monitoring of nearbydomestic water wells was initiated. The parameters tested for included

;i c: oM K o U U I bo

Ull-l LU t/)o<J LU UJ < «t

h- co o: CL o

AR3UU 1

TCN 4204-01-QAPJPSECTION 3REVISION NO. 0PAGE 10 OF 5104/SEPT/90_____

fecal coliform, odor, color, conductivity, pH, hardness, iron, and chlorideconcentrations. The ground-water monitoring by the owners continued until1979.

In 1986 PADER found high levels of volatile organic compound (VOCs)contamination (primarily trichloroethylene) in the domestic water wellsin the vicinity of the Butz Landfill. Due to the high concentration levelsfound, PADER requested assistance from USEPA. The USEPA Emergency ResponseBranch (ERB) began operations at the site. The USEPA distributed bottledwater and installed treatment and filtration systems in the nearbyresidences with contaminated wells. USEPA also performed a soil vaporsurvey and magnetometer survey of the landfill and installed 17 monitoringwells near the landfill.

The soil vapor survey was limited in extent but revealed low concentrationsof VOCs. The magnetometer survey identified two localized areas of ferrousmaterials (metal) in the subsurface of the southern toe of the landfill.No further investigation has been done to confirm the presence of thesematerials.

Ground-water sampling of the 17 monitoring wells was completed, and alimited number of surface water and soil samples on and near the landfillwere collected. These results indicated the primary contaminants werevolatile and semi volatile organic compounds. Results of previous samplingefforts are contained in Tables 2-2, 2-3, and 2-4 of the Work Plan.

A H 3 0 U i 6 0

TCN 4204-01-QAPjPSECTION 3REVISION NO. 1PAGE 11 OF 5126/NOV/90_____

Currently, the USEPA Technical Assistance Team (TAT) continues to collectground water samples from selected residential wells on a quarterly basis.The data provided from this sampling, as well as the data collected fromother investigations has provided a good starting point for this RI/FS.However, the extent of contamination in the shallow aquifer, subsurfacesoils, surface water, and sediments has not been fully characterized.Additionally, the total extent of contamination in the deep aquifer is notknown. Therefore, a number of data gaps still exist for the site.

The following identified data gaps require a high confidence level in thedata to be collected:

• identification of contaminant sources;. identification and quantification of contaminants in the subsurface

soils within the landfill;. identification and quantification of contaminants in the surface

water and sediments in the vicinity of the landfill; and• extent of contamination in the deep and shallow aquifer.

The following identified data gaps require a less than high confidencelevel in the data to be collected:

• depth to bedrock below landfill;• areal extent of the landfill; and• thickness/volume of the landfill.

A R 3 0 0 1 6 1

TCN 4204-01-QAPJPSECTION 3REVISION NO. 0PAGE 12 OF 5104/SEPT/9Q____

The sampling schedule, objectives, and procedures are discussed in detailin the Field Sampling Plan.

.AR3G0162

TCN 4204-01-QAPjPSECTION 4REVISION NO. 0PAGE 13 OF 5104/SEPT/90____

4.0 PROJECT ORGANIZATION AND (RESPONSIBILITIES

The Butz Landfill project organization chart is presented on Figure 4-1.The site-specific quality assurance project organization is presented onFigure 4-2. Personnel responsibilities for quality assurance are presentedon Table 4-1. A more detailed description of the personnelresponsibilities can be found in the Tetra Tech Quality Assurance ProgramPlan (September 1988).

A complete listing of address and phone numbers of key project personnelis located in the Field Sampling Plan (FSP) and the Health and Safety Plan(HSP).

8

14R300 i 63

TCN 4204-01 -QAPjPSECTION 4

BUTZ LANDFILL REVISION NO. _p_QUALITY ASSURANCE

PROJECT ORGANIZATION CHART

U.S.E.P.A, REGION IIIQUALITY ASSURANCE OFFICER

I

U.S.E.P.A. REGION HI|__.RSCC I I

U.S.E.P.A. REMEDIALPROJECT MANAGERVICTOR JANOSIK

TETRA TECHWORK ASSIGNMENT MANAGERCHRISTOPHER BURNS, Ph.D.

TETRA TECHPROGRAM DIRECTORCARL HSU, Ph.D., P.E.

1111

- — - TETRA TECHQUALITY ASSURANCE OFFICl

JAMES MERCER, Ph.D.i11

TETRA TECHREMEDIAL TASK MANAGER

SITE QA OFFICERTAD YANCHESKI

GEOLOGISTSCHEMISTS-

FIELD TECHNICIANS

1i

TETRA TECHSITE HEALTH & SAFETY OFFI

MARY MUSETTI

FIGURE 4-2QUALITY ASSURANCE PROJECTORGANIZATION CHARTBUTZ LANDFILL

10


TABLE 4-1

PERSONNEL RESPONSIBILITIES FOR QUALITY ASSURANCE

Personnel Responsibilities

USEPA Region III Primary Provide oversight of all program activities.Contact, Remedial Project Review final project QA objectives, needs,Manager (RPM) problems, and requests. Approve appropriate

QA corrective actions as needed.

USEPA Region III Quality Provide contacts and approval for methods andAssurance Officer (QAO) analytical procedures. Ensure compliance with

USEPA QA/QC policies.

USEPA Regional Sample Control Provide coordination between USEPA andCenter (RSCC) Tetra Tech for field operations and analytical

services. Provide interface between contractlaboratory and USEPA analytical laboratory toensure comparability and compatibility betweenfield operations and analytical requests.Monitoring of analytical requirements.

Tetra Tech Program Director Implement necessary action and adjustments toaccomplish program objectives. Overseeproject performance to ensure contractcompliance.

Tetra Tech Work Assignment Oversee project performance and provideManager (WAM) technics! expertise to acnompt&i project

objectives. Ensure that project tasks aresuccessfully completed within the projectedtime periods.

11

• AR300166

TCN 4204-01-QAPjPSECTION 4REVISION NO. 0PAGE 17 OF 5104/SEPT/90_____

TABLE 4-1 (CONT)



Tetra Tech Remedial Task Oversee remedial investigation activities,Manager (TM) subcontractor management, technical support,

supervise and schedule field activities.

Tetra Tech Field Coordinator Oversee field operations and sampling design.Provide on-site technical support and superviseStandard Operating Procedures (SOP)implementation, project modification, andcorrective action during field operations.Contract Lab Program (CLP) contact.

Tetra Tech Site QA Officer, Site: Conduct field sampling operations inSafety Officer (SSO) accordance with approved sampling and

analysis plan. Ensure that all QA protocols(including chain-of-custody documentation,sample collection and labeling, sample storageand shipping, instrument calibration) arefollowed as required. Recognize andimplement necessary corrective actions.Document field operations. Ensure that healthand safety guidelines are followed to avoid anycompromise of sample integrity. Documentany health and safety issues affecting samplecollection. Provide data validation.

Tetra Tech Health and Safety Provide technical assistance as required toOfficer resolve on-site health and safety issues

requiring corrective action. Prepare Healthand Safety Project Plan.

12

U K o Q O l b ?

TCN 4204-01-QAPjPSECTION 4REVISION NO. 0PAGE 18 OF '5104/SEPT/90

TABLE 4-1 (CONT)



Tetra Tech Quality Assurance Provide technical QA assistance on site toOfficer (QAO) accomplish project objectives including

suggestions for corrective action implementa-tion. Perform system audits.

Central Regional Provides analytical support Performs allLaboratory/Contract Laboratory required QC sample analyses includingProgram (CRL/CLP) analytical duplicates, blanks, matrix spikes,

performance evaluation samples, and StandardReference Material (SRM). Initiates anddocuments required corrective action.Preliminary review of data for completenessand transcription or analytical error. Followsgood laboratory practices and USEPA guide-lines.

13

A R 3 u 0 i b bn

TCN 4204-01-QAPjPSECTION 5REVISION NO. 1PAGE 19 OF 5126/NOY/90______

5.0 QUALITY ASSURANCE OBJECTIVES

The overall quality assurance objectives for measurement data are to ensurethat data of known and acceptable quality are provided. All measurementswill be made to yield consistent results representative of the media andconditions measured. All data will be reported in units consistent withthose of other agencies and organizations to allow comparability ofdatabases.

The USEPA specifies five major characteristics of data quality that mustbe addressed in environmental sampling and analytical projects. These are:

• Precision - A measure of agreement among individual measurements ofthe same property under similar conditions. It is expressed in termsof percent difference between replicates or in terms of the standarddeviation.

• Accuracy - The degree of agreement of a measurement (or measurementaverage) with an accepted reference or true value. It is a measureof system bias. It is usually expressed as the difference ofmeasured from true values or as a percentage of the difference.

• Representativeness - Expr&»*es the degree to which data accuratelyand precisely represent a characteristic of a data population,process condition, sampling point, or environmental condition.

14

TCN 4204-03-QAPjPSECTION 5REVISION NO. 1PAGE 20 OF 5126/NOV/90______

• Completeness - A measure of the amount of valid data obtainedcompared to the amount expected to be obtained under normalconditions, usually expressed as a percentage.

• Comparability - Expresses the confidence with which one data set canbe compared to another. To achieve comparability in this project,analyses will be performed wherever possible according to the methodsand procedures of the ERA CLP. Standard reference materials willbe used to document traceability of calibration standards.Performance evaluation samples will be regularly analyzed to assurelaboratory performance comparable to that of other laboratoriesperforming environmental analyses.

The data quality levels summary for the Butz Landfill is given inTable 5-1. A summary of the proposed sampling for the Butz Landfill siteis presented in Table 5-2. Quality assurance objectives for precision,accuracy, and completeness have been established for each measurementvariable, where possible, and are presented in Tables 5-3 through 5-6.The goal of 100% completeness for background soils is important since onlya limited number of samples are planned to characterize naturally occurringor non-site related levels in the area of the site. For sediment andsurface water, 90% completeness is desireable in order to establishcontaminant gradients in the streams. Many more soil samples will fcecollected; therefore, a completeness goal of 75% should be sufficient.

For field QC data, such as calibration checks, no QA objectives have beenestablished by the USEPA. Field QC shall be maintained for descriptivepurposes.

15

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TABLE 5-6

BUTZ LANDFILL

OBJECTIVES FOR MEASUREMENT DATACOMPLETENESS OBJECTIVES

Parameter (a)

TCL Volatile OrganicsBackground Surface Water/SedimentSedimentSurface waterGround water

TCL BNA ExtractablesBackground Surface Water/SedimentSedimentSurface waterGround water

TCL Pesticides/PCBsBackground Surface Water/SedimentSedimentSurface waterGround water

TAL InorganicsBackground Surface Water/SedimentSedimentSurface waterGround water

Completeness

95%90%90%90%

95%90%90%90%

95%90%90%90%

95%90%90%90%

(a) UnitsSoil - ug/lcgSediment - ug/kgWater • ug/1

flR3U0179

TCN 4204-01-QAPjPSECTION 6REVISION NO. ;QPAGE 25 OF 5104/SEPT/90_____

6.0 SAMPLING PROCEDURES

A detailed discussion of sampling activities for the Butz Landfill is foundin the FSP, Part I of the Sampling and Analysis Plan.

The following considerations form the basis for the sampling plan developedfor the Butz Landfi11:

* site background and history;• sampling objectives;• sample location and frequency;• sample designation;• sampling equipment and procedures; and• sample handling and analysis.

The sampling objectives, locations, and frequency are based upon anevaluation of the data quality objectives discussed in Section 5. Samplingprocedures are derived from Tetra Tech Standard Operating Procedures foundin Appendix A of the FSP.

A summary of the analytical parameters, number of samples, samplepreservation, and holding times proposed for the Butz Landfill is shownon Table 6-1.

20

AR300I80

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TCN 4204-01-QAPjPSECTION ___7_REVISION NO. 0PAGE 28 OF 5104/SEPT/90____

7.0 SAMPLE CUSTODY

Sample custody is a vital aspect of the RI program, because data generatedmay be used as evidence in a court of law. The samples must be traceableby chain-of-custody procedures from the time of sample collection untilthe time the data are utilized for any major decision. Evidence ofcollection, shipment, and laboratory receipt must be documented toaccomplish this.

Procedures regarding sample custody are descussed in Section 8 of the FSP.

23

TCN 4204-01-QAPjPSECTION 8REVISION NO. 0PAGE 29 op 5104/SEPT/90____

8.0 CALIBRATION PROCEDURES AND FREQUENCY

Calibration procedures, calibration frequency, and standards for laboratorymeasurement variables and systems shall be in accordance with USEPA CLPrequirements.

Calibration procedures, calibration frequency, and standards for fieldmeasurement variables and systems shall be according to Tetra Tech SOP,Field Measurement of Organic Vapors. pH. and conductivity, which isdetailed in Appendix A of the FSP. A summary of equipment maintenance andcalibration protocols are given in Table 8-1.

An example of the equipment calibration log is shown on Figure 8-1. Fieldlogging of calibration records will include, where appropriate:

• Type and identification number of equipment;. Calibration frequency and acceptable tolerances;• Calibration dates;• Identification of individual(s) and/or organizations performing the

calibration;• Reference standards used for each calibration;• Calibration data;• Certifications or statements of cal ibration provided by manufacturers

and external agencies, and traceable to national standards; and• Information on calibration acceptance or failure.

24


TABLE 8-1

BUTZ LANDFILL

EQUIPMENT MAINTENANCE AND CALIBRATION PROTOCOLS

Equipment Caiibrant Frequency

PID (Photoionization Calibrate with isobutylene or Start of each dayDetector), FID (Flame other chemical-specificlonization Detector) calibration gas

Temperature Check against an NBS Start of each daythermometer

1 Specific Conductance Meter Calibrate with one calibration Start of each daysolution

Dissolved Oxygen Meter Calibration according to Start of each daymanufacturer's recommen-dations with ambient air

pH Meters Calibrate with two pH buffer Start of each daysolutions

Rechargeable Equipment Charge After use, asBatteries required

Sampling Accessories (tubing, Periodic maintenance performed As requiredsubmersible pumps) . & recorded in equipment

- maintenance log

25

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26 AR300I86

TCN 4204-01-QAPjPSECTION ____9_REVISION NO. 0PAGE 32 OF 5104/SEPT/90

9.0 ANALYTICAL PROCEDURES

Methods and references for most analyses are summarized in Table 6-1.Analysis of samples collected at the Butz Landfill will be performed bycontract laboratories with established protocols and QA procedures thatmeet USEPA guidelines ensuring that data generated will meet data qualityobjectives.

The USEPA CLP shall be utilized for the chemical analyses. The CLProutinely analyzes liquid and solid environmental samples for organic andinorganic priority pollutants and hazardous substance list (HSL) compounds.Routine Analytical Services (RAS) and Special Analytical Services (SAS)are proposed for the Butz Landfill samples at this time. SAS requestsare contained in Appendix A.

All analytical procedures, including procedural steps and options, QCrequirements, etc., for RAS are referenced in accordance with the CLPStatement of Work (SOW), or are specified by method in the SAS requests.Target detection limits are detailed in Appendix B.

27

AR300187


10.0 DATA REDUCTION, VALIDATION, AND REPORTING

The following procedures summarize the practices utilized by Tetra Techfor data reduction, validation, and reporting. The data review flow chartis given in Figure 10-1. These procedures are utilized for both field dataand laboratory data. The USEPA CLP is proposed for this project; thereforedata reduction, validation, and reporting will be conducted by others aspart of that program. However, procedures for non-CLP laboratory datareduction, validation and reporting are included should Tetra Tech berequired to perform this analyses.

10.1 Field and Technical Data

Both objective (measurement) and subjective (description) data are subjectto data validation. All data collection in the field shall be documentedfollowing the procedures detailed in Section 6.0, Field Documentation ofthe FSP. Objective data shall be validated at the time of collection (forexample, triplicate measurements) as well as by the Field TM to ensure thatthe correct codes and units have been included.

After data reduction into tabular or figure form, the objective data shallbe reviewed for anomalous or inconsistent values by the Task Manager. Anyanomalous or inconsistent data shall be resolved or clarified by evaluatingthe raw field data, equipment calibration logs, etc., and consulting withfield personnel.

28

A R 3 U U I 8 8

RESAMPLE

TCN 4204-01 -QAPjP

DATA FLOW

SAMPLECOLLECTION

FIELDDATA

ANALYSISOF SAMPLES

LABORATORYQC REVIEW

(NO^"*""

PREPARE RESULTSAND QC REPORT

SUBMIT TO QAMANAGER

JQA MANAGERREVIEWS DATA

NO _YES

NO

YES

DATA REPORTSTO FILE

DATA REPORTS TOPROJECT MANAGER

JPROJECT REPORT

PAGE 34 OF 5104/SEPT/90

IS SAMPLESTILL OK?

NO

REJECT

FIGURE 10-1DATA REVIEW FLOW CHARTBUTZ LANDFILLMONROE COUNTY, PENNSYLVANIA

29 AR30DI89


Subjective field and technical data shall be evaluated by the Task Managerfor reasonableness and completeness. Whenever possible, peer review shallalso be utilized in the data validation process in order to maximizeconsistency in data evaluation. Periodic field reviews of subjective datacollection shall be conducted.

Data reduction, validation and reporting of engineering analysis andcalculation data shall follow the procedures documented in Tetra TechStandard Operating Procedures, Engineering Analysis and CalculationValidation Procedures (Appendix C).

All validated field and technical data shall be reported in preliminarydraft and final RI reports for review and comment.

10.2 Laboratory Data

Any non-CLP laboratories used for this study will be required to submitdata with sufficient quality assurance support to enable reviewers todetermine conclusively the quality of the data (see Tables 10-1 and 10-2).Data must be of comparable quality to USEPA CLP data packages. The USEPACLP data packages provide the required quality assurance documentation.Overall criteria to assess usability will be as per USEPA FunctionalGuidelines for Data Validation (USEPA, 1988a,b,c,d).

30

AH300I90

TCN 4204-01 -QAPjPSECTION 10REVISION NO. 0PAGE 36 OF 5104/SEPT/90

TABLE 10-1

RECOMMENDED DOCUMENTATION FOR INDEPENDENT QA REVIEWOF DATA ON ORGANIC SUBSTANCES

1. Analyses of the requested priority pollutant acids, bases, neutrals (includingpolychlorinated biphenyls (PCB's) and pesticides), and chemically similarcompounds should be reported as follows:

• Sample concentrations reported in proper units (e.g., sediment inug/kg dry weight) to the appropriate number of significant figures onstandard data sheets;

• Lower limits of detection for undetected values reported for eachcompound on a sample-by-sample basis;

• Internal standard recoveries for analyses using method recoverystandards (including isotope dilution Gas Chromatography/MassSpectrometry (GC/MS)), reported on the data sheets as percentrecoveries; and

• Ancillary information, including the actual spike level of any recoverystandards (wet-weight basis), wet weight/dry weight ratio of thesediment sample, final volume of the extract, and injection volume.

2. Other documentation should include the following:

• The reconstructed ion chromatogram for each sample (or for eachsample fraction if the extract has been analyzed in distinct chemicalfractions);

• Gas Chromatography/Electron Capture Detector (GC/ECD)chromatograms for pesticide/PCB analyses, with identification of peaksused for quantitation and any confirmation chromatograms;

• Complete data for all method blanks, reported as absolute mass ofeach blank contaminant determined; samples associated with eachblank should be indicated; and

• Raw data quantitation reports, including tabulated results(identification, GC/MS scan number/retention time, area, and quantity)for compounds in each sample analyzed by GC/MS.

31

/1R30QI9

TCN 4204-01-QAPjPSECTION 10REVISION NO. 0PAGE 37 OF 5104/SEPT/90

TABLE 10-2

RECOMMENDED DOCUMENTATION FOR INDEPENDENT QA REVIEWOF DATA ON INORGANIC SUBSTANCES

To minimize the amount of backup information provided, only the "raw"instrument readings for the duplicate and spike analyses are requested.Additional backup information would only be required if a review of the QAsample data indicated the need. Data reports from the laboratory shouldinclude:

• Sample concentrations reported in proper units to the appropriatenumber of significant figures;

• Method blank data associated with each sample;

• Quantity of sample digested and final dilution volume;

• Instrument detection limit for each element (denoting method ofdetection);

• Method detection limit;

• Summary of all deviations from the prescribed methods;

. Background corrections used (e.g., Zeeman);

• Spiked sample results with associated calibration procedures andinstrument readings;

• Results from all reference materials analyzed with the samples;

• All problems associated with the analyses;

• A statemer* in the cover letter describing how standard calibrationwtie generated and applied to the samples for quantitation;

* A statement in the cover letter describing any significant problems inany aspect of sample analysis (e.g., instrumental malfunctions, softwareproblems during quantification); and

« A tabulation on standard data sheets of instrument mass detectionlimits.

32

AK300I 92

TCN 4204-01-QAPjPSECTION 11REVISION NO. 1PAGE 38 OF _____26/NOV/90______

11.0 INTERNAL QC CHECKS

Quality control of the analytical data will involve both the collectionof field sample duplicates and blanks, spiking of samples by the laboratoryQA/QC coordinator, laboratory analysis of samples, and evaluation of thedata. In addition to the procedures for sample collecting and handlingdescribed in the FSP, all laboratory quality control procedures specifiedin the organic and inorganic CLP SOW, and methods specified in the SASrequests will be implemented. Quality control checks in the field willconsist of blank and duplicate samples, peer review, and potential fieldaudits. The FSP will detail the data quality objectives and specify thenumber and type of QC samples necessary to meet these objectives.

The CLP QC program for organic and inorganic routine laboratory analysisis structured to provide consistent results of known and documentedquality. The program places stringent quality control requirements on alllaboratories performing sample analyses. Any data package in whichspecific samples do not meet CLP QA/QC criteria will be brought to theattention of the MAM by the Tetra Tech QAO. The WAM will discuss with theTetra Tech QAO the appropriateness of using analytical results of samplesin which their counterpart blanks, spikes, replicates, and duplicates arenot within these standards.

**VC* •"

Field QC procedures will be limited to field calibrations described inSection 8.0 and cross-contamination preventive procedures. All draft andfinal reports generated are subject to internal QA review procedures. Allreports are reviewed by a number of the senior technical review staff for

33

A-R300I93


each project deliverable. Any revisions or corrections required by thesenior technical reviewer are incorporated into the report before itsrelease to USEPA.

34

TON 4204-01-QAPjPSECTION 12REVISION NO. 1PAGE 40 OF "5126/NOV/9Q_____

12.0 PERFORMANCE AND SYSTEM AUDITS

Audits shall be performed to ascertain whether the QAPjP is being correctlyimplemented, and to review and evaluate the adequacy of field andlaboratory performance, where applicable. At least one unannouncedperformance audit will be conducted during field activities. Follow-upaudits shall be conducted should inconsistencies or problems be identified.The audits, to be conducted by the Tetra Tech QAO or designated Tetra Techpersonnel, will assess the effectiveness of the QA program, identify non-conformances, and verify that identified deficiencies are corrected.Audits, at a minimum, shall evaluate:

• project responsibilities;• sample handling and custody procedures;• document/data management control;• sample identification; and• corrective action procedures.

An example of the Tetra Tech performance and system audit protocol islocated in Appendix D.

The results of all audits shall be reported according to the proceduresoutlined in Section 16.0, Quality Assurance Reports to Management.

35

flR300!95

TON 4204-01-QAPjPSECTION 13REVISION NO. 0PAGE 41 OF 5104/SEPT/90____

13.0 PREVENTIVE MAINTENANCE

Preventive maintenance of equipment is essential if project resources areto be used cost-effectively. Preventive maintenance will take two forms:(1) a schedule of preventive maintenance activities to minimize downtimeand ensure accuracy of measurement systems and (2) availability of criticalspare parts and backup systems and equipment. The preventive maintenanceapproach for specific pieces of equipment used in sampling, monitoring,and documentation will follow manufacturers specifications and good fieldand laboratory practices. Performance of these maintenance procedures willbe documented in the field notebooks.

Field instruments, in general, will be maintained in accordance withmanufacturers' specifications. Contracts on major instruments withmanufacturers and service agencies are used to provide routine preventativemaintenance and to ensure rapid response for emergency repair service.Minimal instrument downtime is experienced through the use of thesecontracts, as well as through the availability of back-up equipment.

Support equipment, including safety devices, pumps, vehicles, etc., arealso periodically inspected to maintain performance standards necessaryfor all site activities.

While on-site, all equipment maintenance and coordination is theresponsibility of the Field Task Manager.

36

AR300J 96

rTCN 4204-01-QAPjPSECTION 14REVISION NO. 0PAGE 42 OF 5104/SEPT/90

14.0 SPECIFIC PROCEDURES TO BE USED TO ASSESS DATA PRECISION, ACCURACY,REPRESENTATIVENESS, AND COMPLETENESS

Routine procedures to be used for measuring precision and accuracy oflaboratory data include use of replicate analyses, matrix spikes, andprocedural blanks. Replicate matrix spikes and method blanks are analyzedroutinely through the Contract Laboratory Program.

Accuracy as measured by analysis of SRM or regional reference material willbe determined by comparing the measured value with the 95 percentconfidence interval established for each analyte.

Completeness will be measured for each set of data received by dividingthe number of valid measurements actually obtained by the number of validmeasurements that were planned.

Specific equations regarding precision, accuracy, and completeness aredetailed in Tetra Tech SOP, Assessment of Data Precision. Accuracy.Representativeness. Comparability, and Completeness (PARCC) (Appendix E).

All data sets shall be evaluated for the PARCC parameters by the QAOfficer.

37

• AR300I97


15.0 CORRECTIVE ACTION

The WAM has primary responsibility for taking corrective action; if he/sheis unavailable, the Tetra Tech QAO shall be contacted for instructions.

Any problems resulting in loss of data or reduction in data integrity willbe reported by the program manager to USEPA RPM.

Some of the types of problems and corrective actions to be taken are listedbelow:

Performance/System Audits

If problems are detected by the Tetra Tech QAO during any audit:

• The QAO shall immediately notify the field/lab person responsible,the WAN, and the program manager of the problem(s) and any action(s)he has taken.

• The WAM and the responsible field/lab person shall correct theproblem, then notify the QAO.

• The QAO shall then prepavv anu send a problem/action-taken memo tothe program manager and the WAM.

*>38

flR300!98 r

TCN 4204-01-QAPjPSECTION 15REVISION NO. 0PAGE 44 OF 5104/SEPT/90

Data Outside Control Limits

If any time the data falls outside the control limits detailed inSection 5.0 (Quality Assurance Objectives), the field and/or lab personthat observes data problems, shall immediately notify the WAM. The WAM,once aware of the data problems, shall decide on the severity of theproblem and take the appropriate action:

• Minimal data loss: The problem/corrective action taken shall bedocumented; no further action is necessary.

• Moderate data loss: A problem memo shall be prepared and sent to theUSEPA RPM and the USEPA QAO; a collective decision on the appropriateaction shall then be taken.

• Severe data loss; A problem memo shall be prepared and sent to theUSEPA RPM and the USEPA QAO.

The WAM shall then implement the corrective action, document the problemand action taken on the Corrective Actions Checklist (Table 15-1), andprepare and send a problem/action-taken memo to the USEPA RPM and USEPAQAO.

Loss of Data

The WAM shall investigate the problem, then perform one or more of thefollowing actions:

39

/IR300I99

TABLE 15-1CORRECTIVE ACTIONS CHECKLIST

Sample Program Identification:

Sampling Dates:

Material to be Sampled:

Measurement Parameter:

Acceptable Data Ranee:

Corrective Actions Initiated Bv:

Title: Date:

Problem Areas Requiring Corrective Action:

TCN 4204-01 -QAPjPSECTION 15REVISION NO. 0PAGE 45 OF Jl_04/SEPT/90

Measures to Correct Problems:

Means of Detecting Problems (field observations, systems audit, etc.):

Approval for Corrective Action:

Title: Date:

Signature:

40

AR300200

TCN 4204-01-QAPJPSECTION 15REVISION NO. 0PAGE 46 OF 5104/SEPT/90_____

• If the loss occurred in the field, a staff member shall be sent to thesite to correct the problem. If a major problem is then discovered,the staff member shall contact the WAM for additional instructions.

• If the loss occurred in-house, the WAM shall correct the problem.

• If the problem is limited in scope, the problem/action taken isdocumented; the WAM then prepares and sends a problem/action-taken memoto the USEPA RPM and the USEPA QAO.

• If a large quantity of data are affected, the problem/action taken isdocumented; the WAM then prepares and sends a problem/action-taken memoto the USEPA RPM and the USEPA QAO.

Significant QA Problems

In general, the WAM shall identify technical problems.

• The WAM prepares and sends a problem memo to the USEPA RPM and theUSEPA QAO; if the problems are significant, the action is determinedcollectively.

T'"T\

• The action taken is documented.

. For problems concerning protocol or loss of QA, the corrective actiondecision flow is presented in Figure 15-1.

41

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42 AR300202


16.0 QUALITY ASSURANCE REPORTS TO MANAGEMENT

Review of the appropriateness and adequacy of the QA Program is on-going.Inspections and audits shall be conducted during the course of the workassignment, as detailed in Section 12.0, Performance and Systems Auditsand Frequency. Within 20 workings days of the completion of the audit,the Tetra Tech QAO and/or a representative shall prepare and submit anaudit report to the WAM, with copies forwarded to the USEPA RPM, andorganization or group audited.

The report shall address, at a minimum, the following aspects:• Staff qualifications;• Equipment maintenance records;• Equipment calibration records;• Protocol adherence;• Documentation practices;• Sample traceability and control;. Data traceability and document control;• Record keeping practices;• Review and validation practices;« Computation practices;• QC data and practices; and• QA compliance.

Within 30 days after receipt of the audit report, the WAM will prepare andsubmit to the QAO a reply to the audit. This reply shall include a plan

43

^300203


for implementing the corrective actions to be taken (including a scheduleof action) as well as measures to prevent reoccurrence. The reply shallalso address revisions, where required, of the QAPjP. The QAO willascertain the effectiveness of corrective actions (by re-audit or otherverification) and issue a final audit report detailing corrective actionsand the audit closed.

The WAM will report a summary of QA audit results to the USEPA RPM andUSEPA QAO after the close of each audit. Once all audits are complete,a final QA report shall be prepared to summarize:

• QA management;• Measures of data quality from the project;• Summary of quality problems, quality accomplishments, and corrective

actions taken;• Summary of QA performance and system audits;• Data quality assessment;• Documentation of QA related training; and. Status of QAPjP.

44

flR30020l*


17.0 REFERENCES

Tetra Tech. 1990 Draft Work Plan, Volume I (Technical) RemedialInvestigation/Feasibility Study, the Butz Landfill, Jackson Township,Pennsylvania. Prepared for U. S. Environmental Protection Agency,Region III. Tetra Tech Inc., Newark, DE.

Tetra Tech. 1988 Draft Quality Assurance/Quality Control Program Plan,ARCS Contract No. 68-W8-0092. Prepared for U. S. EnvironmentalProtection Agency, Region III. Tetra Tech, Inc., Fairfax, VA.

U. S. Environmental Protection Agency. 1984 (revised January 1985).USEPA Contract Laboratory Program Statement of Work for OrganicsAnalysis, Multimedia, Multiconcentration. IFB WA85-T176, T177, T178.USEPA, Washington, D.C.

U. S. Environmental Protection Agency. 1985a US USEPA Contract LaboratoryProgram Statement of Work for Inorganic Analysis, Multimedia, Multi-Concentration. SOW No. 785. July 1985. Environmental MonitoringSupport Laboratory, USEPA, Las Vegas, NV.

U. S. Environmental Protection Agency. 1988a Laboratory Data Validation -Functional Guidelines for Evaluating Organic Analyses. Prepared forHazardous Site Evaluation Division. February 1988. USEPA,Washington, D.C.

45


U. S. Environmental Protection Agency. 1988b Laboratory Data Validation -Functional Guidelines; for Evaluating Inorganic Analyses. Preparedfor Hazardous Site Evaluation Division. June 1988. USEPA,Washington, D.C.

U. S. Environmental Protection Agency. 1988c Region III Modifications tothe Inorganic Functional Guidelines. June 1988 Region III CRL,USEPA, Annapolis, MD.

U. S. Environmental Protection Agency. 1988d Region III Modificationsto the Organic Functional Guidelines. June 1988. Region III CRL,USEPA, Annapolis, MD.

46

AR30G2Q6

TCN 4204-01-QAPjPSECTION AREVISION NO. 0PAGE NA OF -NA04/SEPT/90_____

APPENDIX A

SPECIAL ANALYTICAL SERVICES (SAS) REQUESTS

R30D207

U. S. Environmental Protection Agency SAS NumberHWI Sample Management OfficeP. 0. Box 818 Alexandria, VA 22313PHONE (703) 557-2490 or FTS 557-2490

SPECIAL ANALYTICAL SERVICESRegional Request

__ Regional Transmittal __ Telephone Request

A. EPA Region and Client: EPA Region III

B. Regional Representative: Colleen K. Walling

C. Telephone Number: (301) 266-9180

0. Date of Request: September 4, 1990

E. Site Name: Butz Landfill

Please provide below a description of your request for Special AnalyticalServices under the Contract Laboratory Program. In order to most efficientlyobtain laboratory capability for your request, please address the followingconsiderations, if applicable. Incomplete or erroneous information may resultin delay in the processing of your request. Please continue response onadditional sheets, or attach supplementary information as needed.

The awarded laboratory is responsible for meeting all requirements as specifiedin this client request. Any changes in method(s) or other specifications mustbe approved by Region III prior to the award. The referenced Statement of Workmust be used including all current revisions of that SOW. If these stipulationsare not met, Region III will recommend review for reduced payment.

description of analytical service requested:

Analysis of 20 low concentration aqueous samples for Total Suspended Solids(TSS), Total Dissolved Solids (TDS), Chemical Oxygen Demand (COD), TotalOrganic Carbon (TOC), and Alkalinity (ALK).

A-l/1R30G208

2. Definition and number of work units involved (specify whether whole samplesor fractions; whether organics or inorganics; whether aqueous or soil andsediments; and whether low, medium, or high concentration):

16 low concentration aqueous (surface water) samples;1 field duplicate;1 matrix spike (MS) and matrix spike duplicate (MSD) pair;1 field blank; and1 equipment rinseate blank.

3. Program (specify whether Superfund (Remedial or Enforcement), RCRA, NPDES,etc.), and justification for analysis and Site Account Number:

SUPERFUND Remedial

SAS Approved by:

4. Estimated date(s) of collection:

OCTOBER 1 through OCTOBER 15, 1990

5. Estimated date(s) and method of shipment:

Samples will be shipped within 24 hours after collection if labs areavailable. Shipment will be by an overnight carrier.

6. Required number of days results required after receipt of lab samples:

Data packages are due within 35 days of laboratory receipt of samples.Samples must be analyzed within the required CLP holding times.

7. Analytical protocol required (attached copy if other than a protocolcurrently used in this program):

TDS - EPA Method 160.4TSS - EPA Method 160.2COD - EPA Method 410.1 .TOC - EPA Method 415.1ALK - I-PA Method 310.1

8. Special technical instructions (if outside protocol requirements, specifycompound names, CAS numbers, detection limits, etc.):

Alkalinity - Do not open sample bottle before analysis.

9. Analytical results required (if known, specify format for date sheets, QA/QCreports, Chain-of-Custody documentation, etc.). If not completed, formatof results will be left to program discretion.

Data package must include: all raw data, all instrument and/or equipmentcalibration results, calculations, blank results, duplicate results, chain-of-custody forms, SAS request forms, SAS packing list(s) or trafficreport(s), copy of air bill(s), and copies of analyst's logbooks (signedby analyst) with date and time of sample preparation and analysis.

The cover page and all sample report forms MUST be labeled with the completeEPA sample number as it appears on the chain-of-custody and CLP paperwork.

The case narrative must document all problems encountered and subsequentresolutions. List instrumentation and methods employed for analysis. Also,note whether samples were preserved and, if so, the procedure used inpreservation.

10. Other (use additional sheets or attach supplementary information, asneeded):

11. Name of sampling/shipping contact: Christopher Burns (302) 738-7551

32, Data RequirementPrecision Desired

Parameter Detection Limit (+ or - Concentration)

TDS As per Method 160.4 As per Method 160.4TSS As per Method 160.2 As per Method 160.2COD As per Method 410.1 As per Method 410.1TOC As per Method 415.1 As per Method 415.1ALK As per Method 310.1 As per Method 310.1

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13. QC RequirementsLimits

Audits Required Frequency of Audits (Percent or Concentration)

IDS As per Method 160.4 As per Method 160.4TSS As per Method 160.2 As per Method 160.2COD As per Method 410.1 As per Method 410.1TOC As per Method 415.1 As per Method 415.1ALK As per Method 310.1 As per Method 310.1

14. Action required if limits are exceeded

If problems occur, contact ERA Region III and SMO immediately for furtherinstructions.

15. Request prepared by: Christopher Bums

16. Request reviewed by:

Date:

Please return this request to the Sample Management Office as soon as possibleto expedite processing of your request for special analytical services. Shouldyou have any questions or need any assistance, please contact your Regionalrepresentative at the Sample Management Office.

A"4 A R 3 G 0 2 I I

RESIDUE, VOLATILE

Method 160.4 (Gravimetric, Ignition at 550°C)

STORE! NO. Total 00505Non-Filterable 00535

Filterable 00520

1. Scope and Application1.1 This method determines the weight of solid material combustible at 550°C.1.2 The test is useful in obtaining a rough approximation of the amount of organic matter

present in the solid fraction of sewage, activated sludge, industrial wastes, or bottomsediments.

2. Summary of Method2.1 The residue obtained from the determination of total, filterable or non-filterable residue

is ignited at 550°C in a muffle furnace. The loss of weight on ignition is reported as mg/1volatile residue.

3. Comments3.1 The test is subject to many errors due to loss of water of crystallization, loss of volatile

organic matter prior to combustion, incomplete oxidation of certain complex organics,and decomposition of mineral salts during combustion.

3.2 The results should not be considered an accurate measure of organic carbon in thesample, but may be useful in the control of plant operations.

3.3 The principal source of error in the determination is failure to obtain a representativesample.

4. Sample Handling and Preservation4.1 Preservation of the sample is not practical; analysis should begin as soon as possible.

Refrigeration or icing to 4°C, to minimize microbiological decompostion of solids isrecommended.

5. Precision and Accuracy5.1 A collaborative study involving three laboratories examining four samples by means of

ten replicates showed a standard deviation of 111 mg/1 at 170 mg/1 volatile residueconcentration.

6. Reference6.! The procedure ro be used for this determination is found in:

Standard Methods for the Examination of Water and Wastewater, 14th Edition, p 95,Method 208E,( 1975).

Approved for NPDESIssued 1971

A"5 AR3002I2

r-i

RESIDUE, NON-FILTERABLE

Method 160.2 (Gravimetric, Dried at 103-105'C)

STORE! NO. 00530

1. Scope and Application1.1 This method is applicable to drinking, surface, and saline waters, domestic and industrial

wastes.1.2 The practical range of the determination is 4 mg/1 to 20,000 mg/1.

2. Summary of Method2.1 A well-mixed sample is filtered through a glass fiber filter, and the residue retained on the

filter is dried to constant v/eight at 103-105°C.2.2 The filtrate from this method may be used for Residue, Filterable.

3. Definitions3.1 Residue, non-filterable, is defined as those solids which are retained by a glass fiber filter

and dried to constant weight at 103-105*C.4. Sample Handling and Preservation

4.1 Non-representative particulates such as leaves, sticks, fish, and lumps of fecal mattershould be excluded from the sample if it is determined that their inclusion is not desiredin the final result.

4.2 Preservation of the sample is not practical; analysis should begin as soon as possible.Refrigeration or icing to 4*C, to minimize microbiological decomposition of solids, isrecommended.

5. Interferences5.1 Filtration apparatus, filter material, pre-washing, post-washing, and drying temperature

are specified because these variables have been shown to affect the results.5.2 Samples high in Filterable: Residue (dissolved solids), such as saline waters, brines and

some wastes, may be subject to a positive interference. Care must be taken in selecting thefiltering apparatus so that washing of the filter and any dissolved solids in the filter (7.5)minimizes this potential interference.

6. Apparatus6.1 Glass fiber filter discs, without organic binder, such as Millipore AP-40, Reeves Angel

934-AH, Gelman type A./E, or equivalent.NOTE: Because of the physical nature of glass fiber filters, the absolute pore size cannotbe controlled or measured. Terms such as "pore size", collection efficiencies and effectiveretention are used to define this property in glass fiber filters. Values for these parametersvary for the filters listed above.

6.2 Filter support: filtering apparatus with reservoir and a coarse (40-60 microns) fritteddisc as a filter support.


AR3002I3

NOTE: Many funnel designs are available in glass or porcelain. Some of the mostcommon are Hirsch or Buchner funnels, membrane filter holders and Gooch crucibles.All are available with coarse fritted disc.

6.3 Suction flask.6.4 Drying oven, 103-105°C.6.5 Desiccator.6.6 Analytical balance, capable of weighing to 0.1 mg.Procedure7.1 Preparation of glass fiber filter disc: Place the glass fiber filter on the membrane filter

apparatus or insert into bottom of a suitable Gooch crucible with wrinkled surface up.While vacuum is applied, wash the disc with three successive 20 ml volumes of distilledwater. Remove all traces of water by continuing to apply vacuum after water has passedthrough. Remove filter from membrane filter apparatus or both crucible and filter ifGooch crucible is used, and dry in an oven at 103-105°C for one hour. Remove todesiccator and store until needed. Repeat the drying cycle until a constant weight isobtained (weight loss is less than 0.5 mg). Weigh immediately before use. After weighing,handle the filter or crucible/filter with forceps or tongs only.

7.2 Selection of Sample VolumeFor a 4.7 cm diameter filter, filter 100 ml of sample. If weight of captured residue is lessthan 1.0 mg, the sample volume must be increased to provide at least 1.0 mg of residue. Ifother filter diameters are used, start with a sample volume equal to 7 ml/cm! of filter areaand collect at least a weight of residue proportional to the 1.0 mg stated above.NOTE: If during filtration of this initial volume the filtration rate drops rapidly, or iffiltration time exceeds 5 to 10 minutes, the following scheme is recommended: Use anunweighed glass fiber filter of choice affixed in the filter assembly. Add a known volumeof sample to the filter funnel and record the time elapsed after selected volumes havepassed through the filter. Twenty-five ml increments for timing are suggested. Continueto record the time and volume increments until fitration rate drops rapidly. Addadditional sample if the filter funnel volume is inadequate to reach a reduced rate. Plotthe observed time versus volume filtered. Select the proper filtration volume as that justshort of the time a significant change in filtration rate occurred.

7.3 Assemble the filtering apparatus and begin suction. Wet the filter with a small volume ofdistilled water to seat it against the fritted support.

7.4 Shake the sample vigorously and quantitatively transfer the predetermined samplevolume selected in 7.2 to the filter using a graduated cylinder. Remove all traces of waterby continuing to apply vacuum after sample has passed through.

7.5 With suction on, wash the graduated cylinder, filter, non-filterable residue and filterfunnel wail with three portions of distilled water allowing complete drainage betweenwashing. Remove all traces of water by continuing to apply vacuum after water haspassed through.NOTE: Total volume of wash water used should equal approximately 2 ml per cm'. For a4.7 cm filter the total volume is 30 ml.

7.6 Carefully remove the filter from the filter support. Alternatively, remove crucible andfilter from crucible adapter. Dry at least one hour at 103-105°C. Cool in a desiccator andweigh. Repeat the drying cycle until a constant weight is obtained (weight loss is less than0.5 mg).

8. Calculations8,1 Calculate non-filterable residue as follows:

Non-filterable residue, mg/l =(A "

where:

A = weight of filter (or filter and crucible) 4- residue in mgB = weight of filter (or filter and crucible) in mgC = ml of sample filtered

9. Precision and Accuracy9.1 Precision data are not available at this time.9.2 Accuracy data on actual samples cannot be obtained.

Bibliography

1. NCASI Technical Bulletin No. 291, March 1977. National Council of the Paper Industry forAir and Stream Improvement, Inc., 260 Madison Ave., NY.

mflR3002!5

CHEMICAL OXYGEN DEMAND

Method 410.1 (Titrimetric, Mid-Level)

STORET NO. 00340

1. Scope and Application1.1 The Chemical Oxygen Demand (COD) method determines the quantity of oxygen

required to oxidize the organic matter in a waste sample, under specific conditions ofoxidizing agent, temperature, and time.

1.2 Since the test utilizes a specific chemical oxidation the result has no definite relationshipto the Biochemical Oxygen Demand (BOD) of the waste or to the Total Organic Carbon(TOC) level. The test result should be considered as an independent measurement oforganic matter in the sample, rather than as a substitute for the BOD or TOC test.

1.3 The method can be applied to domestic and industrial waste samples having an organiccarbon concentration greater than 50 mg/lv-Fer-iowerconcentrations of carbon such asin surface-water samples, the Low-Level Modification-should-boused. When the chlorideconcentration of the sample exceeds 2000 mg/1, the modification for saline waters isrequired.

2. Summary of Method2.1 Organic and oxidizable inorganic substances in the sample are oxidized by potassium

dichromate in 50% sulfuric acid solution at reflux temperature. Stiver sulfate is used as acatalyst and mercuric sulfate is added to remove chloride interference. The excessdichromate is titrated with standard ferrous ammonium sulfate, usingorthophenanthroline ferrous complex as an indicator.

3. Sampling and Preservation3.1 Collect the samples in glass bottles, if possible. Use of plastic containers is permissible if it

is known that no organic contaminants are present in the containers.3.2 Biologically active samples should be tested as soon as possible. Samples containing

settleable material should be well mixed, preferably homogenized, to permit removal ofrepresentative aiiquots.

3.3 Samples should be preserved with sulfuric acid to a pH < 2 and maintained at 4'C untilanalysis.

4. Interferences4.1 Traces of organic material either from the glassware or atmosphere may cause a gross,

positive error,4.1.1 Extreme care should be exercised to avoid inclusion of organic materials in the

distilled water used for reagent preparation or sample dilution.4.1.2 Glassware used in the test should be conditioned by running blank procedures to

eliminate traces of organic material.

Approved for NPDESIssued 1971Editorial revision 1978

4.2 Volatile materials may be lost when the sample temperature rises during the sulfuric acidaddition step. To minimize this loss the flask should be cooled during addition of thesulfuric acid solution.

4.3 Chlorides are quantitatively oxidized by dichromate and represent a positiveinterference. Mercuric sulfate is added to the digestion flask to complex the chlorides,thereby effectively eliminating the interference on all but brine and estuarine samples.

5. Apparatus5.1 Reflux apparatus: Glassware should consist of a 500 ml Erlenmeyer flask or a 300 ml

round bottom flask made of heat-resistant glass connected to a 12 inch Allihn condenserby means of a ground glass joint. Any equivalent reflex apparatus may be substitutedprovided that a ground-glass connection is used between the flask and the condenser.

6. Reagents6.1 Distilled water: Special precautions should be taken to insure that distilled water used in

this test be low in organic matter.6.2 Standard potassium dichromate solution (0.250 N): Dissolve 12.259 g K2Cr2O7, primary

standard grade, previously dried at 103*C for two hours, in distilled water and dilute to1000ml.

6.3 Sulfuric acid reagent: Cone. H2SO4 containing 23.5g silver sulfate, Ag2SO4, per 4.09kgbottle. With continuous stirring, the silver sulfate may be dissolved in about 30 minutes.

6.4 Standard ferrous ammonium sulfate (0.25 N): Dissolve 98.0 g of Fe(NH4)2(SO4)2«6H:Oin distilled water. Add 20 ml of cone. H2SO4 (6.8), cool and dilute to 1 liter. This solutionmust be standardized daily against standard K2Cr2O7 solution (6.2).6.4.1 Standardization: To approximately 200 ml of distilled water add 25.0 ml of 0.25 N

K2Cr2O7 (6.2) solution. Add 20 ml of H2SO4 (6.8) and cool. Titrate with ferrousammonium sulfate (6.4) using 1 drop of ferroin indicator (6.6). The color change issharp, going from blue-green to reddish-brown.

Normality = (ml K,Cr,O,)(0.2S)ml Fe (NH4), (SO4),

6.5 Mercuric sulfate: Powdered HgSO4.6.6 Phenanthroline ferrous sulfate (ferroin) indicator solution: Dissolve 1.48 g of 1-10

(ortho) phenanthroline monohydrate, together with 0.70 g of FeSO4»7H:O in 100 ml ofwater. This indicator may be purchased already prepared.

6.7 Silver sulfate: Powdered Ag2SO4.6.8 Sulfuric acid (sp. gr. 1.84): Concentrated H2SO4.

7. Procedure7.! " ace several boiling stones in the reflux flask, followed by 50.0 ml of sample or an

aliquot diluted to SO.O ml and 1 g of HgSO4 (6.5). Add 5.0 ml cone. H2SO4 (6.8); swirluntil the mercuric sulfate has dissolved. Place-reflux-flask in-an ics-beth and slowly add,with swirling,-25.0-ml-of 0.25 N Kj€r2Or(6.2). Now add 70 ml of sulfuric acid-silver

A-10AR3002I7

sulfate solution (6.3) to the cooled reflux flask, again using slow addition with swirlingmotion. _Caution: Care must be taken to assure that the contents of the flask are well mixed. If notT] jsuperheating may result, and the mixture may be blown out of the open end of the

_£ondenser -=LJ7.1.1 If volatile orgamcs are present in the sample, use an allihn condenser and add the

sulfuric acid-silver sulfate solution through the condenser, while cooling the flask,to reduce loss by volatilization.

7.2 Apply heat to the flask and reflux for 2 hours. For some waste waters, the 2-hour refluxperiod is not necessary. The time required to give the maximum oxidation for awastewater of constant or known composition may be determined and a shorter period ofrefluxing may be permissible.

7.3 Allow the flask to cool and wash down the condenser with about 25 ml of distilled water.If a round bottom flask has been used, transfer the mixture to a 500 ml Erlenmeyer flask,washing out the reflux flask 3 or 4 times with distilled water. Dilute the acid solution toabout 300 ml with distilled water and allow the solution to cool to about roomtemperature. Add 8 to 10 drops of ferroin indicator (6.6) to the solution and titrate theexcess dichromate with 0.25 N ferrous ammonium sulfate (6.4) solution to the end point.The color change will be sharp, changing from a blue-green to a reddish hue.

7.4 Blank-Simultaneously run a blank determination following the details given in (7.1) and(7.2), but using low COD water in place of sample.

8. Calculation8.1 Calculate the COD in the sample in mg/1 as follows:

COD, mg/liter = (A - B)N x 8,000S

where:A = milliliters of Fe(NH4)2(SO4)2 solution required for titration of the blank,B = milliliters of Fe(NH4)2 (SO4)2 solution required for titration of the sample,N = normality of the Fe(NH4)2(SO4)2 solution, andS = milliliters of sample used for the test.

9. Precision and Accuracy9.1 ' Eighty-six analysts in fifty-eight laboratories analyzed a distilled water solution

containing oxidizable organic material equivalent to 270 mg/1 COD. The standarddeviation was ±17 7C m 'l COD with an accuracy as percent relative error (bias) of-4.7%. (EPA Method Research Study 3).

Bibliography

1. Standard Methods for the Examination of Water and Wastewater, 14th Edition, p 550,Method 508 (1975).

2. Annual Book of ASTM Standards, Part 31. "Water". Standard D1252-67. p473 (1976).

A-llAR3002I8

ORGANIC CARBON, TOTAL

Method 415.1 (Combustion or Oxidation)

STORET NO. Total 00680Dissolved 00681

1. Scope and ApplicationI.I This method includes the measurement of organic carbon in drinking, surface and saline

waters, domestic and industrial wastes. Exclusions are noted under Definitions andInterferences.

1.2 The method is most appl icable to measurement of organic carbon above 1 mg/1.2. Summary of Method

2.1 Organic carbon in a sample is converted to carbon dioxide (CO2) by catalytic combustionor wet chemical oxidation. The CO2 formed can be measured directly by an infrareddetector or converted to methane (CH4) and measured by a flame ionization detector.The amount of CO2 or CH4 is directly proportional to the concentration of carbonaceousmaterial in the sample.

3. Definitions3.1 The carbonaceous analyzer measures all of the carbon in a sample. Because of various

properties of carbon-containing compounds in liquid samples, preliminary treatment ofthe sample prior to analysis dictates the definition of the carbon as it is measured. Formsof carbon that are measured by the method are:A) soluble, nonvolatile organic carbon; for instance, natural sugars.B) soluble, volatile organic carbon; for instance, mercaptans.C) insoluble, partially volatile carbon; for instance, oils.D) insoluble, paniculate carbonaceous materials, for instance; cellulose fibers.E) soluble or insoluble carbonaceous materials adsorbed or entrapped on insoluble

inorganic suspended matter; for instance, oily matter adsorbed on silt particles.3.2 The final usefulness of the carbon measurement is in assessing the potential oxygen-

demanding load of organic material on a receiving stream. This statement applieswhether the carbon measurement is made on a sewage plant effluent, industrial waste, oron water taken directly from the stream. In this light, carbonate and bicarbonate carbonare not a part of the oxygun demand in the stream and therefore should be discounted inthe final calculation or removed prior to analysis. The manner of preliminary treatment«»f f*»e i;.£.ple and instrument settings defines the types of carbon which are measured.Instrument manufacturer's instructions should be followed.


A-12

4. Sample Handling and Preservation4.1 Sampling and storage of samples in glass bottles is preferable. Sampling and storage in

plastic bottles such as conventional polyethylene and cubitainers is permissible if it isestablished that the containers do not contribute contaminating organics to the samples.NOTE 1: A brief study performed in the EPA Laboratory indicated that distilled waterstored in new, one quart cubitainers did not show any increase in organic carbon aftertwo weeks exposure.

4.2 Because of the possibility of oxidation or bacterial decomposition of some components ofaqueous samples, the lapse of time between collection of samples and start of analysisshould be kept to a minimum. Also, samples should be kept cool (4*C) and protectedfrom sunlight and atmospheric oxygen.

4.3 In instances where analysis cannot be performed within two hours (2 hours) from time ofsampling, the sample is acidified (pH < 2) with HC1 or H2SO4.

5. Interferences5.1 Carbonate and bicarbonate carbon represent an interference under the terms of this test

and must be removed or accounted for in the final calculation.5.2 This procedure is applicable only to homogeneous samples which can be injected into the

apparatus reproducibly by means of a microliter type syringe or pipette. The openings ofthe syringe or pipette limit the maximum size of particles which may be included in thesample.

6. Apparatus6.1 Apparatus for blending or homogenizing samples: Generally, a Waring-type blender is

satisfactory.6.2 Apparatus for total and dissolved organic carbon:

6.2.1 A number of companies manufacture systems for measuring carbonaceousmaterial in liquid samples. Considerations should be made as to the types ofsamples to be analyzed, the expected concentration range, and forms of carbon tobe measured.

6.2.2 No specific analyzer is recommended as superior.7. Reagents

7.1 Distilled water used in preparation of standards and for dilution of samples should beultra pure to reduce the carbon concentration of the blank. Carbon dioxide-free, doubledistilled water is recommended. Ion exchanged waters are not recommended because ofthe possibilities of contamination with organic materials from the resins.

7.2 Potassium hydrogen phthalate, stock solution, 1000 mg carbon/liter: Dissolve 0.2128 gof potassium hydrogen phthalate (Primary Standard Grade) in distilled water and diluteto 100.0 ml.NOTE 2: Sodium oxalate and acetic acid are not recommended as stock solutions.

7.3 Potassium hydrogen phthalate, standard solutions: Prepare standard solutions from the. stock solution by dilution with distilled wi>icr. ^ *"

7.4 Carbonate-bicarbonate, stock solution, 1000 mg carbon/liter: Weigh 0.3500 g of sodiumbicarbonate and 0.4418 g of sodium carbonate and transfer both to the same 100 mlvolumetric flask. Dissolve with distilled water.

AR300220

7.5 Carbonate-bicarbonate, standard solution: Prepare a series of standards similar to step7.3.NOTE 3: This standard is not required by some instruments.

7.6 Blank solution: Use the same distilled water (or similar quality water) used for thepreparation of the standard solutions.

8. Procedure8.1 Follow instrument manufacturer's instructions for calibration, procedure, and

calculations.8.2 For calibration of the instrument, it is recommended that a series of standards

encompassing the expected concentration range of the samples be used.9. Precision and Accuracy

9.1 Twenty-eight analysts in twenty-one laboratories analyzed distilled water solutionscontaining exact increments of oxidizable organic compounds, with the following results:

Increment as Precision as Accuracy asTOC Standard Deviation Bias, Bias,

_mg/Iiter TOC, mg/liter %____________mg/liter

4.9 3.93 +15.27 +0.75107 8.32 + 1.01 +1.08

(FWPCA Method Study 3, Demand Analyses)

Bibliography

1. Annual Book of ASTM Standards, Part 31, "Water", Standard D 2574-79, p 469 (1976).2. Standard Methods for the Examination of Water and Wastewater, 14th Edition, p S32,

Method 505, (1975).

A~14 n r-, f', r, f, i~. D <II h 0 U (J £ 2 i

ALKALINITY

Method 310.1 (Titrimetric, pH 4.5)

STORE! NO. 00410

1. Scope and Application1.1 This method is applicable to drinking, surface, and saline waters, domestic and industrial

wastes.1.2 The method is suitable for all concentration ranges of alkalinity; however, appropriate

aliquots should be used to avoid a titration volume greater than 50 ml.1.3 Automated titrimetric analysis is equivalent.

2. Summary of Method2.1 An unaltered sample is titrated to an electrometrically determined end point of pH 4.5.

The sample must not be filtered, diluted, concentrated, or altered in any way.3. Comments

3.1 The sample should be refrigerated at 4°C and run as soon as practical. Do not opensample bottle before analysis.

3.2 Substances, such as salts of weak organic and inorganic acids present in large amounts,may cause interference in the electrometric pH measurements.

3.3 For samples having high concentrations of mineral acids, such as mine wastes andassociated receiving waters, titrate to an electrometric endpoint of pH 3.9, using theprocedure in:Annual Book of ASTM Standards, Part 31, "Water", p 115, D-1067, Method D. (1976).

3.4 Oil and grease, by coating the pH electrode, may also interfere, causing sluggishresponse.

4. Apparatus4.1 pH meter or electrically operated titrator that uses a glass electrode and can be read to

0.05 pH units. Standardize and calibrate according to manufacturer's instructions. Ifautomatic temperature compensation is not provided, make titration at 25 ± 2* C.

4.2 Use an appropriate sized vessel to keep the air space above the solution at a minimum.Use a rubber stopper fitted with holes for the glass electrode, reference electrode (orcombination electrode) and buret.

4.3 Magnetic stirrer, pipets, flasks and other standard laboratory equipment.4.4 Burets, Pyrex 50,25 and 10 ml.

5. Reagents5.1 Sodium carbonate solution, approximately 0.05 N: Place 2.5 ±0.2 g (to nearest mg)

Na,CO3 (dried at 250*C for 4 hours and cooled in desiccator) into a 1 liter volumetricflask and dilute to the mark.


A-15n

5.2 Standard acid (sulfuric or hydrochloric), 0.1 N: Dilute 3.0 ml cone H:SOj or 8.3 ml coneHC1 to 1 liter with distilled water. Standardize versus 40.0 ml of 0.05 N Na:CO, solutionwith about 60 ml distilled water by titrating potentiometrically to pH of about 5. Liftelectrode and rinse into beaker. Boil solution gently for 3-5 minutes under a watch glasscover. Cool to room temperature. Rinse cover glass into beaker. Continue titration to thepH inflection point. Calculate normality using:

Ax B53.00 x C

where:A = g Na2CO3 weighed into 1 literB = ml Na2CO3 solutionC = ml acid used to inflection point

5.3 Standard acid (sulfuric or hydrochloric), 0.02 N: Dilute 200.0 ml of 0.1000 N standardacid to 1 liter with distilled water. Standardize by potentiometric titration of 15.0 ml 0.05N Na2CO3 solution as above.

6. Procedure6.1 Sample size

6.1.1 Use a sufficiently large volume of titrant (> 20 ml in a 50 ml buret) to obtain goodprecision while keeping volume low enough to permit sharp end point.

6.1.2 For < 1000 mg CaCO3/l use 0.02 N titrant6.1.3 For > 1000mgCaCO3/l use 0.1 N titrant6.1.4 A preliminary titration is helpful.

6.2 Potentiometric titration6.2.1 Place sample in flask by pipetting with pipet tip near bottom of flask6.2.2 Measure pH of sample6.2.3 Add standard acid (5.2 or 5.3), being careful to stir thoroughly but gently to allow

needle to obtain equilibrium.6.2.4 Titrate to pH 4.5. Record volume of titrant.

6.3 Potentiometric titration of low alkalinity6.3.1 For alkalinity of <20 mg/1 titrate 100-200 ml as above (6.2) using a 10 ml

microburet and 0.02 N acid solution (5.3).6.3.2 Stop titration at pH in range of 4.3-4.7, record volume and exact pH. Very

carefully add titrant to lower pH exactly 0.3 pH units and record volume.7. Calculations

7.1 Potentiometnc titration to pii 4. S

Alkalinity, mg/1 CaCO3 = *" v 3 ml of sample

. ,-,H i 1 U U U

where:A = ml standard acidN = normality standard acid . <.'•'(

7.2 Potentiometric titration of low alkalinity:

Total alkalinity, mg/1 CaCO, =6 J (2B " ? * N x,mi of sample

where:B = ml titrant to first recorded pHC = total ml titrant to reach pH 0.3 units lowerN = normality of acid

8. Precision and Accuracy8.1 Forty analysts in seventeen laboratories analyzed synthetic water samples containing

increments of bicarbonate, with the following results:

Increment as Precision as Accuracy asAlkalinity Standard Deviation Bias. Bias,

mg/liter. CaCO, mg/liter, CaCO3 % mg/1, CaCO,

8 1.27 +10.61 +0.859 1.14 +22.29 +2.0

113 5.28 - 8.19 -9.3119 5.36 - 7.42 -8.8

(FWPCA Method Study 1. Mineral and Physical Analyses)

8.2 In a single laboratory (EMSL) using surface water samples at an average concentrationof 122 mg CaCOj/1, the standard deviation was 13.

Bibliography

1. Standard Methods for the Examination of Water and Wastewater, 14th Edition, p 278,Method 403, (1975).

2. Annual Book of ASTM Standards, Part 31, "Water", p 113, D-1067, Method B, (1976).

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D. Date of Request: September 4, 1990




1. General description of analytical service requested:

Analysis of 20 low concentration sediment samples for Total Organic Carbon(TOC)•

A-18AR300225


16 low concentration sediment samples;1 field duplicate;1 matrix spike (MS) and matrix spike duplicate (MSD) pair;1 field blank; and1 equipment rinseate blank.

3. Program (specify whether Superfund (Remedial or Enforcement), RCRA, NPDES,etc.)f and justification for analysis and Site Account Number:

SUPERFUND Remedial

SAS Approved by:








^^ TOC - Army Corps of Engineers Method CE80 and CE81

A-19 ,....,.-,/-! i i J U U £ 2. b




The cover page and all sample report forms MUST be labeled with the completeERA sample number as it appears on the chain-of-custody and CLP paperwork.




12. Data RequirementsPrecision Desired

Parameter Detection Limit (+ or - Concentration)

TOC's As per Method CE80 & As per Method CE80 &Method CE81 Method CE81

A-20/4R30G227



As per Method CE80 & As per Method CE80 &Method CE81 Method CE81



15. Request prepared by: Christopher Burns


Date:


A"21 . fiR3D0228

&EPAAD/A103 ~cc

ENVIRONMENTAL PROTECTION AGENCY/E CORPS OF ENGINEERSTECHNICAL COMMITTEE ON CRITERIAFOR DREDGED AND FILL MATERIAL

by

Russell H. Plumb. Jr.1Great Lakes Laboratory

State University College at Buffalo1300 Elmwood Avenue

Buffalo. New York 14222

May 1981

Tiifltar pul.ic r«lcc*o u=-.d bt:l«»; t

ia

u S Environmental Protection Agency/Corps ofengineers Technical Committee on Critena

9 for Dredged and Fill Materialu co 'EPA-4805572010

MMui 4ki Large Lakes LaboratoryUS Environmental Protection > 3 ^y

9311 Groh RoadGrosse Me, Michigan 48138

Box 631. Vicksburg. Miss.ss.pp. 39180

TSflBNAL TECHNICALINPORMATION SERVICE

A-22 AR300229

CARBON, TOTAL ORGANIC AND INORGANIC

Carbon may exist in sediment and water samples as either

inorganic or organic compounds. Inorganic carbon is present as carbo-nates, bicarbonates, and possibly free carbon dioxide. Specific typesof compounds that are considered to be included in the organic carbonfraction are nonvolatile organic compounds (sugars), volatile organiccompounds (mercaptans), partially volatile compounds (oils), andparticulate carbonaceous materials (cellulose).7'2

The basis of the method is the catalytic or chemicaloxidation of carbon in carbon-containing compounds to carbon dioxidefollowed by the quantification of the carbon dioxide produced.Alternately, the carbon may be reduced to methane and appropriatelyquantified. It follows, then, that the distinction between inorganic

carbon and organic carbon is the method of sample pretreatsent. Thereare presently tvo procedures for defining this separation. One methodis based on sample treatment with a strong acid. Analysis of anuntreated sample is a measure of total carbon while analysis of theacid-treated fraction is a measure of organic carbon. Inorganic carbonis calculated by subtraction. The second method of separation isbased on differential thermal combustion with organic compounds beingconverted to carbon dioxide at 500°C to 650°C3*1* and inorganic carbonbeing converted to carbon dioxide at 950°C to 1300°C.1"5

Sample Handling and Storage

Flowcharts for the handling of samples intended for organiccarbon and inorganic carbon analysis are presented in Figure 3-C andFigure 3-7. Water and sediment samples to be analyzed for inorganic

( t

carbon may be stored in'glass or plastic containers. There is no'effective preservative because of the carbon dioxide reserve in theatmosphere. The only precaution that can "be taken for inorganic

* References for this procedure can be found on page 3-76.

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A-25• A 1(3002:32

carbon is to completely fill the sample container at the time ofsampling (exclude all air bubbles), tightly seal the container, andcomplete the analysis immediately (Figure 3-6).

Water samples for organic carbon analysis should be storedin glass containers unless substitute containers have been shown not.to affect total organic carbon (TOC) analyses. Samples should beprocessed as soon as possible (vithin 2k hr if possible) to minimizechange due to chemical or biological oxidation. Atmospheric uptakeof carbon dioxide is less critical since it vould be evolved when thesample is acidified prior to analysis. Sediment samples for organiccarbon analysis may be stored in either plastic or glass containers(Figure 3-7). Air drying of sediments (S2) may lead to lov TOCresults due to oxidation or volatilization. Therefore, moist storage(SID) or frozen storage (S3) vould be the preferred method of storage.If samples are frozen, excessive temperatures should not be used tothav the samples.

A-26

to R o u 0

Procedure for Water Samples (Wl, W2. S1A)

Method 1: Infrared Analysis6'7ApparatusSample homogenizer such as a Waring blender or ultrasonic blenderMagnetic stirrer

Hypodermic syringeTotal carbon analyzer, either a single channel'or a dual channel

instrument (Dov-Beckman Carbonaceous Analyzer ModelNo. 915, Dohnnann Envirotech DC-50 carbon analyzer,Oceanography International Total Carbon Analyzer, Leco,or equivalent)

ReagentsDistilled vater: the distilled vater used in the preparation of

standards and dilution of samples should be of thehighest quality in order to have a small blank.

Organic carbon, stock solution, 1000 mg/£ C: dissolve 2.125 ganhydrous potassium biphthalate, KHCs HuOi., in distilledvater and dilute to 1 I in a volumetric flask.

Organic carbon, standard solutions: prepare standard solution bydilution of the stock solution as required.

Inorganic carbon, stock solution, 1000 mg/C: dissolve 3-500 g sodiu=bicarbonate, NaHCOs, and k.klQ g sodium carbonate, NazCOa,in distilled vater in a l-£ volumetric flask and make upto the mark.

Inorganic carbon, standard solution: prepare standards,from the stocksolution-as required.

Packing for total carbon tube: dissolve 20 g cobalt nitrate,COCNOah ' 6H20, in 50 ml distilled vater. Add thissolution to 15 g long-fiber asbestos in a porcelainevaporating dish. Mix and evaporate to dryness on asteam bath. Place the dish in a muffle furnace andbring to 950°C. After 1 to 2 hr at this temperature,remove the dish and allow to cool. Break up any largelumps and mix adequately but not excessively. With thecombustion tube held in a vertical position, taper jointup, put about 1/2 in. of untreated asbestos in the tubefirst, then transfer in small amounts, approximately 1 gof catalyst into the tube vith forceps or tveezers. Asit is added, tap or push, the material gently vith a l/l»-in.glass rod. Do not force the packing. The weight of therod itself is sufficient to compress the material. Whencompleted, the length of the packing should be about 5 or6 cm. Test the packed tube by measuring the flov rate of

A"27

gas through it at room temperature, and then at 750°C.The rate should not drop more than 20 percent.

Packing for carbonate tube (dual channel instrument): place a small vadof quartz vool or asbestos near the exit end of thecarbonate evolution tube. From the entrance end add 6 to12 mesh quartz chips, allowing these to collect against thevad to a length of 10 cm. Pour an excess of 85 percentphosphoric acid, H3POi., into the tube vhile holding itvertically and allow the excess to drain out.

Nitrogen gas, carbon dioxide free.Procedure

Turn on the infrared analyzer, recorder, and tube furnaces,setting the total carbon furnace at 950°C and the carbonate furnace at175°C. Allow sufficient warm-up time for stable, drift-free operation;about 2 hr is required. If used daily, the analyzer can be left oncontinuously. Adjust the oxygen flow rate to 80 to 100 sl/mln throughthe total carbon tube. With other instruments, follow manufacturer'sdirections to warn up the instrument*.

Immediately prior to carrying out calibrations or analyses,inject several portions of the appropriate standard into the tube to beused, until constant readings are obtained. The actual injectiontechnique is as follows: rinse the syringe several times with thesolution to be analyzed, fill, and adjust the volume to be pipeted.Wipe off the excess with soft paper tissue, taking care thaft no lintadheres to the needle. Remove the plug from the syringe holder, insertthe sample syringe, and inject the sample into the combustion tube witha single, rapid movement of the thumb. Leave the syringe in the holderuntil the flow rate returns to normal, then replace it with the plug.

Successively introduce a convenient sized aliquot (20 to50 yl) of each organic carbon standard and a blank into the total carbontube and record peak heights. Between injections allow the recorderpen to return to its baseline. When a dual channel instrument is usedthe" standardization procedure must be repeated using carbonate standardsto calibrate the low temperature channel.

Thoroughly nix the sample. Inject a convenient sizedaliquot (20 to 50 yl) of the sample into the total carbon tube and

A-28AR30G235

record the peak height. This result is a measure of the organic carbonconcentration and the inorganic carbon concentration of the sanple.

Thoroughly mix the sample using a Waring blender or an ultra-sonic homogenizer. Transfer 10 to 15 ml of sample to a 30-ral beaker andacidify vith concentrated HC1 to a pH of 2 or less. Purge the samplewith carbon dioxide free nitrogen gas for 5 to 10 min. Plastic tubingshould not be used during the purging process unless it has been

previously shown that it will not add organic carbon to the sample.Mix the acidified sample on a magnetic stirrer. While

stirring, withdraw a subsample from the beaker using a hypodermicneedle with a 150-um opening. Inject the sample into the carbonanalyzer to be used and record the peak height. This result is a.measure of the organic carbon concentration of the saaple.

Using either clear or filtered water samples, analyticalprecision.will approach 1 to 2 percent or 1 to 2 mg/1 carbon, whicheveris greater. Analytical precision for unfiltered water samples willincrease to 5 to 10 percent because of the difficulty associated withsaapling particulate matter and the fact that the needle opening ofthe syringe limits the maximum size of the particles that can beincluded in the sample.Calculations

Dual-channel instrument. Prepare calibration curvesderived fron the peak heights obtained with the standard total carbonand inorganic carbon solutions.

Determine the concentration of total carbon and inorganiccarbon in the sample by comparing sample peak heights with the cali-bration curves.

Determine the concentration of total inorganic carbon inthe sample by subtracting the organic carbon value from the totalcarbon value.«

Single-channel instrument. Prepare a calibration curvederived from the peak heights obtained vith the standard total carbonsolutions. Determine the total carbon concentration in the sample bycomparing the peak height of the first sample injection vith the

A-29

AR300236

calibration curve. Determine the organic carbon concentration in thesample by comparing the peak height of the second sample injection vith

the calibration curve. Inorganic carbon concentrations are calculatedby subtracting the organic carbon concentration from the total carbonc one entrat ion.

A-30 , 0 f, -,k \\ o u u L o /

fI

_ References

1. U. S. Environmental Protection Agency. "Manual of Methods forChemical Analysis of Water and Wastes." Methods Development andQuality Assurance Research Laboratory, National EnvironmentalResearch Center; Cincinnati, Ohio. 298 p. (197 ).

2. U. S. Environmental Protection Agency. "Methods for ChemicalAnalysis Of Water and Wastes." Environmental Monitoring andSupport Laboratory, Office of Research and Development, ZPA;Cincinnati, Ohio (1979).

3- Giovannini, G., Poggio, G., and Sequi, P. "Use of an AutomaticCHN Analyzer to Determine Organic and Inorganic Carbon in Soils."Unpublished Report, Laboratory of Soil Chemistry, via Corridoni,Pisa, Italy. 9 p. (1975).

k. Konrad, J. G., Chesters, G., and Keeney, D. R. "Determination ofOrganic- and Carbonate-Carbon in Freshwater Lake Sediments by aMicrocombustion Procedure." J. Thermal Analysis 2:199-208 (1970).

5. Kemp, A. L. W. "Organic Matter in the Sediments of Lakes Ontarioand Erie." Proc. 12th Conference Great Lakes Research 12:237-2 9(1969).

6. Environment Canada. "Analytical Methods Manual," Inland WatersDirectorate, Water Quality Branch; Ottawa, Canada (197*0.

7. American Public Health Association. Standard Methods for theExamination of Water and Wastewater. APHA; New York, New York.1193 p. (1976).

8. Gaudette, H. £., Flight, W. R., Toner, L., and Folger, D. W."An Inexpensive Titration Method for the Determination of OrganicCarbon in Recent Sediments." J. Sed. Petrology W»:2l*9-253 (197M.

A-31/". I.I '.' , •. :;••• /"i t-*H i i U u U C. 0 0







D. Date of Request: September 4, 1990





Analysis of 17 low concentration sediment samples for grain size, %moisture, and % solids.

A-32


16 low concentration sediment samples;1 field duplicate;

3. Program (specify whether Superfund (Remedial or Enforcement), RCRA, NPDES,etc.), and justification for analysis and Site Account Number:

SUPERFUND Remedial

SAS Approved by:








Grain Size - (1) ASTM 0422-63(2) ASTM D421-85(3) Chapter 3 from Procedures in Sedimentary Petrology

% Moisture - (1) ASTM 02216-80% Solids - (1) EPA Method 160.3

A-33


Sieves must pass the Sieve Accuracy Testing (Chapter 3 in Procedures inSedimentary Petrology).

Contact ERA Region III or SMO for further instructions.








Parameter Detection Limit f+ or - Concentration)

Grain Size As per Method D422-63, D421-84, Chapter 3 fromProcedures in Sedimentary Petrology

% Moisture As per Method D2216-80

% Solids As per Method 160.3

A'34



Grain Size - Sieve Calibration As per Method of Chapter 3 -Procedures in Sedimentary Petrology

% Moisture - As Per Method 02216-80


If problems occur, contact EPA Region III and SMO immediately for furtherinstructions.

15. Request prepared by: Christopher Burns


Date:


A-35

Designation: D 422 - 63 (Reapproved 1972)'1 Attachment 1Page 1 of 7

Standard Method forParticle-Size Analysis of Soils1P-u standard * ;ssued under the rued designation D •<:: the number .mmed.ateh following tne Jcsunancn ndxaics -e.•ntmjUaoptionor m the case of revision, the vear oflast re%ision \ number m pjre.-.tneses .nd.catcs the -car ,i ast -j--<uc-ericnrt S2silon ••• ndicates an editonjl change since tne last revision or i " ""

F—Secfon ; *as added editonaii\ j.id (ut<<eguent sections renumbered .n Juiv •>*•*

I, Scope replaceable stimng paddle made of rr.e-.ai. plastic.I | This method covers the quantitative determination of rubber, as shown m Fig. I The shaft snail be of such Icr.r.r.

the distribution of panicle sizes in soils. The distribution of tnat tne stimng paddle will operate not less than '• m .•> )particle sizes larger than 75 urn (retained on the No. 200 Tim) nor more than I': m. i38.l mmi above the Vttcrr. or'sieve) is determined by sieving, while the distribution of the dispersion cup. A special dispersion cup .ror.for- r.E :oparticle sizes smaller than 75 urn is determined by a either of the designs show'n in Fig. 2 shall be provider :o ho.sedimentation process, using a hydrometer to secure the the sample while it is being dispersed.necessary data (Notes I and 2). 3.2.2 Apparatus B shall consist of an air-jet Jispcrs-.or.NOTE I—Separation mav be made on the No. 4 <4 ?s-mm). No, 40 CUP3 <Note conforming to the genera! details shown .n F:g.

M-5'Mrnl. or No, 200 (75-um) sieve instead of the No, 10. For whatever 3 (Notes 4 and 5).sicê used, the size shall be indicated in the report,NOTE 2—Two types of dispersion devices are provided: (/) a NOTE 3—The amount of air required b> an air-jet dispersion cup s

high-speed mechanical stirrer. and (*) air dispersion. Extensive investi- of the order of I ft'/min. some small air compressors arc not capac.c ;:'jations indicate that air-dispersion devices produce a more positive supplying sufficient air to operate a cupdispersion of plastic soils below the 20-um size and appreciably less NOTE a—Another air-type dispersion device, known as a dupersicndegradation on all sizes when used with sandy soils. Because of the tube, developed by Chu and Davidson at Iowa State College, nas wndefinite advantages favoring air dispersion, its use is recommended. The snown ,o g,ve resuits equivalent to those secured b> the a.r-et j^rerresults from the two types of devices differ in magnttude. depending cups When lt ls used xtklng of the amox ,an ^. ,..... .upon soil tvpe. leading to marked differences in panicle sue distnbu- sed.menution cvl.nder. thus eliminating the r.ccd -or irar.sfcrnrsgtion. especially for sizes finer than 20 urn. slurry Wnen ,he air lsp<:rsion tube IS used. „ snail ,0 ... >n

n tne1. Referenced Documents NoTE j_Water may condense ,„ air !ines ahen r.ot .n use Th,s1 1 -\ST\f Standards water must be removed, either by using a water trap on the air:.;r.e. or r>D421 Practice for Dry Preparation of Soil Samples for "jlowing the water out of lhe line before usm? 3n> of tnc iir •«

Particle-Size Analysis and Determination of Soil d«P««'on P«nx»es.Constants' _ 3j Hydrometer—An ASTM hydrometer, graduated to

Ell Specification for W,re-Cloth Sieves for Testing ^d in either speciHc gravity of the suspension or grams perPurposes --»,.,. 4 litre of suspension, and conforming to the requirements for

E 100 Specification for ASTM Hydrometers hydrometers 151H or I52H in Specifications E 100. Dimen-, Annaratus s'ons °^ *X)t hydrometers are the same, the scale being the, . ~ , i-i •• f t r t i r • f only item of difference.3.1 Balances-* balance sensitive to 0.01 g for weighing 3 sedimentation CvfliiAr-A glass cylinder essentiallvthe matenal passing a No. 10 (2 OO-mm) sieve and a balance 5? . h ^ n , 63 . -

sensitive to 0.1 ft of the ma« of the samp e to t,e weighed for rked for volu8me mL The diameter

S "Si23S£ ap usTSr B may be -"» •- -h that the iflOOn-L mar, ,s 36 , 2 cm from theuscd * ^ bottom on the inside.3.2.1 Apparatus A shall consist of a mechanically oper- 3.!\ Thermometer-* thermometer accurate to IT

ated stimng device in which a suitably mounted electric (°-5 c>- ,motor turns a vertical shaft at a speed of not less than 10 000 3.6 S/>v«-A series of sieves, of square-mesh woven-w,rerpm without load. The shaft shall be equipped with a cloth, conforming to the requirements of Specification E 1 !

A full set of sieves includes the following (Note 6):

1 Thu method it under UK jurisdiction of ASTM Committee D-IS on Soil andRock and n the direct responsibility of Subcommittee OII.03 on Tenure, > Detailed'<«orkin|dnvnnp for this cup are available at a nominal cost fromPUttictly. and Density Chanctenstics of Sotli. the Amencan Society for Tewm and MitenaU. 1916 Race Si.. Philadelphia, PA-

Current riiucn wprovtd NOV. 21. 1963. Onpnally published 1935. Replaces 19103. Order Adjunct No. 12-40422040. ^ fc \D 422-62. ^B ;

J Aimutl took of ASTM Standards. Vol 04.01. ^' Aiuiitfl took of ASTM SlonJarli. Vol (4.02.4 Annual look of ASTM Stunted}. Vol 14.01.

A-36 '

iljjl)) 0422 Attachment 1Page 2 of 7

t

-No. 18 3W Co «0.049'

Chrome

•Punch0.20J- io.oor

(a) (b)

Metric Equiviltnti~ 0001 0049 0203 ~—————-mm____003_____l 24_____5 16_____i£7_____'90

FIG. 1 0«uil of Sbmng Piddltf

J-m i*<-mmi NO lOOOO-mm)2-in 150-mml No ZOfgSO-umiI'-in lj'5-mmi No 40(425-umll-m clJO-mmi N0 60f?50-|jm>'«-m 1190-mm) No. |40(i06-umi''••m i9 5-mmi N'o ;00r5-um>NO 4 '4 "5-mmj

MOTE 6—A set of sieves giving uniform spacing of points for thegraph, as required in Section 17. may be used if desired. This set consistsof (he following sieves:

J-in, rj-mm) No l6(IH-mmlI'-i-m l3*5-mm) No 30 (600-um)vm il»0-mm) No 50(300-umi'i-m i« 5-mmi No. 100 (ISO-urn)No4i475-mmi No. 200 Ill-urn)NO S 12 '6-mmi

3." Water Bath or , Constant-Temperature Room—Auater bath or constant-temperature room for maintainingthe soil suspension at a constant temperature during thehvdrometer analysis. A satisfactory water tank is an insulatedtank that maintains the temperature of the suspension at aconvenient constant temperature at or near 68*F (20*C).Such a device is illustrated in Fig. 4. In cases where the workis performed in a room at an automatically controlledconstant temperature, the water bath is not necessary.3.8 Beaker—A beaker of 250-mL capacity. "• !3 ?_6 'Is3.9 Timing Device—A. watch or clock with a second -^—————=——————22——————!L:——————

hand. F1Q. 2 Oiipcrsiwi Cupt el Appar«tu«

4. Dispersing Agent be brought to the temperature that is expected to prevail4.1 A solution of sodium hexamettphosphate (sometimes during the hydrometer test. For example, if the sedimenta-

called sodium metaphosphate) shall be used in distilled or tion cylinder is to be placed in the water bath, the distilled ordemmeralized water, at the rat? of 40 g of sodium demineralized water to be used shall be brought to thehexametaphosphate/Iitre of solution (Note 7). temperature of the controlled water bath; or. if the sedimen-NOTE 7_Soluuon$ of this nil if acidic, slowly revert or hydrolyze *"<"> cylinder is used in a room with controlled tempera-

back to the orthophosphate form with a rwulunt decrease in dispersive lure, the water for the test shall be at the temperature of theaction. Solutions should be prepared frequently (at least once a month) room. The basic temperature for the hydrometer test is 68'For adjusted to pH of 8 or 9 by means of sodium carbonate. Bottles (20*Q. Small variations of temperature do not introduceconuinini solutions should have the date of preparation marked on jyi nce, tiul are of practical significance and do not1 em' prevent the use of corrections derived as prescribed.4.2 All water used shall be either distilled or

demineralized water. The water for a hydrometer test shall

A-37

•AR3QQ2M:-

Attachment 1Page 3 of 7

—» 3

FIG. 3 Air-Jot Dup«riion Cup* of Appir«tu» B

5. Test Sample5 I Prepare the test sample for mechanical analysis as

outlined in Practice D421. Dunng the preparation proce-Jure the sample is divided into two portions. One ponioncontains onl> particles retained on the No. 10 (2.00-mm)sieve y-hile the other portion contains only panicles passingthe No, 10 sieve. The mass of air-dned soil selected forpurpose of tests, as prescribed in Practice D42I. shall besufficient to yield quantities for mechanical analysis asfollows:

5.1.1 The size of the portion retained on the No. 10 sieveshall depend on the maximum size of particle, according tothe following schedule:

Nominal Diameter ofLirint Panicles, Approtimiie Minimum

in immi M»u of Portion. fv, 19 5) 500

JOOO

..;_.. JTT>._i.._._rt-« .-c:::::|:-!l.

I j

" I

-35S ™

Waltr B«Ui5.1.2 The size of the portion passing the No. 10 sieve shall

5.2 Provision is made in Section 5 of Practice D421 for s«vcs- <» •» mafly * may be needed depending on theuc,ghing of the air-dry soil selected for purpose of tests, the »mPle- or «P°n the sp«ific«ions for the material underseparation of the soil on the No. 10 sieve by dry-sieving and test- .âshing, and the weifhinf of the washed and dried fraction 6.2 Conduct the sieving operation by means ot a lateralretained on the No. 10 sieve. From these two masses the >"d ve«>< motion of the sieve, accompanied bv a jamngpercentages retained and passing the No. 10 sieve can be action m order to keep the sample moving contmuousK over

* -jrdance with 1 2. 1. tne surface of the sieve. In no case turn or manipulate

pasinitheNo. IO«eveinda«Jdin|thuvaloetotJiemMiofUiew«sh«d sieve passes that sieve dunng I mm of*nd oven-dncd portion retained on the No. 10 tieve. mechanical sieving is used, test the thoroughness of sieving

«IFVP AIMAI vc;i«! M PORTION HETAINED ON NO 10 bv using *' hand method of sievin« «* descnbcd above.SIEVE "S J RrTAINEDON NO' I0 6.3 Determine the mass of each fraction on a balanceconforming to the requirements of 3.1. At the end of

6. Procedure weighing, the sum of the masses retained on all the sieves6.1 Separate the portion retained on the No. 10 (2.00- used should equal closely the original mass of the quantity

mm) sieve into a series of fractions using the 3-in. (75-mm), sieved.

A-38flR3002i*5

<iSD> D422 Attachment 1Page 4 of 7

Pt«iNrATHFSio' m 'm YSBSr« RTIO% ! 9 2 Pla" the Umpie in lhe :50'mL beaker and -^ *"•-•P*SSI.NCTHE.NO. 10 (2.00-mm) SIEVE ,;; mL Of sodlurn hexamc!apho5ph;lle soiu!lon -, . LStir until the soil is thorough!) wetted. Allow ;0 soak ;br a:

". Determination of Composite Correction for Hjdrometer least 16 h.Readin? ^ 3 At the end of the soaking penod. disperse the samr.e" 1 Equations for percentages of soil remaining m suspen- further, using either stirring apparatus A or B If siirr.r.;

sion. as given in I J.3. are based on the use of'distilled or apparatus A is used, transfer the soil - water siurr. from :-edemmerali/eo --vater \ uispersirE agent is used in ;he water. beaker into the special dispersion cup snow-. ,n F:e 1however, and the <pe.:ik sravir. of the resulting liquid is '•'•ashing anv residue from the rx-akcr into ;he :up •*.:-appreciable greater than that of distilled or Jermncraiued distilled or Jerruncrah/ed wjter Note >• \^ j,s;.,.;J •water dcmincrahzed water, if neccssar-, so that :nc ;jp * -•..—.•

" I I Both soil hvdrometers are calibrated at 6*'F 120'Ci. than haif" ''""• Stir for a penod of ' mmand \anations in temperature from this standard tempera- VOTE •>—A -arze sus.svnnge is a comensem JCM.-; :-->r -ar.j..-? •--lure produce inaccuracies in the actual hvdromcter readings. . *aicr m me *jsnmg operation Oiher ucv:c»s .n: ,Jc me *is,-.»r."The amount of the maccuracv increases as the variation boitie and a hose »nh no«ie ronnecied w j prcssur.Kj iss-cj *ji-.--from me standard temperature increases. :ank

'.I 1 Hvdrometers are graduated by the manufacturer to 9 J If stimng apparatus B iRg. 3> is used, remove :.-.cbe read at the bottom of the meniscus formed b> the liquid cover cap and connect the cup to a compressed air suppr. :•••on the stem. Since it is not possible to secure readings of soil means of a rubber hose. A air gage must be on trie "lir.esuspensions at the bottom of the meniscus, readings must be between the cup and the control valve Open the centra.taken at the top and a correction applied. valve so that the gage indicates 1 psi i" kPai pressure :Note

7.1.3 The net amount of the corrections for the three io>. Transfer the soil - water slurrv from the beaker to trieitems enumerated is designated as the composite correction, air-jet dispersion cup by washing with distilled orand ma> be determined experimentally. demmeralized water. Add distilled or demoralized water. ,f

7.2 For convenience, a graph or table of composite necessary, so that the total volume in the cup is 250 mL. bu;corrections for a series of 1" temperature differences for the no more.range of expected test temperatures may be prepared andused as needed. Measurement of the composite corrections j .°Jjter ,,Ure' from emermflne air- e^cnamoc-"hen11°" ~"\tu"may be made at two temperatures spanning the range of ,s transferred to the dispenion cupexpected test temperatures, and corrections for the interme-diate temperatures calculated assuming a straight-line rela 9-5 ,plac,e the cov«r caP on the CUP i?"d °Pcr! :ne J:r" >nsh,p between the two observed values. contro1 valve untl1 the 8a«e Press"re 1S 20 PSi -i'5

7J Prepare 1000 mL of liquid composed of distilled or Disperse the soil according to the following scheduleeminerahzed water and dispersing agent in the same Dispcn.on Pcnouproportion as will prevail in the sedimentation (hydrometer) Plasticity index m.ntest. Place the liquid in a sedimentation cyclinder and the " 5 ?cvlmder in the constant-temperature water bath, set for one over:o !«of the two temperatures to be used. When the temperature of _ ., , , '",.__, ithe liquid becomes constant, insert the hydrometer, and. Soils containing large percentages of mica need be dispersedafter a short interval to permit the hvdrometer to come to the for on|y ' mm. After the dispersion penod. reduce the gagetemperature of the liquid, read the hydrometer at the top of Pf«?ure <° ' PSI VW*™°y to transfer of soil - water slumthe meniscus formed on the stem. For hydrometer 15IH the to the sedimentation cylinder.composite correction is the difference between this readingand one: for hydrometer I52H it is the difference between l0' Hydrometer Testthe reading and zero. Bring the liquid and the hydrometer to 10.1 Immediately after dispersion, transfer the soil - waterthe other temperature to be used, and secure the composite slurry to the glass sedimentation cylinder, and add distilledcorrection as before. or demineralized water until the total volume is 1000 mL.

10.2 Using the palm of the hand over the open end of the8 HvzroscoDic Moisture cylinder (or a rubber stopper in the open end), turn theo. Hygroscopic Moisture cylinder upside down and back for a penod of I mtn to

8.1 When the sample is weighed for the hydrometer test, comr>lete the agitation of the slurry (Note 11). At the end of,weigh out an auxiliary portion of from 10 tr »5 i in a small , Uljn xl tne cylinder in a convenient location and takemetal or glass container, dry the sample to a constant mass in hydrometer readings at the following intervals of timean oven at 230 ± 9'F (110 ± 5*C). and weigh again. Record (measured from the beginning of sedimentation), or as manythe masses. u may needed, depending on the sample or the specifica-

tion for the material under test: 2. S. 15. 30, 60. 250. and9. Dispersion of Soil Simple 1440 min. If the controlled water bath is used, the sedimen-

9.1 When the soil is mostly of the clay and silt sizes, weigh »'">" cylinder should be placed in the bath between the 2-out a sample of air-dry soil of approximately 50 g. When the and 5'mm readings.soil is mostly sand the sample should be approximately 100 NOTE it—The number of turns during this minute should beg. approximately 60, counting the turn upside down and back as two turns.

A-39

in «

Attachment 1<®>D422 Page 5 of 7

soil remaining in the bottom of the cylinder dunng the first few TABLE 1 V«lu«i ol CorrtcHon Fietor. a. for Oiff»r»ni Specificshould be loosened by vigorous shaking of the cylinder while it is _________ Grtvitiii of Soil Ptrticltt*inverted

lOJ When it is desired to take a hydrometer reading. J95 o9<ârcl'ully insert the hydrometer about 20 to 25 s before the *9° J35reading is due to approximately the depth it will have when 280 *|*the reading is taken, As soon as the reading is taken, carefully 2 75 o 38•cmove the hydrometer and place it wuh a spinning motion J 7° :39ltl a graduate of clean distilled or demmeralized water 2°* ;^

SiifE I-—It is important to remove the hydrometer immediatelv ^5 '22jKf each reading Readings shall be uken at the lop of the "nemscus i *? j *3yrmcd bv the suspension around the stem, since it is not possible to '

readings at the bottom of the meniscus. ' Bof us* n•ouauon 'or oe'certage of son 'emainng r s-sae"s<x- *-<r s.--;Mydromettr '52H

10J After each reading, take the temperature of thesuspension by inserting the thermometer into the suspcn- ,4 ; Calculate the mass of a total sample represented bv5|ljni the mass of soil used in the hydrometer test, by dividing the

oven-dry mass used by the percentage passing the No .0II. Sieve Analysis (2.00-mmi sieve, and multiplying the result by 100 This

11 I After taking the final hydrometer reading, transfer va'u« 'S the weight W in the equation for percentagethe suspension to a No. 200 (75-um) sieve and wash with up remaining in suspension.viatcr until the wash water is clear. Transfer the material on l4-3 The percentage of soil remaining in suspension at the(he No. 200 sieve to a suitable container, dry in an oven at level at which the hydrometer is measuring the density of the;30 ± 9*F 1110 ± 5'Q and make a sieve analysis of the suspension may be calculated as follows .Note 13): Forportion retained, using as many sieves as desired, or required hydrometer 151H:for the material, or upon the specification of the material p . [(iooooo/W) x GKG - C,',](R - c,junder test. ÔTE |j_The bracketed portion of the equation for hvdrometer

151H is constant for a series of readings and may be calculated first andCALCfLATIONS AND REPORT then multiplied by the portion in the parentheses.

For hydrometer I52H:12. Sieve Analysis Values for the Portion Coarser than the p, (na/w} x

No. 10 (2.00-mm) Sieve12 1 Calculate the percentage passing the No. 10 sieve by * "e-correct,on faction to be applied to the reading of

jiv.d.ng the mass passing the No. 10 sieve by the mass of soil hydrometer 152H. (Values shown on the scale arcoriginally split on the No. 10 sieve, and multiplying the result computed using a specific gravity of 2.65. Correctionbv 100, To obtain the mass passing the No. 10 sieve, subtract factor5 arc n in Tab(e ^the mass retained on the No. 10 sieve from the original mass. f . percentage ofso,| remaining m suspension at the level

12.2 To secure the total mass of soil passing the No. 4 al wnich the hydroincter measures the dens.tv of thei475-mm) sieve, add to the mass of the material passing the suspensionNo 10 sieve the mass of the fraction passing the No. 4 sieve R , hydrornete; reading cornposite correction ap-and retained on the No. 10 sieve. To secure the total mass of p|ied (Section 7)soil passing the '/.-in. (9.5-mm) sieve, add to the total mass of w m oven.dry mass of soil in a total test sample reprc-soil passing the No. 4 sieve, the mass of the fraction passing xfMd b mass of xA disperxd (xe u 2) gthe 'v.n. sieve and retained on the No. 4 sieve For the G . speciflc ^ of the „« parucles. andremaining sieves, continue the calculations in the same G/ . specificgravuy of the liquid in which soil panicles aremanner- . „ , suspended. Use numerical value of one in both

12.3 To determine the total percentage passing for each instances in the equation. In the first instance anysieve, divide the total mass passing (see 12.2) by the total pos&Me variation produces no significant effect, andmass of sample and multiply the result by 100. in lhe on,! instance, the composite correction for R

is based on a value of one for G,.b. hjr»t3itt}pkt Moistwt Correction Factor 15, Diameter of Soil Particles

13.1 The hydroscopic moisture correction facto? is the I5.| The diameter of a particle corresponding to theratio between the mass of the oven-dried sample and the percentage indicated by a given hydrometer reading shall beair-dry mass before drying. It is a number less than one. calculated according to Stokes' law (Note 14), on the basisexcept when there is no hygroscopic moisture. that a particle of this diameter was at the surface of the

suspension at the beginning of sedimentation and had settled14. Percentages of Soil in Suspension to the level at which the hydrometer is measuring the density

14.1 Calculate the oven-dry mass of soil used in the of the suspension. According to Stokes' law:hydrometer analysis by multiplying the air-dry mast by the D - </[30n/980(G - (7,)] x L/Thygroscopic moisture correction factor.

A-40AR3002ii7

Attachment 1®> D 422 Page 6 of 7

TABLE 2 Values of Effective Depth Based on Hydrometer anddiameter of particle, mm. Sedimentation Cylinder oi Specified Sues-1coefficient of viscosity of the suspending medium (inthis case water) in poises (vanes w-nh changes in Actual e*ecwe »C;uai E-'ecuve Acâitemperature of the suspending medium). Hygrometer Oemndistance from the surface of the suspension to the "eaong _ _-J_™_ _ _ gapinglevel at which the density of the suspension is being ; °°° :63 3 '53measured, cm 'For a ejven h>drometer and sedimen- ] '.*° '. '**tation cvlmder. values var. according to the hvdrom- 1303 -53 5 -saeter readings This distance is known as effective ' X* -52 4 -55depth (Table 2i). ' oc5 '-° 3 '-5

f = interval of time from beginning of sedimentation to t yx -47 5 .= 3 -6 . -4the taking of the reading, mm. ; oor 144 ' -52 1- •::

<7 = specific gravity of soil particles, and ' xs |42 3 '-: ~-3 ',:.o"; = specific gravity (relative density) of suspending me- ! g^ j" ,90 ,*? " [!

dium (value may be used as 1.000 for all practicalpurpOSCS). '3" '34 11 -45 *: 35

' 012 131 '2 '43 43 94S'OTE !•* — Since Slok.es' law considers the terminal velocitv of a ' °13 ]29 '3 '4 2 Jo =:

single sphere falling in an infinity of liquid, the sizes calculated represent ' °'* 126 u :4° 14 3'the diameter of spheres that would faJI at the same rate as the soil 123 '5 '38 J5 39panicles. , OI6 ,2 , ,6 ,37 16 a,

, , , ._ , , , 1 017 118 17 135 47 3515.2 For convenience in calculations the above equation \ oia us is 133 48 34may be written as follows: 1019 113 19 132 49 33

_ .. r-=. ' 020 110 20 130 50 3'U m \f L/ J

where- ' °2' 107 21 129 =' "9.• A *• u r u 1022 105 22 127 52 '3A. = constant depending on the temperature of the suspen- 1023 102 23 125 53 -5

sion and the specific gravity of the soil panicles. Values ' oz« 100 24 124 54 -4of A' for a range of temperatures and specific gravities ' °25 97 25 122 55 r3are given in Table 3. The value of A.' docs not change for , 026 94 26 ,20 56a senes of readings constituting a test, while values of I 1027 92 27 119 37 -:andTdovary. I02B 89 28 "7 58 53.3 Values of b may be computed with sufficient accu- ]$£ H ™ ]}*t {:

Tacy. using an ordinary 10-tn. slide rule.1031 81

NOTE 1 5 — The value of L is divided by T using the A • and 5-scaJes. i 032 7 ethe square root being indicated on the D -scale. Without axeruining the ' 033 7 6value of the square root it mav be multiplied by K. using either the C- or ' 034 73;sn n

1 037 6.S

16. Sieve Analysis Values for Portion Finer than No. 10 10M 62(2.00-mm) Sieve * VakJM °* •tl*«lv» Motn art c*cu<aito from mt equation

16.1 Calculation of percentages passing the various sieves t • t, * "»it, - tv»<)iused in sieving the portion of the sample from the hydrom- *** ; êter test involves several steps. The first step is to calculate ti I MlMVt ong'in stem of me hydrometer from the too of the ou» to •*the mass of the fraction that would have been retained on the ma* tor * nyaromnw rt»*ng, em.No. 10 sieve had it not been removed. This mass is equal to *•» " over* length & me nyaremeter ou«. cm.the total percentage retained on the No. 10 sieve (100 minus £ 12S «?St£S e nd*. «m»total percentage passing) times the mass of the total sample vuuet u*eo m cttcuunng me viiuei n Taue 2 are as tatowsrepresented by the mass of soil used (as calculated in 14.2). F» eo« hydrometers. ISIM ana is2M:and the result divided by 100. £» ; 112!J!1,

16.2 Calculate next the total mass passing the No. .?00 /I2T.8cm»sieve. Add together the fractional masses retained on all the For hydrometer isiH. ' *sieves, including the No. 10 sieve, and subtract this sum from *•• " 10-5 ""(or • f * <"'«»the mass of the total sample (as calculated in 14.2). r rSJeMsaT11"9

16.3 Calculate next the total masses passing each of the L, - io.s cm xx a re»*ig <x o g/»mother sieves, in a manner similar to that given in 12.2. • 2.3 em (or a reeang « so g/»ire

16.4 Calculate last the total percentages passing by di-viding the total mass passing (as calculated in 16.3) by the 17. Graphtotal mass of sample (as calculated in 14.2), and multiply the ,7 , \vTien the hydrometer analysis is performed, a graphresult by 100.

A-41

Attachment 1D 422 Page 7 of 7

________ TABIJE 3 V«lu«> of K tor Ui» In Equation tor Computing Ol«',i«t«r olPirteltin Hydromet«r Antlyti*T«mo«fHuf», Soeaftc Grtviry ol So! P«rtcws __

*C 2«S 250 255 260 265 2~70 275 '. ~~ fio 285'6 001S10 001S05 001*81 301*57 001*35 001*1* 001394 00137* CO'15617 0015U 001*88 001*62 001*39 OOU17 001396 001376 001356 001338'8 001*92 001*67 001*43 001*21 001399 001378 001359 001339 00-321!9 001*7* 001**9 001*25 001*03 001382 001361 0013*2 0'323 30-30520 001*58 001*31 001*08 001386 001365 0013*4 001325 001307 30-.289

21 001*38 23««14 001391 001369 0013*8 001328 0013W 2 1291 12*322 30I«J1 201397 001374 001353 001332 001312 00129* 2 ^S 125823 001*0* 201381 001358 001337 001317 001297 001279 : 1251 1J«2* 001388 001365 0013*2 001321 001301 001282 00126* 3 1246 122925 001372 001349 001327 001306 001286 .001267 001249 0

28 001357 001334 001312 001291 001272 001253 001235 027 001342 001319 001297 001277 001258 001239 001221 028 001327 001304 001283 001264 0012** 001255 001208 00119129 001312 001290 001269 0012*9 001230 001212 001195 00117830 001298 001278 001258 001236 001217 001199 001182 001165

'25!1246',232

'2'81204

:2'

12038••562•49

of the test results shall be made, plotting the diameters of the almost entirely of panicles passing the No. 4 i4-5.mrr.iparticles on a logarithmic scale as the abscissa and the sieve, the results read from the graph may be reported aspercentages smaller than the corresponding diameters to an follows:arithmetic scale as the ordmate. When the hydrometer ,,, Gnvel, wssioj j-m »nd reumcd on NO * «evtanalysis is not made on a portion of the soil, the preparation o s*od. ousms NO 4 «eve »nd retained on NO :ooof the graph is optional, since values may be secured directly (a> c°*"« »»d- p""" s° * «v« «<J reamed onfrom tabulated data. .b , Mrt!ura"and. pusmi NO 10 ™«< ,Bd retained 30

NO. *0 sieveReport 1C) Fine sind. piumi No 40 sieve and retained on No

18.1 The report shall include the following: m Su. '.ao'* to o.oos mm *18.1,1 Maximum size of panicles. m a*v «e. imuier uun o oos mm %18.1.2 Percentage passing (or retained on) each sieve. CoUoidi. jmaiier uun 0.001 mm i

which may be tabulated or presented by plotting on a graph [§,4 For matenals for which compliance with definite(Note 16). specifications is not indicated and when the sod contains

18.1.3 Description of sand and gravel panicles: material retained on the No. 4 sieve sufficient to require a18,1.3.1 Shape— rounded or angular. sieve analysis on that portion, the results may be reported as18,1.3.2 Hardness— hard and durable, soft, or weathered follows (Note 17):

and friable,_ ._ ; .r M L " , ,181.4 Specific gravity, if unusually high or low,

18.1.5 Any difficulty in dispersing the fraction passing the s.eveSueNo. 10 (2.00-mm) sieve, indicating any change in type and 3 (oamount of dispersing agent, and 2*in.

18.1.6 The dispersion device used and the length of thedispersion penod. '-'B-

"••ID.NOTE 16 — This tabulation of fnph represent! the gradation of the *•<"•

sample tested. If panicles Urfer thin those contained in the umpte *tre NO. * «,75-mm>removed before tesuni. the repon shall so tute pvint the atoount and J]0i "J !?,, m°lmax.mumsue.

18.2 For materiiJs tested for compliance with definite HYDROMETER ANALYSISspecifications, the fractions called for in such specifications o.o?« mmshall be reported. The fractions smaller than the No. 10 sieve ° °°* «™shall be read from the graph.

18.3 For matericis for which w .Jiance with, definite NOTE n— No. 8 (2.36-mm) and No. 50 (30r>um) sieves may bespecifications is not indicated and wnen the soil is composed substituted for No. 10 and No. 40 sieves.

**? SocMry fer r««*>g •* MMwM (MM no oenacn impfeUng «• vtH4*Y of try P*** "V"* *•"*•**< eenmeoonmtnttonto m thU wuroita, Una ot tf»i iranMfd m t*pmtiy tav»»a ffur Otltmnttan ol tl» v*H*y el my tucfi

ptttnt no*». «w «• m* ol wangumn el men iigm, mi tnamt imtr own

T7* «»KMn* k fu vt » r*i*on mYour eam*n* ** nem* ctnM

nvMfw. wtiteh yeu mr «w»t » yen ** «* n* eomnmnt imn net fiewwd • «r /IMWIB jw «ftou« m*t« your1 919 *e« ST.. MMMWiaM, M I9T03.

A-42

Designation: D 421 - 85 Attachment 2Page 1. of 2

Standard Practice forDry Preparation of Soil Samples for Particle-Size Analysis andDetermination of Soil Constants1

5. Sampling; This practice covers the dry preparation of soil samples - ' Expose the soil sample as received from :r.e r'.e.vi :c :-.•.:

s -c;cived from the field for particle-size analysis and the Jirat ro°m temperature until dned ihorouEr.ly B.-eai«. ,~ •-?i^crmmation of the soil constants. aggregations thoroughly in the mortar witn a rubccr- -.--.;:-'"' - r-'j/v standard may involve hazardous materials, oper- pestle. Select a representative sample of the amount r:c_::'.,"v and equipment This standard does not purport to to P«rform 'he desired tests by the method of quar.e-r.g ;-•ri-n .i/i'" lim Sa1ei\'problems associated with us use It is b> l.he use of 3 samPl«r- The amounts of matenai rc .::j -

,':; v /m n- ot h er w« r/»« standard to nonsuit and *x?°™ m/d,l*ld.ual tests arf_3S follo*s^ •n/i\n appropriate aaietv and health practices and deter- " ' , ••Ji.e.-inunsis ror tnc par.ic.c-s;zc.ir.j,;.=,$.*' / L. / I/ matenal passing a No. 10 (2.00-mmi sieve is -•'•cui-•'''' ••

"•'" ' ' amounts equal to 115 g of sandy soils and 6; g jf e:tner 5ut, _. or clav soils.

Referenced Documents « ,;, r«tf ./or 5<7//O«5 M-For :ne tests for soilcor.-: i iST\f Standards stants. matenal passing the No. 40 UZJ-ami sieve .s requiredD .21' Practice for Wet Preparation of Soil Samples for in total amount of 220 g, allocated as follows:Panicle-Size Analysis and Determination of Soil r«i ,;-n™Constants" Liquid limit .•

Specification for Wjre-Clotn Sieves for Testing Pianiciirmt• 3 Ceninfufe moisture sauivaJentPurposes Volumetnc shnnkaje :.)

Check lesu ,5i Significance and Use

, . , . 6. Preparation of Test Sample« i This practice can be used to prepare samples for par--,ie-5ize and plasticity tests where it is desired to determine 6-' S*1*" tnat P°nion of tne a«r-dned sample selected for•csi values on air-dned samples, or where it is known that 31r P" 56 of ««s and record the mass as the mass of the MtaljnmB does not have an effect on test results relative to "l *mpie «n«"e«ed for hygroscopic motsture. Separate '

f . ^ . a r*t-»iT the test sample by sieving with a No. 10 (2,00-mmi sieve.<jmples prepared in accordance with Practice D 2217. Grind that fraction reta ned o rhe N 10

with a rubber-covered pestle until the aggregations of soil4. Apparatus panicles are broken up into the separate grains. Then separateJ I Balance, sensitive to 0.1 g. the ground soil into two fractions by sieving with a No. 10J : \fortar and Rubber-Covered Pestle, suitable for break- sieve.

ing up the aggregations of soil particles. 6.2 Wash that fraction retained after the second sieving4 3 Sieves—A senes of sieves, of square mesh woven wire free of all fine matenal. dry. and weigh. Record this mass as

Joth. conforming to Specification E 11. The sieves required »ne mass of coarse matenal. Sieve the coarse matenal. afterjrc as follows: ing washed and dried, on the No. 4 (4.75-mm) sieve and

record the mass retained on 5ft* Np. (4 sieve.No. 4(4.75-mm>so {J IHJ" 7. Test Sample for Particle-Size Analysis

7.1 Thoroughly mix together the fractions passing the No.4.4 Sampler—* riffle sampler or sample splitter, forquart- ,0 (2.00-mm) sieve in both sieving operations, and by the

cnng the samples. method of quartering or the use of a sampler, select a portion_____ weighing approximately 115 g for sandy soils and approxi-————— mately 65 g for silt and clay soil for particle-size analysis.' Thu practice is under the jurisdiction of ASTM Committee D-18 on Soil and«. k ind ii the direct responsibility of Subcommittee D11.03 on Texture. Ptasucity. _ —. Samote fflf Soil Constants

j« edition approved July 26.1913. Published September iw. Onunaiiy g j Separate the remaining portion of the matenal passing........... ~WI.JI(I97W_ the No. 10 (2.00-mm) sieve into two parts by means of a No.

i ufll 40 (425-um) sieve. Discard the fraction retained on the No.

A-43 SR30Q250

Attachment 2D421 P**e 2 of 2

40 sieve. Use the fraction passing the No. 40 sieve for the determination of the sou constants

Thi Amtricin Sociny lor fisting trie Uttima :wts ?o oosrf.w 'tsotaifg ;ft itu&ft ~t wy saie"i • yrts asierw r> zor-tc*i\t\ tny i(tm mtfinonte m IM sitmltra 'Jstrs 3' '"'S ftanaira if* tiomsiy lawsta !"tt leser-iration it ••» .a c ••< :' i-< ;Olltnf "guts, tna tnt ntt ot \nlnngwnvn ot iucr> •••g/'ts. in tnnrtiy :"•" a*" 'S

''"is itanotfd il sufiiKf fo nnjion Jf J y '""• Oy •'"• 'OSOO SiO't IKfineti cormritt tra "lull £>• -tyitwta tvtr/ '.»* «|f j jro' tor riwsta ta*»r 'tioorovtO or vmnariwn YOU' coi""«ntj J't 'rvita tnn»r lor rtvmon ot ms atratrg or 'or lea f'O"«i Hii-carzsv-a snouia >• taa'*ssta 10 4SrM Htiaauirrtrs four commtnti *•» 'eetiv* artful co"j.o«'jfior II 4 r ttt.rg :/ ,—* -«SDO'%s c-e'«<:•""«' rs— «"»»t »"ic" /oo <~«y *(Te"fl .' /oo *e«/ .'«ai ooc :on-memj -a»t »of -Kt'vea a 'tir -t*""j ,vt* r'ct,"? -^«e ,:o'

'3'5 »ac» Si

A-44

PROCEDURESIN SEDIMENTARYPETROLOGY

Edited by.x-

ROBERT E. CARVER

University of GeorgiaAthens, Georgia

WILEY-INTERSCIENCE

A Division of John Wilcy & Sons, Inc.New York • London • Sydney • Toronto


A-45

AR-3-&0252


CHAPTER 3

SIEVE ANALYSIS

ROY L. INGRAM

University of North Carolina, Chapel Hill, North Carolina

The distribution of sizes of sedimentary particles with intermediatediameters in the range of 1/16 to 16 mm (sand and fine gravel) ismost commonly determined by sieving. In the United States, theUnited States Standard sieves or the Tyler Standard sieves (Table 1)are used by most workers.

TABLE 1 Sieve openings

WentworthScale,mm

16

8

Phi Scale

-4.00-3.75-3.50-3.25-3.00-2.75-2.50-2.25

V2~Scale.mm

16.00013.45411.3149.5148.0006.7275X5'4.75V

U. S. Standard "

Opening,mm

16.013.511.29.518.006.73•» ss4.76

Mesh

3K4

Perm UsableVariation

Average± %

33333333

Maxi.+ %

6666661010

1

Tyler6Mesh

2Yi33W449

A-46 3R300253


TABLE 1 Sieve openings (Continued)

a A.S.T.M., 1966, pp. 447-448.b W. S. Tyler Co.. 1967, p. 10.

50

A-47

WentworthScale,mm

j «

2

1

1/2

1/4

1/8

1/16

1/32

Phi ScaJe

-2.00-1.75-1.50-1.25-1.00-0.75-0.50-0.250.000.250.500.751.001.251.501.752.002.252.502.753.003.253.503.754.004.254.504.755.00

4Y/2~ Scale,mm

4.0003.3642.8282.3782.0001.6821.4141.1891.0000.8410.7070.5950.5000.4200.3540.2970.2500.2100.1770.1490.1250.1050.0880.0740.0620.0530.0440.0370.031

U.S. Standard"

Opening,mm4.003.362.83

Mesh

PermissableVariation

Average±%

Maxa.+ %

i

Tyler bMesh

5 3 j 10 56| 3 10 67! 3 10 7

2.38 8j

2.00! 101.681.411.191.00

12141618

0.841 200.7070.5950.5000.4200.3540.2970.2500.2100.1770.1490.1250.1050.0880.0740.0630.0530.0440.037

253035404550607080100120140170200230270325400

3 10 8 :1

3 103 103 1033555

5555556666677777

10

910 ;1214

15 I 1615 20 ;151515252525252540404040406060606060

24 :28

32354248606580100115150 :170200250270325400


TESTING SIEVES 65

ACCURACY OF SIEVES

Three different types of sieves may be purchased. Most commcr-ci.illv available sieves arc manufactured to meet the tolerancesestablished under ASTM Specifications Ell-Gl. (Sec Table 1.) TheNational Bureau of Standards will, for a fee, check a set of sieves andwill certify them if they meet ASTM specifications. The manufac-turer selects matched sieves to sivc results for a given sample that arccomparable to those obtained from the manufacturer's Master Sieves.Matched sieves arc the most accurate available.

TESTING SIEVES

Sieves may be checked for accuracy in several different ways(ASTM, 1966. and W. S. Tylcr Co., 196?', p. 39).

Use of Standard SamplesThe use of calibrated glass spheres is recommended for checking

and determining the effective sieve openings. Calibrated glass spheresmay be obtained from the Supply Division, National Bureau ofStandards, Washington, D. C. Three standard samples arc nowavailable at $9.50 each: No. 1017, 0.050 to 0.230 mm; No. 1018,0.210 to 0.980 mm; and No. 1019, 0.90 to 2.55 mm. Instructionsarc provided for using the glass spheres in calibrating sieves.For routine checking of sieves each laboratory should maintain its

own standard sample. A set of sieves should be checked periodicallywith a standard size split of the standard sample to sec if the setcontinues to give the same results. A new set of sieves can also bechecked against the standard to see if the sets give comparableresults. If they do not, calibration factors can be calculated for eachsieve that will make the results comparable.

Measurement of OpeningsSeveral methods of measuring openings arc given in ASTM

Specification £11-61. One method is to use a microscope and measurethe openings. Six nonoverlapping fHd? ••£ view are selected. In each

A-48

1Attachment 3Page 5 of 5

66 SIEVE ANALYSIS

field measure at least 50 openings perpendicular to the wires, withthe openings being located in a diagonal direction across the field(Fig. 8). The openings in three of the fields should be measured atright angles to those in the other three fields. Tabulate the resultsand check against Table 1.

REFERENCES

American Society for Testing Materials, 1963, Grain s.zc analysis ofsoils, D422-63, pp. 203-214, in 1967 Book of ASTM Stand-ards, Pt. 11, Philadelphia.

———, 1966, Sieves for testing purposes, Ell-61, pp. 446—452, in1966 Book of ASTM Standards, Pt. 30, Philadelphia.

Folk, R. L., 1968, Petrology of sedimentary rocks, Hemphills,Austin, Texas, 170pp.

Jackson, M. L., L. D. Whitting, and R. P. Pcnnington, 949,

Fig. 8 Testing sieves by microscopic measurement of openings located alongdiagonals of openings.

A-49.6R300256

RESIDUE, TOTAL

Method 160.3 (Gravimetric, Dried at 103-105°O

STORET NO. 00500

1 . Scope and Application1 . 1 This method is applicable to drinking, surface, and saline waters, domestic and industrial

wastes.1 .2 The practical range of the determination is from 10 mg/1 10 20,000 mg/1 .

2. Summary cf Method2.1 A well mixed aliquot of the sample is quantitatively transferred to a pre-weighed

evaporating dish and evaporated to dryness at 1 03- 1 05'C3. Definitions

3,1 Total Residue is defined as the sum of the homogenous suspended and dissolvedmaterials in a sample.

4. Sample Handling and Preservation4. 1 Preservation of the sample is not practical; analysis should begin as soon as possible.

Refrigeration or icing to 4*C, to minimize microbiological decomposition of solids, isrecommended.

5. Interferences5. 1 Non-representative particulates such as leaves, sticks, fish and lumps of fecal matter

should be excluded from the sample if it is determined that their inclusion is not desiredin the final result.

5.2 Floating oil and grease, if present, should be included in the sample and dispersed by ablender device before aliquoting.

6. Apparatus6. 1 Evaporating dishes, porcelain, 90 mm. 100 ml capacity. (Vycor or platinum dishes may

be substituted and smaller size dishes may be used if required.)7. Procedure

7.1 Heat the clean evaporating dish to 103-105'C for one hour, if Volatile Residue is to bemeasured, heat at 550 ± 50*C for one hour in a muffle furnace. Cool, desiccate, weigh andstore in desiccator until ready for use.

7.2 Transfer a measured aliquot of sample to the pre-weighed dish and evaporate to drynesson a steam bath or in a drying oven.7.2.1 Choose an aliquot of sample sufficient to contain a residue of at least 25 mg. To

obtain a weighablc residue, successive Iky. -AS, of sample may be added to the samedish.

7.2.2 If evaporation is performed in a drying oven, the temperature should be lowered toapproximately 98*C to prevent boiling and splattering of the sample.


A-50HR300257

7.3 Dry :he evaporated sample for at least I hour at 103-105'C. Cool in a desiccator andweigh. Repeat the cycle of drying at 103-105*C, cooling, desiccating and weighing until aconstant weight is obtained or until loss of weight is less than 4% of the previous weight,or 0.5 mg, whichever is less.

•8. Calculation8. 1 (Calculate total residue as follows:

Tota: residue, mg/1 = <A "

whers:

A = weight of sample + dish in mgB = weight of dish in mgC — volume of sample in ml

9. Precision and Accuracy9.1 Precision and accuracy data are not available at this time.

Bibliography

1. Standard Methods for the Examination of Water and Wastewater, 14th Edition, p 91, Method208A,(1975).

A-51

Designation: D 22 1 6 - 80

Standard Method forLaboratory Determination of Water (Moisture) Content of Soil,Rock, and Soil- Aggregate Mixtures1

. . | This standard is issued under the fixed designation D 2216: the number immediately following the designation indicates the >ear ofI [ j I original adoption or. in the case of revuicn. the year of last revision. A number in parentheses indicates the year of last reapprovai. *I; : superscnpt epsilon id indicates an editorial change since the last revision or reapprovai.

1. Scop* hydrated water at in-situ temperatures or less than 1 IO"C can1.1 This method covers the laboratory determination of b* misleading.

the water (moisture) content of soil, rock, and soil-aggregate 3-5 f * term "s°lid panicles" as used in geotechnicii mixtures by weight. For simplicity, the word "material" engineering, is typically assumed to mean naturally occur-

hereinafter refers to either soil, rock, or soil-aggregate mix- rin8 mineral particles that are not readily soluble in water' tures, whichever is most applicable. Therefore, the water content of materials containing extra-

1.2 The water content of a material is defined as the ratio, neous ma«« (such as cement, etc), water-soluble matte:expressed as a percentage, of the mass of "pore" or "free" <sucn & ***$ and highly organic matter typically require

' j water in a given mass of material to the mass of the solid special treatment or a qualified definition of water content.material panicles.

1.3 This method does not give true representative results 4> APP*™*"*for materials containing significant amounts of halloysite, 4.1 Drying Oven, thermostatically-controlled, preferab:;.mommorillonite, or gypsum minerals; nightly organic soils; of the forced-draft type, and maintaining a uniform temperor. materials in which the pore water contains dissolved ature of 1 10 ± 5*C throughout the drying chamber.solids (such as salt in the case of marine deposits). For a 4.2 Balances, having a precision (repeatability) of ±0.01 <material of the previously mentioned types, a modified for specimens having a mass of 200 g or less. ±0.1 g tomethod of testing or data calculation may be established to specimens having a mass of between 200 and 1000 g, or =give results consistent with the purpose of the test g for specimens having a mass greater than 1000 g.

4.3 Specimen Containers — Suitable containers ma ^! 2 Summary of Method material resistant to corrosion and a change in mass V

The mass of material remaining after oven-drying is used as ermina o .the mass of the solid particles. NOTE 1— The purpose of close-fining lids is to prevent loss c

moisture from specimens before initial weighing and to prevent absorp_ _. ._ , , . tion of moisture from the atmosphere following drying and before tm-3. Significance ind U« . wei«htn«.

3.1 For many soil types, the water content is one of the 4 4 Desiccaior .k desiccator of suitable size (a convenmost significant index properties used m establishing a iem ^ 200 to 250-mm diameter) containing a hydrouco™a£?n bt'tween w" behavior and an index property. ^ - -j equipment jj on]y recommended for use whei3.2 The water content of a sod is used in almost every containers having close-fitting lids are not used. See 7.4. 1.

equation expressing the phase relationships of air, water, andsolids in a given volume of material 5 Samples3.3 In fine-fnined (cohesive) soils, the consistency of a ' .. „ . ,. _j .„,

given soil typ? depends on its wateV cositent The water 5-1 Ke?P *« P1* ** m «wred pnorfto «£"*!content of a soil, along with its liquid awl plastic limit, is nonoeaidifak *mght containers at a temperature betweeuted to express* relitive onSSc7oS,S taST approximately 3 and 30'C and in an area that prevents du«

practicable after sampling, especially if potenuallc.rrodibl en (such as l thin-walled tubes, p*cans, etc.) or sample bags are used.

•Tbiinttfaod)«uadffthejuTi»tiax»rfAS™ 6. Test SpedmCBi Rock tod a tic dinet rwpoombtoy of Subccwunra* oiW3 an Tenure, g j por water contents being determined in1 "tSTtdrSSpp T 5 . PubinM Jdy im. On o with another ASTM method, the method of

;' pubtuh«dMOUi«-«3T.LMtpicviM»«iiiioaDtti6.7i. selection specified in that method controls.

A-52 AR300259

W D2216

52 The manner in which the test specimen is selected and indicate an insignificant change (less than about O.l "jj. Specimens ofquired mass is basically dependent on the purpose and may often be dried to constant mass m a penod of aixaut 4 h. *nen

plication) of the test, type of material being tested, and the a forced-* °ven « used.> Of sample (specimen from another test, bag, tube, -V°TE 5—Oven-drying at HO » 5'C does not always result in waterJ-barrel. etc.). In all cases, however, a representative fSivfoTJSS?. !°J«e mlended "* °r uhe bai'c defimuon£„„ of the total sample shall be selected. If aLered soil S2t ^ ^

or more than one soil type is encountered, select an average amount of organic material. In many cases, and depending on theOr individual portions or both, and note which intended use for these types of materials, it might be more applicable to) was tested in the report of the results. maintain the drying oven at 60 ± 5'C or use a vacuum desiccator at aFor bulk samples, select the test Specimen from the vacuum of approximately 133 Pa no mm Hg) and at a temperature

,a«"nal after it has been thoroughly mixed. The mass of raTS *"**?. 23 ;!ndM62lC f" **!* If eithe.r°f these dr^ns,T,aten<u u n u \T "'*»"' methods are used, it should be noted in the report or the results.meMSt material selected shall be in accordance with the NOTE 6-Since some dry materials may absorb moisture from mo.stfollowing table: specimens, dned specimens should be removed before placing moist

Sieve Retaining More Than Recommended Minimum Mass specimens in the oven. However, this requirement is not appiicaoie ifAUout I0"i5 of Sample of Moist Specimen g tne previously dned specimens will remain in the drying oven for an:.0 mm ,No. 10) s.eve ,00 to 200 'ddlUOMi Ume *n°* °f 4b°Ut '6 h'4 "5 mm (No. 4) sieve 300 10 500 7.4 After the material has dried to constant mass removej| ™ ,-°° |° ]°~ the container from the oven and replace the lid. Allow the-(, mm 50oo io 10 ooo material and container to cool to room temperature or until

material HIi accordance with the table in 6.2 1. See Note 2. 7 4 , Jf he ^6.2.2.2 Forcohesivesoils.removeabout3mmofmatenaJ containerand material right after their temperatures;

rrom the exposed periphery of the sample and slice it in half thaj the operation of the bajance wm not affelto check ,f the matenal is layered) pnor to selecting the test conveciion cunents or after cooli in a desiccator.specimen. If the soil is layered see 6.2. The mass of moistmatenal selected should not be less than 25 g or should be in NoTE 7-C°oling '" a desiccator is recommended since it preventsaccordance with the table in 6.2.1 if coarse-grained particles absorP''°n °f «°«"»« fr°™ *e atmosphere dunng cooling.

I "jaged. (Note 2). 8. Calculationhg BLsing a test specimen smaller than the minimum < > , , - , , , _ r u , <• ,,I •fcdicated previously requires discretion, though it may *•' Calculate water content of the malenaj « follows:be adequate for the purpose of the test A specimen having a u, - r/w w\itw w\t v inn , W'w v im

, i , . . , . • ., i n • « " 1\ ™! *)/\ 2 V* f)\ " i W «»» | vwmass less than the previously indicated value shall be noted * »;m the report of the results. where:NOTE 2—In many cases, when working with a small sample con- w •> water content, %,

tuning a relatively large coarse-grained particle, it is appropriate not to fVt « mass of container and moist specimen, g,include this particle in the test specimen. If this occurs, it should be W2 m mass of container and oven-dried specimen, g,noted m the report of the results. ( ^ m mass of container, g,7 Procedu,. * " mass of water, g, and

Wt » mass of sou'd particles, g.'•i Select representative test specimens in accordance a _

*ith Section 6. 9" Repolt7-2 Place the moist specimen in a clean, dry container of 9.1 The report (data sheet) shall include the following:

known mass (Note 3), set the lid securely in position, and 9.1.1 Identification of the sample (material) being tested,determine the mass of the container and moist material by boring number, sample number, test number, etc.wng an appropriate balance (4.2). Record these values. 9.1.2 Water content of the specimen to the nearest 0.1 %I 7 3 Remove the lid and place the container with moist or 1 %, depending on the purpose of the testcatena! in a drying oven maintained at 110 ± 5*C and dry 9.1.3 Indication of test specimen having a mass less thanP 3 constant mass (Notes 4, 5, and 6). the minimum indicated in Section 6.v-^ , , . . . . ,, . . 9.1.4 Indication of test specimen containing more thanNOTE 3—To assist in the oven-drying of large test specimens, they ' * .. M(M /i,«-_j -„«

fey* be placed in containers having a large surface area (such as pans) one soil type (layered, etc).P« »e material broken up into smaller aggregations. 9.1.5 Indication of the method of drying if different from_NOTE 4-The time required to obtain constant mass will vary oven-drying at 110 ± S'C.

nd''ng on the type of material, size of specimen, oven type and 9.1.6 Indication of any material (size and amount) ex-ntVi and other factors. The influence of these factors generally can eluded from the test specimen.Rablished by good judgment and experience with the materials

r* "sled and the apparatus being used. In most cases, drying a test JQ Precision and Accuracy""fcOver night (about 16 h) is sufficient. In cases where there is ! / , , « • e L. •• j *, „<•»*.;*

Hsrningthe adequacy of drying, drying should be continued 10.1 Requirements for the precision and accuracy of thist after two successive periods (greater than 'A h) of drying test method have not yet been developed.

A-53 . flR300260

D2216

'fit American Society tor Testing ana Mtte'iais taxes no acsition resettling ;ne validity of any oaten rgnts asserted m ccnnecnorwit!) my itim msntionta in trtis stanaira Users st tfiis stanaara are expressly aavisea mar aetermmation of tnt validity of any sucnotiem rignts, ana ine nsK ot inlrmgemtnt o< sucn r/gnts. are entirely tne<r own resoonsioiMy

This stanaara is subnet to revision at any time oy tne resoonsiDie tecnncal comminee ano must Ot reviewed every live years andil not revuea, eithtr rttoofovea or witnarawn Your comments are invitee eitner tor revision of tnis stanaara or lor aaaitionai stanoarosana snouia oe aaartssea to ASTM Heaaauanen. four comments will receive careful consideration at a meeting ol tne responsibletecnmca' committee, wnicn you may attend H you ie«i tnat your comments nave not received a lair Hearing you snouia mate your«ws Known to tne ASTM Commute* on Slanoaros, '9'6fljeeS(., Pnnaaeionia PA rOTm

flR30026l

ri

i). S. Environmental Protection Agency SAS NumberHWI Sample Management OfficeP. 0. Box 818 Alexandria, VA 22313PHONE (703) 557-2490 or FTS 557-2490






0. Date of Request:





Analysis of 10 low concentration aqueous samples for full TCL orgam'cs usingEPA Drinking Water Methods detection limits.

A-55

AR3Q0262


5 low concentration aqueous (residential well) samples;1 field duplicate;1 matrix spike (MS) and matrix spike duplicate (MSD) pair;1 field blank;1 equipment rinseate blank; and1 trip blank

3. Program (specify whether Superfund (Remedial or Enforcement), RCRA, NPDES,etc.)i and justification for analysis and Site Account Number:

SUPERFUND Remedial

SAS Approved by:


NOVEMBER 1 through NOVEMBER 15. 1990





7. Analytical protocol required (attached copy if other than a protocolcurrently used in this program): •-.,.. _ _.......„___.,_ .„....„_,.„, _....„„.___„ 'BNA's - EPA Method 625

A-" flR300263


If multiple phase sample, notify ERA Region III and SMO.




The case narrative must document all problems encountered and subsequent• resolutions. List instrumentation and methods employed for analysis. Also,

note whether samples were preserved and, if so, the procedure used inpreservation.




Parameter Detection Limit f+ or - Concentration)

VOA's As per Method 524.2 As per Method 524.2BNA's As per Method 635 As per Method 625Pesticides/PCB's As per Method 508 As per Method 508



VOA's As per Method 524.2 As per Method 524.2BNA's As per Method 635 As per Method 625Pesticides/PCB's As per Method 508 As per Method 508



15. Request prepared by: Christopher Bums


Date:


A"58 flR300265

TCN 4204-01-QAPjPSECTION RREVISION NO. 0PAGE NA OF NA04/SEPT/90

APPENDIX B

PARAMETER DETECTION LIMITS

flR300266

Acetonnrt'e 7S-05-6 iCOAcrolem 107-02-8 130Acrylomtn'e 107-13-1

13071-43-2 5

wunuuicniorametnane 75-27-4 5Sromomecnane 74-83-9 10Caroon recracnlonoe 56-23-5 5

3 Cdroon atsu if me 75-15-0 5i Ch!oroo«n«nt 108-90-7 S

i: 2-Chloro-l.3-Ouuaiene IZ6-99-8 1001. ChlorodiBramomtruiK 124-48-1 S!.' Chloroftrunt 75-00-3 1013 2-ChloroetMyl yinyl ecner 110-75-8 10[i Chloroform 67-66-3 515 Chlorometnjne 74-87-3 1015 3-Chlorooropene 107-05-1 1001' 1.2-Oibromo-3-enloroproMn« 96-12-8 10Id 1.2-Oibromoetiurui 106-93-4 S13 Dibromametn*ne 74-95-3 S20 Trin$-l.4-Oichloro-2-butene UO-57-6 1002. Oichloroaif luoranetMne 75-71-8 102: l.l-Oichloroetnjne 75-35-3 S22 l.2-0icn1oroethjne 107-06-2 52-s 1.1-Oicnloroethylene 75-35-4** f ~,e , -- — —.»,—™ /S-35-4 525 Trwi-Lz-Oiehlorotmtn. 156-60-5 5

S5

29 1.4-0,oMn. "" •———— 5

-—- "^ w.t,,iuro«tn«n« 156-60-51.2-Oichloroorowne 78-87-5

" r>-«M-l.3-OichlopooroDene 10061-02-6 523 cu-1.3-OichloP3propene 10061-01-5

30 Ethyl cy«m«3: Ethyl meth*eryUte 9J-U>1 IM32 «o*».t ;4.2.; !2f '"bucyl ,.coho) 78.34 Methyl ethyl kctone 79.93.3 1035 Methyl -netrwcryUte 80-62-6 10035 Methyl metmnejulfoiwte 64-27-3 20o3? HtthyUcrylon.tr, I. 126.98.7 ' l(JO33 Methylene chloride 75-09-233 Pyr'dlne UO-86-1 400

B-l

Parameter CAS no Target aetection iimiti-g/1)

Vc'dt' 'e< (continued)

40 '. . l.l.2-"etr«cnloraetMne 630-20-5 5«1 ;.1.2.2-Tetr»chlorcttrun« 79-34-5 s42 •etr«hloroetr«ne 127-16-4 543 -olu«ne 108-88-3 544 "rtorcmonethint . 75-25-2 545 ..l.l-Trichloroetrvm« 71-55-6 546 ..1.2-Tncnloroet(vin« 79-00-5 547 'richlorotthene 79-01-6 548 "pjchlorcmonof luoron»trunt 75-69-4 549 ..2.3-Tricnloroprooint 96-18-4 5SO Mnyl chloride 75-01-4 10

Semivo'

51 Acin«phth»l«nt 208-96-8 1052 Actiupnthtni 83-32-9 10S3 Acitophtnont 96-86-Z 1054 2-Acttyl»inofluortnt 53-96-3 1. 00055 4-Aminabiphtnyl 92-67-1 20056 AniHn* 62-S3-3 2057 Anthrictn* 120-12-7 10Sd Ar«mtt 140-57-8 10059 8tfli(*)*nthr«ene 56-55-3 1060 Bwutntthiol lflfl-98-6 1. 00061 Bttizidint 92-87-5 1. 00062 8«nroU)pyrtf» SO-32-6 1063 B««olb)fluor«nthtnt 205-99-2 10$4 Binzo(ghi)p«ry1«ni 191-24-2 1065 Btnzo(k)nuor«nti»fi« 207-08-9 1066 p-ltnzoquinww 106-S1-4 1.00067 Bts(2-ch1on»thwy)Mth«nt 111-91-1 1068 8is(2-chloro«thyU«thtr 111-44-4 1069 BiilZ-chloroiiopi-opyDtthtr 39U8-32-9 1070 B1»(2-«thylhtxyl3p«h«Utt 117-BI-7 1071 4-Brawp*wiy1 ptonyl ttlur 101-55-3 1072 Butyl benzyl phtlwUtt 85-68-7 1073 2-Stc-6utyl-4.6-dmttrophtnol 88-85-7 10074 P-ChU>ro*m1in« 106-47-8 10075 ChlorotottuiUM 510-15-6 10076 p-Chloro-m-tfrwol 59-50-7 1077 2-Chloron«phth*lin; 91-58-7 10

e-2 ^300268

CAS no. Target flttectton limitlug/1)

' 'es .continued

'8 ?-Chlor;pnenoI79 3-Chloropropioni:ri leBO Cnry$«real ortno-Cresol 95-48-7 10S2 p«ra-Cresol 106-44-5 10dj Dtotnz;i.n)«ntnr*c*nt 53-70-3 1084 OiOtnzc(«.e)pyrcnt 192-65-4 SO85 OiD«fUcu, i)pyrtnt 189-55-9 SO<J6 m-Oicn.orooenttnt 541-73*1 1087 o-0icn'oro6tn«n« 95-50-1 1066 p-Oicn orootnztn* 106-46-7 1069 3J'-0-cn!orot>truidint 91-94-1 2090 2.4-Oicnloreprwnol 120-83-2 1091 2.6-Otchloropntnol 87-65-0 1092 Oiftny pntfwlm 84-66-2 1093 3.3'-Oifflttnasy6tnndini 119-90-4 10.00094 p-Oinwtnyl4ffltno4ZoecnzirM 60-11-7 20095 3.3'-Oimttnylbtnzidini 119-93-7 10.00096 2.4-Oim«tnylpntnol 105-67-9 1097 Oimtnyt pntruUti 131-11-3 1098 Oi-n-bLtyl phtruUti 84-74-2 1099 1.4-OintroM<Uifit 100-25-4 100100 4.6-Oinitro-o-crtwl 534-52-1 SO101 2.4-Qiruropfwnol Si-28-5 SOi:: 2.4-Oirttroto)u«nt 121-14-2 10133 2.6-Oinitrotolu«n« 606-20-2 10104 Oi-n-octy) pntrulau 117-84-0 10105 Ot-n-propylnttros«iint 621-64-7 10106 OipWnylMtrw*/

dtpflenylr.ttroMfttM* 122-39-4/86-30-6 10107 1.2-OioWflylhyOruiM 122-66-7 10106 fluor«nth»r;> 206-44-0 10109 Huorcfll 86-73-7 10110 Htiucn lorootnziflt 118-74-1 10111 ntxunioroouudiini 87-68-3 10112 HMicniorocycloMntidiiflt 77-47-4 10

*ln GC/NS armiyiu. tnt»« eoieouAdi cannot M diffirtntuttd.

B-3

/IR300269

CAS no Target aetect'O" limn

iyvg it- 'es (rs

113 neMcnicroetnane 67-72-1 ;oIU nti*cnloropn»nt 7Q-30-J 20. SCOUS ntx*cnioropropene I3da-7i-; 10116 Indenoli.2.3-ca)pyrene 193-39-5 10U7 tsos*frol« 120-58-1 100116 *ttrup,rtltnt 31-30-5 200119 3-Hetriy IcnoUntnrene 56-49-5 100120 •J.J'-MetnyientOis

(2-cnlorMnihnt) 101-14-4 200121 N*pntn*1en« 91-20-3 10122 1.4-NtontnoQuinont 130-15-4 100123 l-N«ontnyUmin« 134-32-7 100124 2-N«(mthyUmtnt 91-59-8 100125 p-Nitro*ni1mt 100-01-6 50126 NitroMruent 98-95-3 10127 4-Nitropnenol 100-02-7 5012d N-Nttrosoai-n-Outyl*mme 924-16-3 100129 N-NitrosoaietnyUmin* 55-18-5 100130 N-Nitrouairatnyl«ain« 62-75-9 100131 N-NitrosomthylcthyUiiHn* 10595-95-6 100132 N-Nttrosoncrpnolint 59-69-2 200133 N-Nurosoptp«ndin« 100-75-4 200134 n-Nitrosopyrrolicint 950-55-2 200135 5-Hitro-o-tolmdmt 99-5S-8 230136 Ptnucn loroacnzirw 608-93-5 10137 Ptnucnlorattrarm 76-01-7 13138 PcnttcnioronitroticftZtnt 62-68-8 130139 Pwucnloroptwnol 87-U6-5 50140 Phtfucttin 62-44-2 100141 Phtiunthrtnt dS-01-8 10142 Phtnol lOfl-95-2 10143 2-Picolirt 109-06-8 100144 PrwiMiM 23950-58-5 100145 Pyrtflt 129-00-0 10146 Rtsoreinal 108-46*3 I.000147 Scroll 94-59-7 100148 1.2.4.S-T«r«hloPObtn«flt 95-94-3 10

B-4

flR300270

f*rget detect 10.' l i m i tug/l)

149 2.3.4.6-Tetrachloropnenol 58-90-2 100ISO 1.2.4-Tnchlc-oD«nzene 120-82-1 10151 2.4.5-Trichlc-opnenol 95-95-4 5015? 2,4.6-Trtchlc-opneno) 88-06-2 10153 rris(2.3-diBromopropy1)

Dnosphjte 126-72-7 10.000

154 Antimony 7440-36-0 60155 Arsenic 7440-38-2 10156 Barium 7440-39-3 200157 Beryllium . 7440-41-7 5ISd Cadmium 7440-43-9 5159 Chromium (tot.il) 7440-47-3 10160 Chromium (hex<ivdlent) 10161 Copper 7440-50-8 25162 LMd 7439-92-1 5163 Mercury 7439-97-6 0.2164 Nickel 7440-02-0 40165 Selenium 7782-49-2 5166 Silver 7440-22-4 101C7 TM Ilium 7440-28-0 10168 Vanadium 7440-62-2 SO169 Zinc 7440-66-6 20

Inorganics

170 Cyanide S7-12-5 10171 Fluor ide 16964-48-8 500172 Sulfide 8496-25-8 1000

Ormnochlorine

173 Alarm 309-00-2 O.OS174 tlpto-BHC 319-84-6 O.OS175 bet*-eK 319-85-7 O.OS176 dc)t4-BHC 319-86-8 O.OS

B-5

• flR30027

Parameter CAS no. Target aetecnon limn

177 QMM-BH: 53-89-9 Q 0517B ChlorMM 57-74-9 0.5179 000 72-54-8 0.01180 ODE 72-55-9 0.10181 DOT SO-29-3 0.10182 Onldrin 60-57-1 0.10163 Endosulfin I 959-96-8 0 05104 Endosulfin I! 33213-6-5 0.10185 Enann 72-20-8 0.10186 Endnn aldthydt 7421-93-4 0.1167 Htptacnlor 76-44-8 0.05188 Mepuchlor epozidt 1024-57-3 0.05189 Isodrm 465-73-6 O.I190 Ktpont 43-50-0 0.5191 Mttnoxyclor 72-43-5 0.5192 Touptanc 8001-35-2 1.0

Phenoicvjett ic Acid

193 2.4-Oicf.lorophtnoiy*cttic «cid 94-7S-7 0.5194 Stlvax 93-72-1 0.5195 2.4.5-T 93-76-5 0.5

Orqineflheaphorous Insect icioea

19« Oisulfoton 298-04-0 1.0197 F4 )hur 52-d5-7 1.019i Methyl ptrathion 298-00-0 1.0199 tarcttuon 56-38-2 1.0200 Phertti 298-02-2 1.0

201 Aroclor 1016 12674-11-2 O.S202 Aroclor 1221 11104-28-2 0.5203 Aroclor 1232 U141-16-5 0.5204 Aroclor 1242 53469-21-9 0.5205 Aroelor 1248 12672-29-6 0.5206 Aroclor 1254 11097-69-1 1.0207 Aroelor 1260 11096-82-5 1.0

flR300272

Parameter CAS no, Targe: selection limitlug/1)

O'Ox i

208 lexachlorodibenzo-D-dioxms 0,02209 iex4cnloroait>«ruofur«n o.OZ210 3entacnloroaiDenio-p-dioxins 0.02211 Jen:acnlorodic>enrofur*n 0.02212 TetracnlorooiDenzo-p-oioxins 0.02213 "etracnloroaiOeruofuran 0.0221-J 2.3.7.8-TetracnlorooiBenfo-p-aioxm 0.02

v<

B-7

flR300273

TCN 4204-01-QAPjPSECTION ____C_REVISION NO. 0PAGE _.NA OF NA04/SEPT/9Q

APPENDIX C

ENGINEERING ANALYSIS AND CALCULATION VALIDATION PROCEDURES

flR-300271*

TETRA TECH STANDARD OPERATING PROCEDURE

Engineering Analysis and Calculation Validation ProcedureAll analysis and calculations activities shall be completely documented and theresulting documentation formally checked in accordance with the proceduresdetailed below:

General

Calculations/drawings/logs/tables/etc. shall be performed on standard calculationpaper whenever possible or applicable. All calculation/drawing pages shall beindividually identified, with the exception of large computer output. Calcula-tion/drawing paper will provide spaces for the originator's name and date ofwork, the checker's name and date, calculation subject, project number, and pagenumber. All of this information shall be completed for each page. For extrapages, such as large graphs, this information shall also be included.

Calculations/drawings shall, as appropriate, include a statement of calculationintent, description of methodology used, assumptions and their justification,input data and equation references, numerical calculations including units, andresults. Input data may include:

• Regulatory requirements

• Performance and operational requirements under various conditions

. Material, geological, environmental, and geotechnical requirements

• Results of field and laboratory testing or calculations

. Information obtained from external personnel or literature and site datasurveys.

0-1 flR300275

Computer printout that becomes an integral part of the calculations shall bereferenced in the calculations by run number or other unique means ofidentification.

Calculations

Prior to any calculations, the following procedures will be followed:

A. Have experienced lead-person check design criteria for completeness andaccuracy before design begins.

1. Prepare checklists for various type projects to avoid omissions.

B. Require approval of basic design system before starting detailedcalculations.

C. Set up standard design procedures and format for use as guide.

D. Establish format requirements for calculations.

1. Must be neat and legible.

2. List all design assumptions. t

3. List all fonr'-lae and define symbols.

4. Group calculations for various portions of project.

Once all calculations have been completed, assignments for checking calculationswill be made by the Project Manager. An individual with technical expertise inthe calculation subject chosen will be chosen for checking purposes.

c-2

^ Drawings

The following procedures will be followed:

A. Require experience lead-person to check basic system sketches and typicaldetails for completeness and accuracy before placing on final drawings.

B. Require detailed check of all dimension and notes on drawings.

C. Require lead designer to check all schedules, design criteria, and typicaldetails.

D. Require lead designer to review all drawings to verify that sections anddetails are labeled correctly.

E. Require lead designer to coordinate drawings with other disciplines' drawingsfor workability and conformity.

F. Require supervisor (principal, department head) to "review" all drawings forgeneral check.

G. Prepare a form of standard "General Notes" as a guide to avoid omittingnecessary criteria.

Once all drawings have been completed, the drawings will be cheeked by proceduressimilar to the calculations check.

C"3 flR300'277

Specifications

The following specification procedure will be followed:

A. Do not specify untried or untested materials without reasonable research.

B. Develop standard master guide specifications

1. Edit master copies for each particular project.

2. Do not use specifications from similar or past projects.

C. Require lead designer to prepare technical sections for his/her portion ofproject.

Once specifications have been prepared, a complete technical review of thespecifications will be completed prior to printing, using similar checkingprocedures.

C-4

&R3QQ278

TCN 4204-01-QAPjPSECTION DREVISION NO. 0PAGE NA OF MA04/SEPT/90

APPENDIX D

AUDIT PROTOCOL

QUALITY ASSURANCE AUDIT CHECKLIST

Laboratory:

Screec Address:

hailing Address (If Different):

City ___________________ State _______________ Zip

Laboratory Telephone No.: Area Code _______ No. __

Laboratory Director: _____________

Quality Assurance Supervisor:

Personnel Contacted During Audit:

Name Title

Contract Number:

Contract Title:

Project Officer:

Audit Conducted By:

Agency and Address:

Telephone No.: Area Code _______ So.

Date Audit Performed:

8R30028Q

A. ORGANIZATION AND PERSONNEL

A.I. Review the Pre-AudU Worksheet and list questions from the Organ-ization and Personnel section of the Pre-Audit Worksheet to bediscussed during the QA audit.

—— -

Al.

Q2.

A2.

Q3.

A3.

Q4.

A4.

Q5.

AS.

D-2 flR300281

A.2. Organization and Personnel Checklist

Do personnel assigned to this project have theappropriate educational background to success-fully accomplish the objectives of the program?

Do personnel assigned to this project have theappropriate level and type of experience tosuccessfully accomplish the objectives of thisprogram?

Is project organization appropriate toaccomplish the objectives of this' program?

Is the project adequately staffed to meetproject coomitments in a timely manner?

Are project reporting relationships clear?

If any special training or experience isrequired, is it represented on the project staff?

Does the laboratory have a Quality AssuranceSupervisor who reports Co senior managementlevels?

Was the Project Manager available during theQA audit?

Was tht Quality Assurance Supervisor availableduring Che QA audit?

Docs the project schedule show adequate tine Coaccomplish the sampling program and does it allowfor uncontrollable delays, such as bad weather?

Does the project schedule allow sufficient timebetween sample collection and reporting of thedata to apply adequate analytical quality control,including supervisory review of the data?

res 'Jol Comment

D-3

A.3. Does the project organization plan and schedule give adequate attentionand time to the sampling and analysis effort? ______

Comments on project organization and schedule:

A.4. Are the personnel assigned to this project generally qualified toaccomplish the objectives of the program? ______

Comments on personnel:

D_4

3. FACILITIES

When touring the facilities, give special accencion co: (a) che overallappearance of organization and neatness, (b) che proper maintenance offacilities ana instrumentation, (c) the general adequacy of the facilitiesto accomplish the required work, and (d) sampling equipment required for theproject.

B.I. General Facilities Checklist

Does the laboratory appear to have adequateworkspace (120 sq. feet, 6 linear feet ofunencumbered bench space per analyse)?

Are voltage control devices used on majorinstrumentation (e.g., GC/MS, spectropho-tometers)?

Does the laboratory have a source of distilled/demineralized water?

Is the conductivity of disti lled/demineralizedwater routinely checked and recorded?

Is che analytical balance located away from draftand areas subject to rapid temperature changes?

Has the balance been calibrated within one year?

Are exhaust hood* provided to alloworganized work with volatile material*?

Is the laboratory maintained in a clean andorganized manner?

Are safe and contamination-free work area*provided for the handling of toxic or radio-active material*?

Are the radioactive and/or toxic chemicalhandling area* either a stainle** «teel benchor an imperviou* material covered with absorbentmaterial?

es o Comment

0-5

Are adequate facilities provided for storage ofsamples, including cold storage?

Are chemical waste disposal facilities adequate?

Are contamination-free areas provided for tracelevel analytical work?

Can the laboratory supervisor document that tracemetals-free water is available for preparation ofstandards and blanks?

Is organic-free water available for preparation ofstandards and blanks?

If biotesting is to be conducted, are adequateenvironment-controlled facilities available (e.g.,light, temperature control)?

Is the required field instrumentation and samplingequipment properly maintained?

Is adequate safety equipment (fire extinguishers,showers, eyewash stations) located throughout thelaboratory?

If bacteriological analyses are to b« conducted,is an aseptic work area provided?

Are bacteriological incubators maintained at theproper t«mp«racur« (35 + 0.5*C for total coliformand fecal scr«pcococcu«T 44.5 + 0.2*C for fecalcoliform)? ""

Are boats, ciotors, vehicles, and other mobilefacilities available at required?

es No Comment

P QHJ

on each one. an in.crumenc evaluation form

Inscrumenc——————— . Analysis

flR300286

INSTRUMENT EVALUATIONInstrument:

Instrument Mfg.

Model: ____________________ Year of Acauisition:

Condition:

Calibration Frequency:

Service Maintenance Frequency:

Other Pertinent Information:

Are Manufacturer's operating manualsavailable to the operator?

readily

Is there a calibration protocol available to theoperator?

Are calibrations kept in a permanent record?

Is a permanent service record maintained?

Has the instrument been modified in any way?

ves no

SATISFACTORY? L_J

Commtnts:

D_e SR3Q0287

Instrument:

d)

INSTRUMENT EVALUATION

Instrument Mfg.

Model: ______________________ Year of Acauisition:

Condition:




Are Manufacturer's operating manuals readilyavailable to the operator?





yes no

SATISFACTORY?

Comments:

D D

/JR300288

INSTRUMENT EVALUATIONInstrument:

Instrument Mfg.

Model: _____________________ Year of Acquisition:

Condition:




Are Manufacturer's operating manuals readilyavailable to the operator?





yes •no

SATISFACTORY?

Commenttt:

D

D-IO flR300289

C. ANALYTICAL METHODOLOGY

C.I. Review the Pre-Audit Worksheet and Use. items from the AnalyticalMethodology section of the Pre-Audit Worksheet to be discussedduring the QA audit.

Al.

Q2.

A2.

Q3.

A3.

Q4.

A4.

Q5.

AS.

D-H

C.2. Conduct discussions with two or more individuals who haveanalytical responsibilities in connection with the project. Thefollowing points should be addressed to determine each individ-ual's awareness and application of QA/QC procedures:

1. Specific project responsibilities,2. Level of knowledge of the analytical methods used,3. Awareness of and adherence to the laboratory's QC procedures,

and•*. Appearance and accuracy of the work records.

nalystName Responsibility

; omments:

AnalvstN«BC Responsibility

Conrvents:

DL-12

Analyst __________ __________ __Name Responsibility

Lonments:

AnalyseName Responsibility

Connencs:

C.3. Analytical Methodology Checklist.

.tern

Are stancard -rethods (e.g., EPA, ASTM, StandardMetnods for tne Examination of Water anaWast.ewat.erJ used when available?

lave standard methods been altered in any way?If so, .s it justified?

Are written analytical procedures provided totne analyst?

Are reaeent grade or nigner purity chemicals \used to prepare standards? ;

Are samoles analyzed within the linear rangeof the method in ail cases?

Does the standard curve bracket the concen-tration of the samples on each sample run?

Are fresh analytical standards prepared attne required frequency?

Are standards run periodically during along sample run?

Are reference standards properly labeled withconcentrations, date of preparation, and theidentity of the person preparing the sample?

Do the ana ly Jits record bench data in a neatand accurate manner?

Is the appropriate instrumentation used inaccordance with standard procedures.?

Are methods used which are appropriate to th«;sample matrix (e.g., saline waters , wastewaters)?

Kes No

I

i

i

Comment j

iI

;

1

if

flR300293

Item

Are analytical detection Limits adequate forthe purposes of the project?

Are the analytical procedures used adequatelydocumented? For examoie, if a standard me: nodis not available, is a written procedureincorporated into the project plan?

Are all strip charts properly labeled withinstru-ent conditions, date, and samplenumbers?

Are samp Us properly handled (e.g., organized,chilled as necessary, appropriate containers)before, during, and after analysis?

Yesl

|

.

So -.omment

|

C.4. Are the analytical methods used satisfactory to accomplish the objectivesof the program? _______ Are laboratory practices acceptable? _______

Comments on analytical methods and practices:

a-is

D. SAMPLING AND SAMPLE HANDLING

D.I. Review the Pre-Audit Worksheet and list the items from the Sanolir.sand Sample Handling section of the Pre-Audit Worksheet to bediscussed.

Al

A2.

03.

A3.

Q4.

A4.

Q5.

AS.

ff-16 5R300295

D.2. Conduct discussions with two or more individuals who have samplingresponsibilities in connection with the project. The followingpoints should b« addressed to determine each individual's aware-ness and application of appropriate sampling procedures:

I. Specific project responsibility,2. Level of knowledge of acceptable sampling procedures,3. Adherence to the project sampling plan, and4. Neatness and accuracy of field records.

FieldTechnician

Name Responsibility

Conments:

FieldTechnician

Name (Uapoiuibility

Comments:

D_17 SR300296

0.3. Stapling Equipment and Procedures Checklist.

Item

Are the sampling procedure* specificallydefined in the project QA plan or otherreferenced document?

Is the sampling program well organized?

lave appropriate techniques been used in•electing sampling sites?

Are proper containers used for samolecollection, transport, and storage?

Are sample containers properly prepared beforesamsle collection to avoid sample contamination?Containers for organic* should be solvent rinsed;'or trace metals, acid rinsed.

Are the proper preservatives used in the samples'or each parameter? (See Appendix U)

Are permanent labels affixed to sample containers?

)o the sample labels contain adequate information(date, tine, sample location, samples) and aunique sample identification number?

Are proper techniques used to collect representa-tive samples while avoiding sample contamination?

Are duplicate samples collected? What frequency?

Are samples shipped promptly to the laboratory inorder to meet recommended holding time deadlines?(See Appendix H)

Are chain-of-custody records available for inspec-tion? Are they neat and understandable? Have therequired custody signatures been obtained?

fes o Comment I

SR3002970-18

D.4. Field Notebooks. Review one or raore field notebooks and determine ifthe following information is recorded.

Item Yes|No| Camment

Is a permanent bound notebook used torecord all field data and observations?

Is the notebook reasonably neat andorganized, considering the use underadverse field conditions?

Are field instrument and in situ instru-ment calibration data recorded daily?

Are sample location, time, and numberaccurately and completely recorded?

Are in situ data neatly recorded in anunderstandable manner?

Are ambient data (i.e., weather)recorded when appropriate?

Are the necessary engineering data (e.g.,flow, operating conditions) recorded?

Have supervisory personnel reviewed the fieldnotebook and so indicated by their signature?

! i

I

iii' !i

i

i

D.5. I* th« sampling program adequate to accomplish the objectives of theproject? ________________

Comments on the sampling program and sample collection:

D.19 AR3Q0298

E. QUALITY CONTROL

E.I. Review the Pre-Audit Worksheet and List items from the QualityControl section of the Pre-Audit Worksheet to oe discussed.

Al.

Q2.

A2.

Q3.

A3.

A4.

Q5.

A.5

D-20 flR300299

1.1. Quality Control Manual Checklist

item

-oes :r.e laboratory maintain aQua.:!;/ Control Manual1

Does the manual address the importantelements or a QC program, including thefol lowing :

a. Personnel?

b. Facilities and equipment?

c. Configuration control of instruments?

d. Documentation of procedures?

e. Procurement and inventory practices?

f. Preventive maintenance?

g. Reliability of data?

h. Data validation?

i. Feedback and corrective action?I

j. Instrument calibration?

k. B»cord keeping?

I. Internal audits?

Does the QC Manual specify the frequency ofduplication and spiked sample analysis?

Is at lease 10 percent sample duplicationrequired?

Are QC responsibilities and reportingrelationships clearly defined?

r*T 75" vommenc

ij

i

+•21 AR300300

E.3. Quality Control Procedures Checklist

;iem

Select a reoresentat ive number ofanalyses from the project list and reviewhistorical ouality control data for theseparameters. Are QC records adequate forthe purposes of the project?

Are reference standards analyzed witheach set of samples?

Have standard curves been adequatelyidocumentea?i

Yes No Comment I————— " —————————— I1

j!iI

I1

1

Are laboratory standards traceable tothe National Bureau of Standards, whereappropriate?

Have standards been analyzed every20 or fewer samples to verify that theanalytical eiethod is in control?

Have the prescribed number (QC Manual orProject Plan) of duplicate and spikedsamples been analyzed?

Do duolicate data fall withinacceptable limits of precision?

Are recoveries, calculated from spikedsample data, acceptable?

Are quality control charts maintainedfor sach routes analysis? , ^

Do QC records show corrective actionwhen analytical results fail to MetQC criteria?

Do supervisory personnel review thedata and QC results?

ii

flR30030l

£•«**• Are Q u a i i' v ~ •* n - -> *accomplish the c ^ oT^"":"""" Wn-ril1"

5R300302

F. DATA HANDLING

r.l. Review the Pre-Audit Worksheet and list items from che DataHandling section of the Pre-Audit Worksheet to be discussed.

Al.

Q2.

A2.

Q3.

A3.

04.

Q'.

AS.

D-24 SR300303

F.2. Data Handling Checklist

item

Ask for a demonstration of data handlingprocedures from initial sample check-inCo reporting of the final data. Arethese procedures clear and adequate toavoid data errors?

Are data calculations checked by asecond person?

Are data calculations documented?

Do records indicate corrective actionthat has been taken on rejected data?

Are limits of detection determined andreported properly?

Are results which are below the analyticaldetection limit reported as such?

Are the data reported to « justifiablenumber of significant figures?

Are all data and record* retained at least3 years beyond completion of the project?

Are quality control data (e.g., standardcurve, results of duplication and spikee)accessible for all analytical results?

Are data reported in the appropriate units(e.g., ppm, mg/1, dry weight, metricmeasure)?

es to ^nmmianr

i

P-25

F.3. Are data handling procedures adequate to accomplish the objectivesof the project and to trace the accompanying quality controlresults?

Comments on data handling:

D-26 HR3003

G. SUMMARY

G.I. Summary Checklist

Item

Do responses to audit questions indicate chat .project and supervisory personnel are awareof QA and its application to the project?

Do project and supervisory personnel placepositive emphasis on QA/QC?

Have responses with respect to QA/QC aspectsof the project been open and direct?

Has a cooperative attitude been displayedby all project and supervisory personnel?

Are the personnel assigned to theproject qualified?

Does the organization place the properemphasis on quality assurance?

Have any QA/QC deficiencies beendiscussed before leaving?

Is the overall quality assuranceadequate Co accomplish the objectivesof the project?

Are any corrective actions required?If so, list the necessary actions below.

Yes to comment

•

D-27 AR300306

G.2. Summery Comments and Corrective Actions

e-28 flR300307

TCN 4204-01-QAPJPSECTION EREVISION NO. _0__PAGE MA OF _NA_04/SEPT/90____

APPENDIX EASSESSMENT OF DATA PRECISION, ACCURACY,

REPRESENTATIVENESS, COMPARABILITY. AND COMPLETENESS

flR3.00308

fI

TETRA TECH STANDARD OPERATING PROCEDURE

SPECIFIC PROCEDURES TO BE USED IN ROUTINELY ASSESSING DATA PRECISION

AND ACCURACY. REPRESENTATIVENESS. COMPARABILITY ANDCOMPLETENESS OF THE SPECIFIC MEASUREMENT PARAMETERS INVOLVED

Analytical Precision

Precision is determined by performing replicate analysis. For data sets witha small number of points (2 < n < 8), the estimate of precision will be expressedas range percent (R%):

X; -X2R% = ________ X 100

where X; = highest value determined

\2 - lowest value determined

X = mean value of the set

and n X/X = _

1-1 n

where X; = ith determination

n = number of determinations

For one or two values below the detection limit (BDL):

BDL = DL/2; where DL * detection limit.

E-l3R30Q3Q9

For large data sets (n > 8), the estimate of precision will be expressed aspercent relative standard deviation (%RSD):

n_ (Xi-X)2

S.D. = i-1_____n-1

RSD * S.D. x 100X

where n - number of replicate determinations

nr (Xi-X)2

X - mean s n

Analytical Accuracy

Percent accuracy (A) may be determined from the results of analysis ofperformance audit samples. Where appropriate, accuracy will be assessed bycomparison to a reference method. Accuracy as percent recovery (R) may bedetermined from the results of analysis of surrogate or analyte compounds spikedinto samples.

A « measured value x lOOaniR ** measured value x 200ortrue value amount spiked

R m measured value - amount found in native sample xamount or surrogate spiked

E-2 flR3003lO

Representativeness

Representativeness will be reviewed in relation to the sampling design.

Comparability

If data are to be compared to existing data bases, every effort will be made touse comparable sampling and analysis procedures. If necessary, comparabilitystudies will be designed, comparing two methods.

Completeness

Percent completeness (C) will be determined as below.

c = number of recoverable values xnumber of expected values

E-3

AR3003II