ENGINEERING EVALUATION AND COST ANALYSIS - APPENDIX B ...

I

ENGINEERING EVALUATION/COST ANALYSISAPPENDIX B

TREATABILITY STUDIES WORKPLANFOR

SOUTHERN SHIPBUILDING CORPORATIONSLIDELL, ST. TAMMANY PARISH, LOUISIANA

October, 1994

Prepared for:

J. Chris PetersonDeputy Project Officer

Emergency Response BranchEPA - Region 6

Contract Number: 68-WO-0037

/2.C2-7/ P000048

TABLE OF CONTENTS

SECTION

1.0 INTRODUCTION1.1 Purpose of Treatability Studies1.2 Treatability Studies Objective

2.0 TREATABILITY STUDIES RATIONALE2.1 Potential Removal Actions2.2 Contaminants of Concern

3.0 TECHNICAL APPROACH3.1 Treatability Study 1: Thermal Treatment3.2 Treatability Study 2: Biodegradation3.3 Treatability Study 3: Solidification/Stabilization3.4 Treatability Study 4: Soil Washing

4.0 TREATABIHTY STUDIES MANAGEMENT AND SCHEDULE

5.0 DATA ANALYSIS AND INTERPRETATION

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1.0 INTRODUCTION

1.1 Purpose of Treatability Studies

The purpose of the treatability studies (TS's) is to provide the data needed for the detailed analysis ofremoval action alternatives during the EE/CA and CD process for the Southern Shipbuilding Corporation(SSC) site. The objectives/data requirements of the TS's are both technical and administrative in nature;they have been developed to support the EE/CA and CD process including cost estimation for theabatement of contamination at the SSC site.

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1.2 Treatability Studies Objective

The TS's must support the activities addressed in the EE/CA and CD specifically the data objectives andneeds related to the technical and administrative requirements hi the assessment/selection of removalalternatives. Section 121(b) of the Comprehensive Environmental Response, Compensation, and LiabilityAct (CERCLA) of 1980 mandates EPA to select remedies that "utilize permanent solutions and alternativetreatment technologies or resource recovery technologies to the maximum extent practicable" and toprefer remedial actions in which treatment that "permanently and significantly reduces the volume,toxicity, or mobility of hazardous substances, pollutants, and contaminants is a principal element." Thepreference for alternative treatment technologies is extended'to site/removal actions by CERCLA Section104, which requires that site/removal actions contribute to the efficient performance of remedial actions.

Section 300.430(c) of the National Oil and Hazardous Substances Pollution Contingency Plan (NCP)specifies evaluation criteria to be considered in the aforementioned assessment/selection of removalalternatives. The assessment criteria to be incorporated for the SSC TS's are as follows:

1. overall protection of human health and the environment,

2. compliance with applicable or relevant appropriate requirements (ARARs),

3. long-term effectiveness and permanence

4. reduction of toxicity, mobility, and volume through treatment

5. short-term effectiveness

6. implementability

7. cost

8. agency and community acceptance

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2.0 TREATABILITY STUDIES RATIONALE

2.1 POTENTIAL REMOVAL ACTIONS

Section 3.3 of the EE/CA and CD work plan identifies potential removal actions proposed for theabatement of site contamination as follows:

1. Thermal Treatment

2. Biological Treatment

3. Solidification/Stabilization

4. Soil Washingr5. Landfilling

6. Isolation

7. Liquid Treatment

8. Air Emissions Control «

Data relevant to the evaluation of each of these potential removal actions will be gathered as part of sitecharacterization. Additional data will be generated on the first four alternatives through treatabilitystudies.

Since the finalization of the EE/CA Workplan, the approach to treatability studies has continued to evolveas additional parties got involved in the development of protocol.

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2.2 Contaminants of Concern

In order to meet the EE/CA project timeline, the treatability studies will commence prior to fullcharacterization of the wastes present on-site. There is sufficient previous impoundments characterizationdata to allow treatability testing to begin and reasonable assumptions to be made.

In order to design a treatability study to meet the information needs of a On-Scene Coordinator (OSC)or Remedial Project Manager (RPM), assumptions regarding contaminants of concern as they relate tothe respective treatability test must be made. Some assumptions upon which all four treatability studieswere based follow:

1. The matrices previously defined, indeed exist in the impoundments or surrounding soils.

2. The chemical composition of impoundment waste is relatively consistent with previoussample data.

3. The waste obviously has large petroleum component to it.

4. Volatile aromatic compounds present in the past analyses in relatively low concentrationswould be more readily treated by incineration and biodegradation than heavier molecularweight compounds.

5. The potentially most hazardous compounds found hi the waste are Polycyclic AromaticHydrocarbons (PAHs), especially several classified as carcinogens.

6. Action levels have been established for benzo(a)pyrene equivalents, a subset of PAHs,for the Bayou Bonfouca Superfund Site.

7. Although a variety of metals have been found hi elevated concentrations, the organicconstituents hi the waste are the focus of all four treatability studies.

8. Dioxins, PCB's, pesticides/insecticides have not been detected in previous sampleanalysis of the impoundment waste and all treatability work is based on this assumption

000053

1

3.0 TECHNICAL APPROACH

3.1 THERMAL TREATMENT

3.1.1 Introduction

Based upon existing chemical characterization of the material previously sampled from the two wasteimpoundments, thermal treatment appears to be a viable removal option.

Complete physical and chemical characterization of the wastes, including those parameters deemed to berelevant to thermal treatment is currently being conducted. The parameters which are being analyzed forare presented in the EE/CA work plan. Thermal treatment treatability samples are being collectedconcurrently with sample collection for physical/chemical characterization. Collection methodology andhealth and safety considerations are presented in the EE/CA QASP (Appendix A).

3.1.2 Treatability Contractor

The Incineration Treatability Tests will be conducted by Acurex Environmental Corporation at theIncineration Research Facility hi Jefferson, Arkansas under contract with the U.S.E.P. A. Risk ReductionEngineering Laboratory hi Cincinnati, Ohio. Edward Optaken, through Philip Lin are the EPA liaisonsto the SSC site. Refer to Section 4 for more information on the organization of this study.

3.1.3 Quality Assurance Project Plan

Following is a "Quality Assurance Project Plan" for the incineration treatability tests being conducted byAcurex.

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QUALITY ASSURANCE PROJECT PLAN FOR THESTART INCINERATION TREATABILITY TESTS OF

CONTAMINATED MATERIALS FROM THE SOUTHERNSHIPBUILDING SUPERFUND SITE

Revision 1

September 1994

Acurex Environmental Project 8455.1/8456.1EPA Contract 68-C9-0038, Work Assignment 4-1

Prepared forPhilip C. L. On, Technical Project Monitor

Gregory J. Carroll, Work Assignment ManagerRobert C. Thurnau, Project Officer

U.S. Environmental Protection AgencyRisk Reduction Engineering Laboratory

Cincinnati, Ohio 45268

Prepared byAcurex Environmental Corporation

Incineration Research FacilityJefferson, Arkansas 72079

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TABLE OF CONTENTS

Section12345

Pages RevisionIntroductionQuality Assurance ObjectivesSampling and Analytical ProceduresApproach to QA/QCReferencesAppendix A — Method 8015 Validation forthe Test Program VOC Target Analytes

84147117

111100

DateSeptember 30, 1994September 30, 1994September 30, 1994September 30, 1994

July 29, 1994July 29, 1994

m

000056

LIST OF ILLUSTRATIONS

Figure1-13-1

ThelRFTTUChain of custody

Name Section13

Page4 of 8

4 of 14

LIST OF TABLES

Table Name1-1 Test program measurements2-1 Precision, accuracy, and completeness objectives for critical

measurements2-2 QA objectives for critical analytical measurement MDLs3-1 IRF sample identifier convention3-2 Test program sample analysis summary3-3 Sample analysis aliquot schedule3-4 Sample containers, preservation methods, and hold times3-5 Analysis protocol3-6 Target SVOC analytes3-7 Target trace metal analytes4-1 Scheduled QC arid calibration for the VOC analyses by

GC/FID4-2 Scheduled QC and calibration for the SVOC analyses by

GC/MS4-3 Scheduled QC and calibration for the trace metals analyses by

ICP

Section12

233333334

4

4

Page7 of 82 of 4

4 of 42 of 145 of 146 of 148 of 149 of 1412 of 1413 of 144 of 7

5 of 7

6 of 7

Recipients of copies of this Quality Assurance Project Plan:

P. Lin - RRELG. Carroll - RRELR. Thurnau — RRELE. Opatken — RRELA. Leitzinger — RREL

L. Beach — Acurex Environmental (ERO)C. Goldman — Acurex Environmental (IRF)J. Lee — Acurex Environmental (IRF)D. Tabor — Acurex Environmental (IRF)S. Venkatesh — Acurex Environmental (IRF)

L. Waterland — Acurex Environmental (MVO) A. Siag — Acurex Environmental (IRF)J. MacDonell — Acurex Environmental (MVO) J. Bass — Acurex Environmental (IRF)

IV

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SECTION 1INTRODUCTION

Section 1Revision 1Date: September 30, 1994Page 1 of 8

The Southern Shipbuilding Corporation (SSC) Superfund site in Slidell, Louisiana, is aninactive barge/ship manufacturing and repair facility that conducted gas-freeing and barge cleaningoperations between 1917 and 1971. Wastes resulting from these operations were stored in twoprimary surface containment pits (the north pit and the south pit) located less than 25 miles fromBayou Bonfouca, a deep water channel that feeds into the largest lake in Louisiana, LakePortchartrain. During operations, wastes were initially pumped into the north pit directly frombarges. To avoid overflowing this pit, lighter organics and rainwater were periodically pumped tothe south pit. The south pit was connected to a baffle system. Wastewater was pumped throughthis system, which was designed to remove oily materials before the waste was discharged to BayouBonfouca. The discharge to the bayou was regulated under a National Pollutant DischargeElimination System (NPDES) permit.

The SSC facility has been operated by its current owner since 1957, which reportedly wasreorganized under Chapter 11 bankruptcy in May 1993. All site manufacturing and repairoperations ceased in August 1993 due to owner financial difficulties. Based on the results of ascreening site inspection (SSI) performed by the Louisiana Department of Environmental Quality(LDEQ) in December 1992, and several subsequent site inspections and evaluations by the EPARegion VI technical assistance team (TAT), the site has been placed on the National Priorities List(NPL), and efforts to remediate the site have been initiated.

Wastes and contaminated materials at the site have been classified into six categories asfollows?

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*—Light non aqueous phase liquids (LNAPL): tho "oily" liquid phase on the surface-el-thenorth pond

*—Dense non aqueous phase liquids (DNAPL): tho heavier than water liquid phase-thatrests on the bottom of both pits

*•—Sediment: solids obtained from the bottom of Bayou Bonfouca*—Sludge: oily solids at the bottom of tfie pits*—Soil: clay material beneath the sludge that has not been discolored*—Wastewater: the layer of water below the LNAPL and above the DNAPLThe contaminants of concern in all site materials are various organic constituents classified

as total petroleum hydrocarbons (TPH), target compound list (TCL) volatile organic constituents(VOCs), and TCL semivolatile organic constituents (SVOCs). In addition, site materials containvarying levels of hazardous constituent trace metals.

Four candidate remedies for treating one or more of these site materials are underconsideration: incineration, bioremediation, solidification and stabilization, and soil washing. Aseries of bench-scale treatability studies using these candidate remedies is planned to supply theIPHPdate-to allow choosing the most applicable remedy for |||S|eaeh-material|. The SuperfundTechnical Assistance Response Team (START) within EPA's Risk Reduction EngineeringLaboratory (RREL) has been asked to coordinate these treatability studies. The incinerationtreatability study will be performed in the thermal treatment unit (TTU) at EPA's IncinerationResearch Facility (IRF). This quality assurance project plan (QAPP) describes the treatability testprogram planned.

The objectives of this treatability test program are to:* Determine the degree of organic contaminant decontamination achieved for different

combinations of incineration treatment temperature and treatment residence time;

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degree of decontamination is measured by the decontamination effectiveness, definedto be: 100 • (1 - (mass of contaminant in treated waste)/(mass of contaminant inwaste))

• Determine whether the treatment residue from various combinations of treatmenttemperature and treatment residence time are toxicity characteristic (TC) hazardouswastes because of leachable trace metal content

Treatability data for two site materials will be developed; each site material will be tested at twotreatment temperature/treatment time combinations.1.1 TEST FACILITY DESCRIPTION

The TTU at the IRF consists of a small commercial pathological incinerator that has beenmodified to allow for continuous test material feed and treated material (e.g., ash) removal, forvariable and controlled thermal treatment temperatures, for expanded process operation monitoring,and for combustion flue gas sampling. The TTU is illustrated in Figure 1-1.

The combustor portion of the TTU consists of three chambers: the charge chamber, theretention chamber and the breeching chamber. The charge chamber is designed to accept theTTU's solid material feed stream. It corresponds to the primary combustion chamber, or kilnportion, of a waste incinerator. Its inner cross section is 0.66 m (2 ft 2 in) square, its height 1.9 m(6 ft 2 in), and its chamber volume 0.82 m3 (29 ft3). The retention chamber, which directly followsthe charge chamber, is designed to effect complete organic constituent destruction. It correspondsto the secondary combustion chamber, or afterburner portion, of a waste incinerator. Its inner crosssection is also 0.66 m (2 ft 2 in) square, its height 1.5 m (5 ft), and its chamber volume 0.67 m3

(23.5 ft3). The breeching chamber serves as a second-stage afterburner. Its inner diameter is0.41 m (1 ft 4 in), its total height 0.76 m (2 f t 6 in), and its chamber volume 0.10 m3 (3.5 ft3). Allchambers are lined with a 13-cm (5-in) thickness of refractory.

000060

TEM

\J

CTOMOV-2 [- - Tg

-«- -1TEMP INDICATING

CONTROLLER

(jTO MOV-1 -J,-^ — — - Tl<

1TEMP INDICATING

CONTROLLER

retCONVI

(f)TEMP INDICATOR


STACK

-I SAMPLING~ZJ PORTS

BREECHINGCHAMBER

RETENTIONCHAMBER

CHARGECHAMBER

I II L.

aCOui

BURNERS

BURNER 2

RECORDER

C) BURNER 1

ASH

TEMP INDICATOR

Figure 1-1. The ffiF TTU

000061


As received from the incinerator vendor, all three chambers were designed to be fired withnatural-gas-fueled burners. The burners installed in the charge and retention chambers are natural-gas-fired, with 350 kW (1.2 million Btu/hr) capacities and 5-to-l turndowns. Modulating burnercontrols allow variable firing rates to control temperatures in each chamber at preset levels between260° and 1090°C (500° and 2000°F) with variable air-to-fuel ratio. The breeching chamber has amanually adjustable 220 kW (750,000 Btu/hr) burner. ~

Test material is fed to the charge chamber via a feed system that transports quartz trayscontaining the test material through the chamber via a variable-speed chain-drive mechanism. Eachquartz tray is 18 cm (7 in) long by 8 cm (3 in) wide by 4 cm (1.5 in) deep. The variable-speed chaindrive allows trays containing test material to have charge chamber residence times of between 20min and 1 hr. Multiple trays can be fed in sequence to simulate continuous feed to a thermaltreatment system.

Combustion gas temperatures are recorded using type K or R thermocouples at thefollowing locations in the system:

• Inside feed door• Inside discharge door• Bottom of charge chamber center• Charge chamber exit gas• Retention chamber exit gas• Breeching chamber exit gas• Stack gas

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L2 PLANNED TEST PROGRAMTwo SSC site materials will be subjected to testing:

j ^^^^^^^thc DNAPL and the sludge' from the north pit at the site. Each material will betested at two TTU operating conditions. These test conditions will be:

• Charge chamber gas temperature (i.e., incineration treatment temperature) of 870 °C(1,600°F) with treatment residence tfme of 20 minutes

• Charge 'chamber gas temperature of 980 °C (1,800 °F) with treatment residence time of60 minutes

One 5-gal (19-L) container of each site material will be required at the IRF for the testprogram. In preparation for the tests, each container's contents will be transferred to a 25-gal(95-L) galvanized container and mixed to produce a homogenous mixture. Three samples will bethen be taken to fill three 1-L jars. A 1-lb (0.45 kg) quantity of the mixed material will then beplaced into each of seven quartz trays for feeding into the TTU for each test. Unused test feedmaterial will be returned to the original 5-gal containers.

After completion of each test, the contents of the seven trays will be weighed, mixed witha small shovel in a 2.5-gal (9.5-L) container, then transferred into 1-L jars for storage until analysis.

For each test, the TTU will be allowed to reach steady state at the desired temperaturescondition. The seven feed trays will then be sequentially fed to the TTU each remaining in thecharge chamber for the specified residence time. For each test, the measurements listed inTable 1-1 will be taken. The table also indicates which measurements are critical toward meetingthe test program objectives noted earlier.13 SCHEDULE AND ORGANIZATION

Testing will begin in October 1994. Two tests will be attempted per day, thus, testing shouldbe complete within 1 week.

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Table 1-1. Test program measurements

ParameterProcess measurementsTTU gas temperature (see Figure 1-1)

Analytical measurementsFeed material concentrations:

MoistureAshHeating valueOil and greaseTotal organic carbon (TOC)TPHVOCsSVOCsTrace metals

Treatment residue concentrations:TOCTPHVOCsSVOCsTrace metals

Feed material and treatment residue TCLPleachate concentrations

Trace metals

CriticalMeasurement

S

< •-

/"//

/Ss

s

NoncriticalMeasurement

/SsSS

S

S

S

000064


Dr. Larry Waterland, the Project Manager for the IRF operations and research program,will have the overall responsibility for the success of this project, and will review and approve thisQAPP and the test report. Mr. Johannes Lee, the Onsite Manager of the IRF program, willprovide overall technical direction of this project. Shyam Venkatcsh, the TestEngineer for this project, will be responsible for detailed test preparations; overall conduct of thetests; and test data integration, interpretation, and"'reporting. ||||||S||pDr. Venkatesh will alsodirect the operation of the TTU for all tests. This includes ensuring that the system is operated toachieve desired test conditions; and that operating data are reduced and summarized. Ms. CarlaGoldman, the IRF project QA Manager, will oversee all QA activities for the project. This includesselected auditing of the sampling efforts, and evaluating and reporting all project QA data. Ms.Joan Bass, the Sample Custodian for the IRF program, will handle all sample custody activities inthis project. These include receiving samples from individual samplers, ensuring that all sampleinformation is logged into the IRF laboratory records, and arranging sample transfer to offsitelaboratories for analysis while ensuring that standard IRF chain-of-custody procedures are followed.

The critical VOC and SVOC analyses and the noncritical moisture, ash, and heating valueanalyses for this test program will be performed in the IRF onsite laboratories under the directionof Mr. Dennis Tabor, the IRF Laboratory Supervisor. The critical TPH and trace metal analysesand the TCLP extractions for this test program, and the noncritical TOC, oil and grease, and solidmatrix trace metal analyses will be performed by joffsite, contracted laboratories. Mr. Tabor will direct these offsite analyses as well. The project QAManager will coordinate and monitor the offsite laboratory QA effort, and will transmit theappropriate QA requirements to the laboratory. This will be done by sending this QAPP. It is theresponsibility of the QA Manager to ensure that the QA requirements are followed and that theIRF receives the QAPP-specified QC information back from the laboratory.

000065


SECTION 2QUALITY ASSURANCE OBJECTIVES

As noted in Table 1-4, the critical measurements that will be taken to address the testr-.program objectives discussed in Section 1 are:

• Process parameters— TTU gas temperatures

• Analytical measurements— TPH concentrations in test feed materials and treatment residue samples— VOC concentrations in test feed materials and treatment residue samples— SVOC concentrations in test feed materials and treatment residue samples— Trace metal concentrations in TCLP leachates of test feed materials and treatment

residuesThe Sampling and analysis procedures to be used to obtain these critical measurements are detailedin Section 3. Project quality assurance objective (QAOs) for measurement precision, accuracy, andcompleteness are summarized in Table 2-1.

For the critical measurements, precision will be determined as the relative percent difference(RPD) of duplicate sample analyses. Accuracy will be measured by measuring matrix spikerecoveries from sampled matrices. Completeness will be measured as a percentage of the numberof valid analytical results obtained relative to the number of analyses performed. The definitionsand calculation procedures for determining precision, accuracy, and completeness are given inSection 4.

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Table 2-1. Predsion, accuracy, and completeness objectives for critical measurements

Measurement parameterTTU gas temperatures

SVOCs in feed and residue samples

VOCs in feed and residue samples

Mercury in TCLP leachate samplesOther trace metals in TCLP leachate samples

Measurement/analytical methodType K thermocouples

Extraction, concentration,QC/MS analysisPurge and trap OC/FID analysis

CVAASICP

Reference-

SW-846 Methods 3540Aand 8270ASW-846 Methods 5030Aand 8015ASW-846 Method 7470SW-846 Methods 3015Aand 6010A

Conditions-

Methylene chlorideextractionMethanol extract offeed samples

—Acid digestion

Precision,RPDN.D.a

8

50

50

3030

Accuracy,%±5!!!

D-227b

37-162°

70-13070-130

Completeness,%90I

70

70

7070

*N.D. = No objective defined.bD denotes detected; compound-specific acceptance criteria will be taken from column 5 of Table 6 of Method 8270A.cCompound-specific acceptance criteria will be taken from column 5 of Table 6 of Method 8240A.

M~ <01 (?•"

O"

000067


The TTU gas temperature measurement accuracy objective noted in Table 2-1 is±5 percent. This accuracy objective can be easily met by using standard thermocouples readilyavailable from equipment manufacturers. These thermocouples meet the ANSI MC 96.1 (1975)standard which specifies the limits of error for type K thermocouples to be ±0.75 percent.Thermocouples meeting these standards will be used exclusively for this test program.

QAOs for method detection limits (MDLs) for th&critical analytical measurements are givenin Table 2-2. The MDL objectives in the table are consistent with or above the estimatedquantitation limits (EQLs) documented in the methods to be used to make in measurements. Thelaboratory that will perform the TPH and trace metals analyses will be required to meet the MDLobjectives noted.

The TCLP leachate MDL objectives noted for trace metals in Table 2-2 are, at most, nogreater than 2 percent of the corresponding metal's TCLP regulatory level. Thus, more thansufficient sensitivity will exist to allow evaluating whether treatment residues are TC hazardous.

Because EPA-approved methods will be used for critical measurements, results will berepresentative of the sample media and system conditions being measured. Because all test datawill be reported in a manner consistent with these methods using standard units, the test datagenerated will be comparable to both other IRF data sets and other organization data developedusing comparable EPA-approved methods.

The overall impact to this program of failure to meet one or more of the QA objectives, inspite of the implementation of corrective action measures, would be to compromise the applicabilityof the data to the achievement of the technical objectives. For example, failure to meet an accuracycompleteness objective for analysis of trace metals in treatment residue TCLP leachates wouldlessen the confidence in the reported trace metal concentrations in these samples, which could resultin no, or poorly justified, conclusions regarding whether the treatment residue was a characteristichazardous waste.

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Table 2-2. QA objectives for critical analytical measurement MDLsa

Measurement ParameterSVOCs (see Table 3-6)VOCsTPHTrace metals0

TCLPAsBaCdCrPbHgSeAg

OthersSbBeCoCuMnNiTlVZn

MDL ObjectiveTest Feed and Treatment

Residue, mg/kg1

0.5To

10100.51

0.50.05105

100.155151051

TCLP LeachatesMg/Lbbb

1001005105

0.510050

bbbbbbbbb

aFor samples not requiring dilution to bring analyte concentrations into instrument calibratedrange.bMeasurement not performed on this matrix, QAO not needed."Trace metal measurements in test feed and treatment residue samples are not critical,although MDL objectives have been defined nevertheless.

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SECTION 3SAMPLING AND ANALYTICAL PROCEDURES

3.1 SAMPLING PROCEDURESSamples of the test feed materials and treatment residue matrices will be collected for test

program analyses. Sampling of feed material will be as noted in Section 1. To reiterate, the 5-galof feed material received for testing will be mixed to homogeneous appearance in a 25-gal mixingcontainer, and three 1-L samples will be collected prior to charging the quartz trays for feeding tothe TTU. After a test, the entire treatment residue from the seven trays fed will be collected intoone container and mixed. Mixed treatment residue samples will be transferred to 1-L jars forstorage until analysis.

All samples from a given test will be placed in appropriate containers which will be labeled,transferred to the IRF onsite laboratory, and logged in by the sampler or by the Sample Custodian.After logging in, any requisite splitting, preservation, or preparation for shipping for analyses willoccur. All data pertaining to the sample will be entered into the laboratory informationmanagement system by a member of the laboratory staff.

Each sample generated for this test program will be assigned a unique ID number. Theconvention for assigning ID numbers is outlined in Table 3-1. The sample identifiers are physicallyattached, via labels, to the sample container upon receipt of the sample. The identifier is alsoentered in a sample log, along with information regarding the manner in which the sample wasprepared or preserved, the solvent in which the sample is concentrated, and other informationpertinent to the analysis. Through this procedure, a history is created for each sample that givesinformation as to source, time, and procedures employed on the sample.

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Table 3-1. ERF sample identifier convention

Form of Sample Identifier YMDDHHMM 1 2 3 4 5Original Generation Suffix

Original GenerationY= Year, last digit: 1 = 91,2 = 92, etc...M = Month:

Jan — 1, Fob — 2, Mar — 3, Apr — 4, May — 5, Jun - 6,Jul - 7, Aug - 8, Sep - 9, Oct - A, Nov - B, Dec - C

DD = Day, numeric ,..HH = Hour, numeric 24 hour conventionMM = Minute, numericSuffix

Sample type:A Afterburner exit flue gasB Scrubber liquorE Baghouse exit flue gasF FeedK Kiln exit flue gasP Preburn feedQ Prepared in laboratoryS Stack gasT Kiln bottom ashU Baghouse ashW Scrubber exit/baghouse inlet flue gasZ Other

3 = Sample Fraction0 Total sample1 Individual impinger or impactor stage 12 Individual impinger or impactor stage 23 Individual impinger or impactor stage 34 Individual impinger or impactor stage 4F FilterI Combined impingersM Primary probe wash + ImpingerP Primary probe wash + FilterT Secondary probe wash (Toluene)V Secondary probe wash (HNO3)W Primary probe washX Sorbent resin (XAD -2)Z Other

QA Description0 Not applicableD Split sample duplicateS Spiked sampleP Spiked sample duplicateL Lab blankM Method blankF Field blankT Trip blankZ Other

Sampling Procedure0 Not ApplicableA Cascade impactorC CompositeF Fluoride train (13B)G GrabH Mercury train (101A)M Multiple metals trainP Method 5 (particulate/HCl)R Arsenic train (108)S Modified Method 5 (0010)T High volume Method 17 trainV VOST(0030)X Dioxin train (23)Z OtherPreparation Procedure0 NoneB Organic extract in BenzeneD Digestion or fusion digestateE Aqueous leachate — EP toxicityF Filtration FiltrateG Organic extract in HexaneH Organic extract in Hexane of

TCLP leachateM Organic extract in Methylene chlorideN Organic extract in Methylene chloride

of TCLP leachateS Filtration solidsT Aqueous leachate - TCLPW Aqueous leachate — WaterZ Other

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For onsite work under Category IV projects, a formal chain-of-eustody form is not required.Sample recordkeeping does not involve transport of the samples any significant distance, andtransfer from one IRF staff member to another does not require a transfer document. Analyticalsamples are logged in by the laboratory staff member who prepared the sample or by the SampleCustodian. For transfer of samples from the IRF to another facility, for example, the offsitelaboratories for TPH or trace metal analyses, the Sample Custodian is responsible for sampleshipment. Samples shipped to the offsite laboratory will be shipped via overnight service to avoiddelays in beginning the analysis. A chain-of-custody form (Figure 3-1) is included with eachshipment.

Table 3-2 summarizes the number of samples of each matrix to be collected or prepared forthe set of analyses to be performed.

Table 3-3 summarizes the sample aliquoting schedule for dividing samples taken among theapplicable analytical procedures. Aliquots planned for analysis as noted in Table 3-3 generallycorrespond to respective method-recommended sample sizes. Hf

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COC # 910250ACUREX ENVIRONMENTAL LABORATORY

U.S. EPA INCINERATION RESEARCH FACILITY

CHAIN OF CUSTODY AND ANALYSIS REQUEST RECORD

Page. ofPhone:(501)541-0004Fax: (501)536-6446

Pro]eot NameSend Lab Results to:

ItemNo.MasterIndexNumber

Dennis TaborAcurex Environmental Corfc/o NCTR, Bldg 45Jefferson. AR 72079

Sample ID Number

Relinquished by:(Signature)

Relinquished by:(Signature)

SolidorUq.

Date/Time//

Date/Time//

DateSampled

To:

Phone!

No.ofContain

AnalysisDueDate

Received by:(Signature)

Received for laboratoryby: (Signature) Date/Time//

Preser-vationAnalysis/Method

Requested

Relinquished By:(Signature)

PLEASE FAX ACOPY OF THIS FORMTO ACUREX AFTERSAMPLE NUMBERSHAVE BEEN ASSIGNED

Remarks

1

I.E.Init

Date/Time//

Receiving Party'sSample ID #

Received by:(Signature)

Remarks:

5 93 t^iSI

Figure 3-1. Chain of custody

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Table 3-2. Test program sample analysis summary

Sample matrixTest feed materialTest sampleHlPISI Split sampleMatrix spikeSpike duplicate

TTU dischargeTest sample

' sampleiVJLcurix soiivwSpike duplicate

TCLP leachateTest feed materialTTU discharge

sampleXTSpike duplicate

Method blankTotal

Number of analyses

TPH

2jf-4-Jf4-I4-

4

m*-

VOCs

2|4-|-4-!*•

4|4-flk-I4-

&&•

SVOCs

2

4P-g-j-1-4-

1P2-

TOC

2

4

6

TraceMetals

2

4

241111

16

Moisture, Ash,Heating Value

2

2

Oil andGrease

2

•1

2

TCLPExtraction

2

4

6 £ MB« fl S- g-^ . . s- §reI>-iusoVO

000074

Table 3-3. Sample analysis aliquot schedule

SampleTest feedmaterial

TTUdischarge

TCLPleachates

Total QuantityCollected

3kg

All (at least H400 g expected)

2L

Analyte/ProcedureTPHVOCsSVOCsTrace metals"MercuryTOCMoisture, ash,heating valueOil and greaseTCLP extractionTPHVOCsSVOCsTrace metals*MercuryTOCTCLP extractionTrace metals

Mercury

Aliquot SizePer Analysis

4 g10 g2g2glg10 g

HI188*100 g

4g10 g2g2 glg

100 g100 mL

100 mL

Number of Aliquots Needed1 each sample + 1 BI ^^^K + P1 MS + P= MSD

1 each sample + 1 ||||||i;ip;§ppsplit + ffl MS + f|l MSD1 each sample + 1 |||j||p|||| ||spUt + f|l MS + ffjl MSD1 each sample1 each sample1 each sample1 each sample

1 each sample1 each sample1 per test + 1 i UU^plit + §4 MS + 1 1 MSD1 per test + 1 §||S|||m|l||5plit + |4 MS + 1 1 MSD1 per test + 1 + '|* MS + § 1 MSD

r1 per test1 per test1 per test1 per test6 test samples + 1 method blank + 1 a|||pailplspUt + 1 MS+ 1 MSD """ "" ""•"""""'" '"""6 test samples + 1 method blank + 1 |ii |ipp||yaip|i plit + 1 MS+ 1MSD

^ O 5« tj?P BJ ft 2era R :§ g.n - -

(t3ff

*Other than mercury.

000075


Table 3-4 summarizes the containers to be used for sample aliquot storage until analysis,

analysis hold times to be adhered to. Only ne.w containers are used for sample storage. They arepurchased, precleaned to meet EPA standards, from a laboratory supply vendor, and are certifiedby the vendor as appropriate for use in storing samples for the respective analyte class.

A minimum number of containers will be used to store each sample collected for eachanalysis. Aliquots will be taken from these containers as needed. MS and MSD samples will beprepared from aliquots from these containers as well. After, preparation however, MS and MSDsamples will be stored in separate containers until analyzed.

Unused sample collected will be stored in appropriate containers with appropriatepreservation until the expiration of method hold times. After method hold time has expired, unusedsample will be archived.32 ANALYTICAL PROCEDURES

Table 3-5 lists the analysis procedures to be applied to test program samples. As indicatedin the table, one sample of each feed material and each test treatment residue will be analyzed for

• TPH by Method 418.1• VOCs by purge and trap gas chromatography/flame ionization detector GC/FED by

Method 80 ISA; the high level soil method of sample introduction in Method 5030A,which involves extracting the sample in methanol, then adding the extract to the purge

000076

Table 3-4. Sample containers, preservation methods, and hold times

SampleTest feedmaterial

TTU residue

TCLP extracts

AnalyteTPHVOCs

SVOCs

Trace metals

TOCMoisture, ash,heating valueOil and greaseTCLP extractionTPHVOCs

SVOCs

Trace metals

TOCTCLP extractionTrace metals

Sample Container*G3-S-48I) mL VGAWK*vialsG, T

Go rP

GG

GG o r PGS*4fl|$ mL VOAvialsG,T

G o r P

GG o r PGo rP

It

11

11

1111

11HIII1111111nHiI!

SamplePreservation

MethodCool to 4°CCool to 4°C

Cool to 4°C

None

NoneNone

Cool to 4°CNoneCool to 4°CCool to 4°C

Cool to 4°C

None

NoneNoneHN03 to pH <2

Analysis Hold Time28 days14 days

Extraction: 14 daysAnalysis: 40 daysMercury: 28 daysOthers: 6 months28 days6 months

28,1days28 days28 days14 days

Extraction: 14 daysAnalysis: 40 daysMercury: 28 daysOthers: 6 months28 days28 daysMercury: 28 daysOthers: 6 months

00

"G = glass, P = polyethylene, T « Teflon-lined cap. csI—»VO

000077


Table 3-5. Analysis protocol

SampleTest feed material

TTU residue

TCLP leachate

AnalyteTPH

VOCs

SVOCs

Trace metals(except mercury)MercuryTOCMoisture and ashHeating valueOil and greaseTCLP extractionTPH

VOCs

SVOCs

Trace metals(except mercury)MercuryTOCTCLP extractionTrace metals(except mercury)Mercury

Analysis Method

jjjgg

Purge and trap of methanol extract by Method 5030A,GC/FID by Method 8015Ab

Soxhlet extraction by Method 3540A, GC/MS analysisby Method 8270Ab

Microwave digestion by the BIF method0, ICPanalysis by Method 6010Ab

CVAAS by Method 7471b

Method 9060b

ASTM D-5142ASTM D-3289Method ffita/OfeMethod 1311b

Purge and trap of methanol extract by Method 5030A,GC/FID by Method 8015Ab

Soxhlet extraction by Method 3540A, GC/MS analysisby Method 8270Ab

Microwave digestion by the BIF method0, ICPanalysis by Method 6010Ab


Method 9060b

Method 1311b

Microwave digestion by Method ||||-36§i, ICPanalysis by Method 6010Ab


FrequencyI/feed

I/feed

. I/feed

I/feed

I/feedI/feedI/feedI/feedI/feedI/feedI/test

I/test

I/test

I/test

I/testI/testI/testI/test

I/test"Reference 1, Water and wastes.••Reference 2, SW-846.cReference 3, BIF methods.

000078

The ^


vessel, will be usedS VOCs using GC/mass spectrometry (MS) by Method 8270A of Soxhlet extracts of thesamples in methylene chloride

Trace metals other than mercury using inductively coupled argon plasma (TCP)spectroscopy by Method 6010A; samples will be digested using the microwave-assisted,two acid procedure specified for particulate filter samples in the multiple metals methoddocumented in the boiler and industrial furnace (BIF) regulations (Reference 3)Mercury using cold vapor atomic absorption spectroscopy (CVAAS) by Method 7471TOC by Method 9060

ria measurements are those for TPH, VOCs, and SVOCs

000079


The target VOC analytes will be benzene, ethylbenzene, toluene, and total xylene (BETX).Although none of these are Method 8015A analytes, the method has been validated for them at theIRF. Validation data are given in Appendix A. 4-Bromofluorobenzene (BFB) will be added to allsamples as a surrogate standard prior to analysis. An initial 5-point calibration curve (ICAL) willbe generated by analyzing standards containing the 4 target analytes. Initial calibration acceptancecriteria are given in the method. The calibration curve will be verified each analysis day byanalyzing a midpoint calibration standard. Daily calibration acceptance criteria are also given inthe method. The average response factor from the ICAL will be used for analyte quantitation intest samples. All method specifications and QA procedures will be followed.

The target SVOC analytes are listed in Table 3-6. All target analytes are routine Method8270A analytes. This list of analytes will also be the calibration check compounds (CCCs) and thesystem performance check compounds (SPCCs) referred to in Method 8270A.

Acceptance criteriafor both the ICAL and the continuing calibration check (CCAL), as well as instrument tuningcriteria are given in the method.

000080

Table 3-6. Target SVOC analytes

AcenaphtheneAcenaphthyleneAnthraceneBenzo(a)anthraceneBenzo(b)fluorantheneBenzo(k)fluorantheneBenzo(a)pyren£Benzo(ghi)peryleneCarbazoleChryseneDibenzo(a,h)anthraceneDibenzofuranFluorantheneFluoreneIndeno( l,2,3-cd)pyreneIsophorone2-MethylnaphthaleneNaphthalenePhenanthrenePyrene


All target analytes are base/neutral compounds, so only the base/neutral surrogate standardsnoted in the method — 2-fluorobiphenyl, nitrobenzene-d5, and terphenyl-d14 — will be added to testsamples. Target analyte quantitation in test samples will be by the internal standard procedure.Five internal standards will be used — naphthalene-dg, acenaphthene-d10, phenanthrene-d10,chrysene-d12> and perylene-d12. All other method specifications and procedures will be followed.

The target trace metal analytes are listed in Table 3-7. All those except mercury will bedetermined by ICP. Trace metal analyses in feed and treatment residue samples are not critical

000081


measurements. Nevertheless, all method specifications and QA procedures, with the exception ofrequirements for : !|§|l|sptit-sample and matrix spike sample analyses, will be followed.

In addition to the above, the two test feed material samples will be subjected to additionalanalyses. Specifically, the feed samples will have their moisture content, ash content, and heatingvalue determined by the ASTM procedures noted in Table 3-5. Oil and grease analyses will beperformed on feed samples by Method ^9070. None" of these additional procedures are criticalmeasurements. The moisture content analysis is a loss on drying at 105°C measurement. If either^ffi ^^^^^^he-BNAPL or sludge contains organic constituents with boiling points near orless than 105 °C, their loss will be included in the reported moisture content measurement.

Both the two test feed material samples and the treatment residue sample from each testwill be extracted by the toxicity characteristic leaching procedure (TCLP). The resulting leachateswill be digested using Method ^pp85i-and analyzed by ICP for the seven non-mercury metalsunder the "TCLP metals" heading in Table 3-7. Mercury will be determined in TCLP leachates by

Table 3-7. Target trace metal analytes

TCLP MetalsArsenicBariumCadmiumChromiumLeadMercurySeleniumSilver

Other MetalsAntimonyBerylliumCobaltCopperManganeseNickelThalliumVanadiumZinc

000082

1Section 3Revision 1Date: September 30, 1994Page 14 of 14

CVAAS using Method 7470. The "other trace metals" in Table 3-7 will not be measured in TCLPleachate samples.

000083

SECTION 4APPROACH TO QA/QC


4.1 QC CHECKS•*•.

The QC check program for the laboratory analyses performed for these tests will consist ofanalyzing a method blank, preparing and analyzing MS and MSD samples, and analyzingreplicate samples.

The method blank sample to be analyzed for the test TCLP metals will be the TCLPextraction fluid. This sample will be taken through the entire leaching procedure as if it were a testsample.

As indicated in Table 3-2, one set of matrix spike/matrix spike duplicate (MS/MSD)samples for the test £I?e(Iimaterial feed and treatment residue matrices will be prepared and* vysSvSS&S&S&K I. JL

analyzed for the critical measurements: TPH, VOCs, and SVOC. The spiking level will be at5 times the MDL objective concentrations noted in Table 1-2, unless prior knowledge of the samplenative concentration indicates that this spiking level would be insignificant compared to the nativeconcentration. In such cases, the spiking level will be at twice the native concentration.

.-**-1

000084


VOC and SVOC MS/MSD samples will be prepared by spiking an aliquot of a test sample

respective procedure's target analytes ^^^^p^^ i ^^S l ^ | ^p^ . TPH MS/MSDsamples will bo prepared at the IRF and submitted as routine test program samples to the offsiteanalysis laboratory.—Thus, those external MS/MSD samples will serve as the test program'sindependent check of the laboratory, and will augment this laboratory's own internal MS/MSDanalysis schedule.—TPH MS/MSD samples will be prepared ||f||||by spiking n-hexadecane,isooctane, and chlorobenzene in the proportions cited for the reference oil in Method 418.1

The offsite laboratory performing the trace metal analyses and TCLP extractions will berequired to prepare at least one set of TCLP leachate MS/MSD samples by spiking the 8 TCLPmetals, and to report analyzed trace metal and mercury concentrations and spike recoveries.

Measurement accuracy will be determined as the percent matrix spike recovery from theMS/MSD analyses as well as by the percent surrogate recovery in the VOC and SVOC analyses.Measurement precision will be determined by the RPD of the MS/MSD analyses. In addition, onesample of each of the test sample matrices will be analyzed in duplicate for the criticalmeasurements as a further measure of precision. Specifically, one Sa jpSffila^^test feed material» r •" :«kK iS*5«:iSSi5WiSlSwaSS::

and one treatment residue sample be analyzed in

000085


duplicate for TPH, VOCs, and SVOCs. Separate extractions of the duplicate sample will beperformed to support these analyses. One TCLP leachate sample prepared will be analyzed induplicate for the TCLP metals. The duplicate sample will be separately digested.

Table 4-1 summarizes the QC procedures performed, their frequency, associated acceptancecriteria, and corrective actions to be initiated in the event that acceptance criteria are not met forthe VOC analyses. Tables 4-2 and 4-3 provide analogouslsummaries for the SVOC and TCLP tracemetal analyses, respectively. Acceptance criteria for the method blank will generally be no analyteconcentration above the analyte MDL objective. Not meeting an acceptance criterion will triggeran investigation into the cause of the failure. Corrective actions will depend on the investigativefindings.42 CALCULATION OF DATA QUALITY INDICATORS

As noted above, analytical accuracy will be determined by analyzing matrix spike samplesand determining the recovery of the spiked analytes. Analytical accuracy is also measured bydetermining surrogate recoveries in the VOC and SVOC analyses. The individual recovery valuesfor the specific spiked analytes are then compared to the project QAOs specified in Section 2.Spike recovery is calculated from the expression:

<y RECOVERY = Sample Result - Native Sample Result) x 100Spiked Amount

Measurement precision will be determined by analyzing |||||||Ij||samples in duplicate, andby preparing and analyzing MS/MSD sample pairs. The. RPD of the duplicate g^ganalyses willbe the measure of precision. RPD is calculated from the expression:

RPD = 2 (x, - 100 (4-2)

where:

000086

Table 4-1. Scheduled QC and calibration for the VOC analyses by GC/FID

SectionNumber in

Method 8000A7.4.2

7.4.2, 7.5

8.3

8.11

8.3

8.10

8.1

Procedure5-point ICAL

Continuingcalibration

•Matrix spike/spikeduplicateSample duplicate

Reagent blank

SurrogaterecoveriesProficiency test

FrequencyInitially and asneededDaily

See text

See text

Before anysample

Each sample

Each newanalyst

Acceptance Criteria%RSD for all targetanalytes <20%RF for all target analyteswithin 15% of ICALRT <0.08min of ICALfor all target analytesQAOa

QAOa .

No significantinterference to targetanalytesTable 8/8240A

Table 6/8240A

Corrective ActionRecalibrate

Correct before analysis; otherwise repeatICAL

Flag data and repeat analysis ||;Mrequired to meet test program objectiveFlag data and repeat analysis if requiredto meet test program objectiveFind and remove interference

Flag data and repeat analysis ||e£-required to meet test program objectiveRedo before samples are analyzed

aSee Table 2-1. o «• .'' 5- §

1croJ3I—*VO

000087

Table 4-2. Scheduled QC and calibration for the SVOC analyses by GC/MS

SectionNumber in

Method 8270A7.3.17.3.1

7.3.37.3.47.3.47.4

8.1, 8.6

8.9

8.2, 8.6

8.5

ProcedureDFTPP tuneInertness forDDT5-point ICAL

Continuingcalibration

Matrix spike/spike duplicateSamplereplicateSurrogaterecoveryReagent blank

Proficiency test

Frequency12 hours12 hours

Initially andas needed

12 hours

See text

See text

EachsampleBefore anysampleEach newanalyst

Acceptance CriteriaTable 3/8270ADDE.DDD <20%ofDDT

%RSD of CCCs <30%RRTs within 0.06RF for all SPCCS £0.05RF for all SPCCs £0.05RF for all CCCs within 30% ofICALRT of IS within 30 s of last CCALArea of IS within factor of 2 of lastCCALQAOa

QAOa

Table 8/8270A

No significant interference to targetanalytesTable 6/8270A

Corrective ActionRerun before sample analysisCorrect before sample analysis

Recalibrate

Correct before analysis; otherwiserepeat ICAL

Flag data and repeat analysis ffefrequired to meet test program objectiveFlag data and repeat analysis ||efrequired to meet test program objectiveFlag data and repeat analysis |fefrequired to meet test program objectiveFind and remove interference

Redo before samples are analyzed

C/5hri M

I II° » S'§

IaSee Table 2-1.

000088

Table 4-3. Scheduled QC and calibration for the trace metals analyses by ICP

SectionNumber in

Method 6010A Procedure Frequency Acceptance Criteria Corrective Action7.3

5.2.2.37.4

7.5

8.6.2.1

8.6.2

8.6.3

8.5.2, 8.6.4.2

Section 4 ofQAPP

Calibration

Mid-point calibration checkHigh calibration standardanalysisFlush system with calibrationblank for at least 1 minuteCalibration verification (checkstandard)Calibration verification(calibration blank)

Interelement and backgroundcorrection

Matrix spike/spike duplicate

Sample replicate

Method blank

Each working day

Each calibrationPrior to sample analysis

Prior to analysis of eachsampleAfter every 10 samples andthe end of the analytical runAfter every 10 samples andthe end of the analytical run

At the beginning and end ofan analytical run or twiceduring an 8-hour work shiftSee text

See text

See text

Manufacturer's recommendedprocedure±10% of calibration±5% of actual value

None

Agree within 10% of expectedvalueAgree within 3 standarddeviations

Within ±20% of true valueobtained in 8.6.2 (recalibrationverification)QAOa

QAOa

See text

Manufacturer'srecommended procedureRecalibrateFollow manufacturer'srecommendationsNone

Terminate analysis; correctproblems and recalibrateRerun twice; average of theresults must be within 3standard deviations of themean blank value

Flag data and repeat analysisif required to meet testprogram objectiveFlag data and repeat analysisif required to meet testprogram objectiveSee text

0>cr(tln

•See Table 2-1.

000089


*l = Sample or MS sample analysis resultx9 = Duplicate sample or MSD sample analysis resultCompleteness will be defined as the ratio of the number of accuracy and precision checks

that meet respective QAOs to the total number of accuracy and precision checks performed.Percent completeness (%C) will be separately determined for the accuracy and precision of eachmeasurement as:

%C = — • 100T (4-3)

where:V = Number of accuracy or precision measurements that meet the accuracy or precision

QAOT = Total number of accuracy or precision measurements madeMethod MDL will be statistically determined as specified in method procedures and will be

reported and compared to respective MDL objectives.

000090

SECTION 5REFERENCES

Section 5Revision 0Date: July 29, 1994Page 1 of 1

1. "Methods for Chemical Analysis of Water and Wastes," EPA-600/4-84-017, March 1984.2. "Test Method for Evaluating Solid Waste: Physical/Chemical Methods," EPA SW-846,3rd

edition, Revision 1, July 1992.3. 40 CRF Part 266, Appendix IX.

000091

Appendix ARevision 0Date: July 29, 1994Page 1 of 17

APPENDIX AMETHOD 8015 VALIDATION FOR THE TEST PROGRAM VOC TARGET ANALYTES

Included in this appendix are copies of several' communications containing data to confirmthat the VOC target analytes for this planned test program can be quantitated at the IRF viaGC/FID in accordance with Method 80 ISA. These communications, arranged by topic, are asfollows:

• MDL Study— Memorandum, D. Tabor to B. Tolleson, dated July 15, 1992. This memorandum

briefly describes the IRF equipment and procedure for performing Method 8015A,and documents the results of an MDL study performed for the VOC analytes forwhich the method is used.

• RCRA Audits 529 and 530— Memorandum, M. K. Richards to A. Kern, dated November 2, 1992, with

attachments. This memorandum with attachments documents the acceptableperformance of the IRF laboratory in quantitating toluene and benzene in VOSTaudit cylinders using Method 8015A, GC/FTD.

• WP029— Letter, D. Tabor to G. Simes, dated October 23,1992, forwarding the IRF analytical

results for Water Pollution Performance Evaluation Study 29 (WP029) to EPA— Memorandum, P. Britton to distribution, dated December 30, 1992, with

attachments. This memorandum with attachments documents the acceptableperformance of the IRF laboratory in quantitating benzene, ethylbenzene, and

000092

Appendix ARevision 0Date: July 29, 1994Page 2 of 17

toluene in the water samples comprising Study WP029. Method 80 ISA was used

for the analyses.

000093

Date:From:To:Subject:

IMEMORANDUM

July 15, 1992Dennis TaborBlake TollesonMethod Detection Limits for Volatile Organic Analysis

The Method Detection Limit study report for volatile organics has been revised to include theextrcted solids detection limits. I have attached a copy "Of the report for your files.

cc:CGJLLW

000094

GC/FID Volatile OrganicsMethod Detection Limit StudyMay 1992 Revised July 1992

RESULTSThe Incineration Research Facility Laboratory(IRF) has determined the method detection limit(MDL) for volatile organics in aqueous solutions. They are tabulated in Table One. Theextracted solid sample MDLs are included because the methanol extract is diluted into anaqueous solution.

Table One: Method Detection Limits for Volatile OrganicsName

injectedChloroform1,1,1-TrichloroethaneCarbon TetrachlorideBenzeneTrichloroethene1,2-DichloropropaneBromodichloromethanecis-1,3-DichIoropropeneToluenetrans-1,3-Dichloropropene1,1,2-TrichIoroethane

mg/kg Name

0.170.090.250.010.060.030.180.050.010.020.07

341850

2.012

6.03610

2.04.014

8.54.513

0.503.01.59.02.5

0.501.03.5

injectedTetrachloroetheneChlorobenzeneEthylbenzenem,p-Xyleneo-XyleneBromoformTetrachloroethane1.3-Dichlorobenzene1.4-Dichlorobenzene1,2-Dichlorobenzene

fj.g/L mg/kg

0.050.010.010.010.010.170.100.020.020.02

102.02.02.02.03420

4.04.04.0

2.50.500.500.500.508.55.01.01.01.0

THEORY JThe EPA has specified that the MDL for a single response analyte is the detected level that hasa 99% confidence of not being zero. The confidence interval is calculated by multiplying theStandard Deviation(SD) by the Student's t for a 1-a equal to 0.99. The use of seven replicatesbrings the Student's t to 3.143. Therefore, for seven replicates, 3.143 times the SD is the 99%confidence interval. When this confidence interval is placed on zero, the value at the upperextreme of the interval is the MDL. This is so because only values outside the interval have a99% confidence of being not equal to zero.INSTRUMENTATIONThe IRF has a Hewlett Packard 5880 chromatographic system which uses dual FIDs. The

000095

1system has two Tekmar LSC-2 purge and trap devices attached. Separate columns connect eachP&T to a FID. The LSCs are run simultaneously and each FID is monitored with a separateintegrator. Standards are made up from neat materials or commercially supplied mixes. TheIRF lab has a Barnstead Nano-Pure system for generating organic free deionized water(OFW).EXPERIMENTAL

Seven aliquots of OFW were spiked with a standard to approximately three times the expectedMDL. The aliquots were analyzed and the SD was calculated. The MDL for each FID pathwas taken as 3. 148 times the SD. The MDL was then selected as the higher of the MDLs fromthe paths.ACTIONSince the MDLs have now been established we will change our reporting of results. We willnow have three categories. The first will be samples that have no response or a response belowthe MDL. These results will be reported as NOT DETECTED. The second group will beresults that are between the MDL and the lowest level of the calibration curve. These resultswill be flagged with a J as estimated because the values are an extrapolation from the calibrationcurve. The third set will be samples with results in the calibrated range. These will be reportedwith no concentration flag. The samples that are above the calibration range will be diluted andrerun, or flagged with an E (for Exceeded Range) if the sample was not rerun.

000096

UNITED STATES ENVIRONMENTAL PROTECTION AGENCYOFFICE OF RESEARCH AND DEVELOPMENT

RISK REDUCTION ENGINEERING LABORATORYCINCINNATI. OHIO 452.68

DATE: November 2, 1992SUBJECT: Audit Gases - Acurex Audit Participation and ResultsTO: Ann KernActing Quality Assurance OfficerRisk Reduction Engineering Laboratory

V-FROM: Marta K.ResearchThermal Destruction Branch, WMDDRD

The Acurex Laboratory at the Incineration Research Facility (IRF) atJefferson, Arkansas, requested that a Vost Audit be conducted at the IRF. Icontacted Robert L. Lampe of the Quality Assurance Support Branch of AREAL inResearch Triangle Park. He arranged shipment of the Audit Cylinders andreporting procedures for the Audit.

Two Audit-Gas cylinders were shipped to the Arkansas Laboratory. A poorreport resulted from a supplier mix-up with the cylinder numbering. Theproblem has been corrected, and copies of the final results reports of theAcurex performance are attached for your information.

Acurex analyzed four compounds (carbon tetrachloride, chloroform,tetrachloroethene ("perchloroethylene"), and benzene) in Audit CylinderNo. 529. Two compounds (chlorobenzene and toluene) were the analytes in AuditCylinder No. 530.The official evaluation of Acurex performance is reported in the

attached letters of September 22, 1992, (No. 529) and October 6, 1992,(No. 530) . Historically, acceptable performance is ±50% bias for eachcompound. All of Acurex's results were calculated to be +42% bias - makingtheir performance score overall ACCEPTABLE.In the past, concern has been expressed by the RREL Quality AssuranceOffice for the IRF/Acurex raethodolgy used for VOST analyses. These auditresults are another positive point in the Acurex validation of their VOST(6C/FID) procedure. This information may be of assistance to the QualityAssurance Office in the consideration of future VOST analytical validation.

Attachmentcc: Gregory J. Carrol!Clyde R. DempseyDonald A. OberackerRobert C. ThurnauHoward 0. WallLarry Waterland, et al.

000097

IUNITED STATES ENVIRONMENTAL PROTECTION AGENCY

ATMOSPHERIC RESEARCH AND EXPOSURE ASSESSMENT LABORATORYRESEARCH TRIANGLE PARK

NORTH CAROLINA 2 7 7 1 1September 22, 1992

Ms. Marta RichardsU .S . Environmental Protection Agency26 W. Martin Luther King DriveCinc innat i , OH 45268Re: Results From RCRA Audit N o .529 Conducted By Acurex. on August 26, 1992Dear Ms. Richards:

This- let ter presents EPA's official evaluation of Acurexperformance for RCRA Audit No. 529. Performance was evaluated by comparingthe reported identity and reported concentration for each compound to thosepreviously determined by our contractor using NIST - certified standards. The^compounds in the cylinder you requested are l isted below. The audit resultsfor the concentrations that you reported are given in terms of % bias. % biaswas calculated as follows:

% Bias = [Reported Cone . - EPA Conc . lEPA Cone.Concentration fppb)

X 100

Group 1Audit No. Compound

Carbon tetrachlorideChloroformPerch!oroethyleneVinyl chlorideBenzene

Reported(ppb)40.48.5

10. 143.8

EPA(ppb)32.37 .78 .4

38.4

% Bias+25. 1+ 10 .4+20.2+14.1

Historically, the limit in the % bias for acceptable performance forRCRA audits has been ±50% for each compound. These limits were set in 1981using a very limited data set. We are reviewing the actual results for eachRCRA compound to establish a more realist ic l imit on a compound by compoundbasis.

000098

1

As part of this review we calculated the enclosed cumulative frequencydistribution for % bias for all RCRA audits completed to July 30, 1992. Weare providing this frequency distribution to you for information purposes; itshows how the audited organization's performance compares to the resultsreported for the previous audits. To assist you in using this table we havecircled the location of the auditee's % bias for each compound in the table.We have also provided a footnote to the table that illustrates how tointerpret the data in the table.

±50%At this time the acceptable performance limits for % bias remain at

r-.

If you have questions please call me at 9 19-541 -4531 .Sincere ly .

Robert L. LampeQuality Assurance Support BranchQual i ty Assurance and TechnicalSupport Division (MD-77B)

Enclosure

000099

VOC A U D l i a - I I L H A HL I IUL IUCUMULATIVE PERCENT FREQUENCY DISTRIBUTION OF XUIAS

MATERIALAco lonoAcoton i tr i loAcrylonitri loDonzcnoDromoniQ thanoCarbon TotrachloridoChlorobonzenoChloroformDichlorodifluoromothanoEthylbanzonoFrcon 113Freon 114Ha thy1 Ethyl Ketona .Methylene ChloridoOrtho-XylenaPorchloroothylonoTatrachloroathyleneTolueneTrichloroathylenoTrichlorofluoromothanoVinyl ChlorideVinylidono Chloridol > l-Dichloroathylona1»1i1-Trichloroothano1 ,2-Dib romoo thana1 i2-Dich loroo Ihano1 ,2-Dichloropropanol »4~Dioxano

N251

455

11228554151981

601

26191636

33

205811

-50X0

6007

60402

25000

2200704

• 51331

005000

• 100

-30X0

6007

6070B

25000

3300

20045

2553

00

10 '0

130

100

-20X0

600

246013

41025

000

5600

25045

3061

00

152013

0100

-10X100

600

316022183650

000

5625

035

027115069

033152013

0100

-5X100

600

406032324050

000

5638

043

027165675

033204025

0100

XBIASox1PO

600

'4760 '42 "464 975

0ZO

06738

050

035265678

033204030

0100

«5X100

600

.'JO6056615675

040

06750

10060

05437698167333C6030

01 0 0

+ 10X100

600d4

806760(SD75

060

06750

10068

05437690967334500 i'JO

1 00100

*20X100

800

7 6 )80

C79 ,757675

10060

07875

100dD10062686992

100336000DO

1 0 0100

430X100

800

028089~} '828075

10060

08975

10007

1007779

. 6992

100677500

100100106

iSQX100

800

90100

95899175

100100

08975

10093

10077956992

100678500

100100100

Uslno Th i s Tab leThis table shows the number of t imes (II) each RCRA compound has beenmeasured In the RCRA'aud i t program. It also shows the percentage of the %biases that were less than se l ec ted va lue s , e . g . , -50%, -40X , -30%, etc .For example , carbon tetrach lor ide has been measured in 1 12 aud i t s (N)with the following results:(a) 42% of the results were less than zero(b) 45% (67-22 ) of the resu l t s were between i lOX(c) 66% (79 - 13 ) of the re su l t s were between I20X

000100

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY, . ATMOSPHERIC RESEARCH AND EXPOSURE ASSESSMENT LABORATORY*" RESEARCH TRIANGLE PARK

NORTH CAROLINA 27711October 6, 1992

Ms. Marta RichardsU.S . Environmental Protection Agency26 W. Martin Luther King DriveCincinnati , OH 45268Re: Results From RCRA Audit No. 530 Conducted By Acurex On August 26, 1992Dear Ms. Richards:

There was an error in the compound concentrations supplied to us by ourcontractor on Audit No. 530. As a result the report we sent to you wasincorrect. The correct results are given below. Please accept my apology forany inconvenience this may have caused./tThis letter presents EPA's official evaluation of Acurex performance forRCRA Audit No. 530. Performance was evaluated by comparing the reportedidentity and reported concentration for each compound to those previouslydetermined by our contractor using NIST certified standards. The compounds inthe cylinder you requested are listed below. The audit results for theconcentrations that you reported are given in terms of % bias. The % bias wascalculated as follows:

% Bias = Reported Cone. - EPA Conc . lEPA Cone.Concentration fppb)

X 100

Audit N.Group IIICompound(ppb)

Vinylidene chloride1,1,2-trichloro-1,2,2-trifIuoro-•ethane (F-113)1,2-dichloro-1,1 ,2,2,-tetra-fluoroethane(F-114)Acetonel,4rDioxaneChlorobenzeneToluenePyridine*

Reported(ppb)

EPA % Bias

37. 137 .9 3 1 . 126 .7

+19.3+42.

* Concentration not certified due to.stabil ity problems.

000101

IHistorically, the limit in the % bias for acceptable performance for RCRA

audits has been ±50% for each compound. These limits were set in 1981 using avery limited data set. We are reviewing the actual results for each RCRAcompound to establ ish a more realist ic limit on a compound by compound bas is .

As part of this review we calculated the enclosed cumulative frequencydistribution for % bias for all RCRA audits completed to July 30, 1992. Weare providing this frequency distribution to you for information purposes; itshows how the audited organizat ion's performance compares to the resultsreported for the previous audits. To assist you in using this table we havecircled the location of the auditee's % bias for each compound in the table.We have also provided a footnote to the table tffat i l lustrates how tointerpret the data in the table.

At this ti-.e the acceptable performance l imits for % bias remain at±50%

If you have quest ions please call me at 919-541-4531 .Si i

Robert L. LampeQual i ty Assurance Support BranchQuality Assurance and Technical

Support Div i s ion (MD-77B)Enclosure

000102

VOC AUDITS-RCRA RESULTSCUMULATIVE PERCENT FREQUENCY DISTRIBUTION OF XBIAS

IATERIAL•catena.cetonitrilo.crylonitrilo;onzcnairomomothanalarbon Totrachlorida .:hlorobonzeno:hloroformlichlorodifluoromo thane•thylbenzena!roon 113•'reonla thy 1 Ethyl Ketonalathylene ChloridaJrtho-Xylena•archloroothylena"otrachloroothylono"olucno"riohloroothylono"richlorof luoromo thano'inyl Chloride'inylideno Chlorido. >l-Dichloroothylona. > 1 > 1-Trichloroo thane, ,2-Dibromoothana»2-Dichloroothana»2-Dichloropropana>4-Dioxana

-SO'/. -30X -20X -10X -5XXBIASox +5X nox + 20X- + 30X +50X

251

455

1122855

4151981

601

26191636

33

205811

060

07

60402

25000

2200704

. 513310

05000

- • 100

060

07

60705

25000

3300

20045

25530

010 '

013

0100

060

0246013

41825

000

5600

25045

3061

00

152013

0100

10060

0316022183650

000

5625

035

027115069

033152013

0100

10060

0406032324050

000

5638

043

02716567G

033204025

0100

10060

0476042464 975

020

06738

050

035265670

033204030

0100

10060

05860

' 56615675

040

067SO

10060

0543769016 733356030

0100

10060

0648067686475

060

06750

10068

054376 9096733458050

100100

10080

0768079

(jla)7675

10060

07875

10082

10062686992

'' 10033608050

100100

10080

0828089828075

10060

08975

10087

100(77

796 992

100677580

100100100

10080

098

10095899175

100100

08975

10093

10077)956992

100678580

100100100

Using This TableThis table shows the number of times (N) each RCRA compound has beenmeasured In the RCRA audit program. It also shows the percentage of the %biases that were less than selected va lues , e . g . , -50%, -40%, -30%, etc .For example, carbon tetrachlorlde has been measured in 112 audi ts (M)with the following results:(a) 42% of the results were loss tlinn /ero(b) 45% (67-22) of the results were between ilO'X(c) 66% (79- 13 ) of the results were between i20X

000103

1AcurexEnvironmental' C O R P O R A T I O N

October 23, 1992

Guy Simes, Quality Assurance OfficerRisk Reduction Engineering LaboratoryU.S. Environmental Protection Agency26 W. Martin Luther King Drive MS-223Cincinnati, Ohio 45268

Dear Mr. Simes:Per the instructions of Mr. Robert Thurnau of the U.S. EPA Risk Reduction Engineering

Laboratory, the Incineration Research Facility analytical laboratory has completed the analyses forPerformance Evaluation WP029. The analytical results are enclosed for your review.

WP029 instructions specified that the code "99" be used for all "other" analyses methods and thatthe methods be identified. The code "99" is applicable to all the reported results. PCBs and pesticideswere analyzed by Method 8080 (SW-846). Volatile halocarbons and aromatics were analyzed by purgeand trap GC/FID. The Chloride analyses were done by Method 300 using a Dionex Ion Chromatograph.

The instructions for WP029 also directed us to request the sample true values if we intend to usethe leftover samples as check samples in the future. We do want to be able to use the leftover samplesin this way. Thus, please furnish a copy of the true values to us at your convenience. Thank-you foryour assistance.

Sincerely,

Dennis G. TaborLab Supervisor

enclosurecc: Robert Thurnau - EPA RREL

Larry Waterland - Acurex EnvironmentalJohannes Lee - Acurex EnvironmentalCarla Goldman - Acurex Environmental

Incineration Research Facility, NCTR-Building 45, Jefferson, AR 72079(501)541-0004 FAX: (501)536-6446

Division HQ: 555 Clyde Avenue, P.O. Box 7044, Mountain View. CA 94039 (415)961-5700 FAX: (415)964-6523/5145/V

000104

UNITED STATES ENVIRONMENTAL, PROTECTION AGENCYOFFICE Of RESEARCH AND DEVELOPMENT

ENVIRONMENTAL. MONITORING SYSTEMS LABORATORY45268

DATE: December 30, 1992SUBJECT: Results from Water Pollution PerformanceEvaluation Study 29 (WP029) r\3 (FROM: Paul W. Britton, Statisticlan'sA^J L- !Development and Evaluation Branth •Quality Assurance Research Division v

«•.TO: Quality Assurance Coordinators/OfficersProject OfficersInterested LaboratoriesTHRU: Robert L. Graves, ChiefDevelopment and Evaluation ffranchQuality Assurance Research Division

*

WP029 has been completed by EKSL-Cincinnati in its continuing evaluationof the performance of USEPA, state and other selected laboratories for 80water pollution analytes.The results of WP029 are provided to the addressees as individuallaboratory reports with an explanation of the performance terras and relevantstudy summaries. Each Regional Coordinator 1s also provided with a blankevaluation report which shows every true value and performance evaluationlimit in the study. A list of the laboratory codes assigned within eachregion is sent to the Coordinator. Reports for participating ORD laboratoriesare sent to the directors. Reports for participating contract/grantlaboratories are sent to the responsible project officers. Copies of thereport for each participating regional laboratory are furnished to the QualityAssurance Coordinator/Officer and the Laboratory Director. The RegionalCoordinators and USEPA Project Officers are expected to distribute reports toparticipant laboratories and to Include other study information they considerappropriate* \Overall, 88.3 percent of all data were within acceptance limits and noneof the 148 analyte/sample combinations present had a failure rate over 21percent. One study problem of note: non-filterable residue results were tobe reported In jng/L as previous studies and as indicated on the data reportingform. However, some confusion was caused by the reporting results section ofthe non-filterable residue instruction sheet, which incorrectly indicated mg/Gunits. Whenever results wara noted to be in mg/G, they were converted to tag/Ifor evaluation. Results that were judged quantity-wise to be in mg/G werealso converted.

000105

PERFORKA?fCL' EYALUATIOW REPOHTTPOLLUTIOK sTuor Hcif.flEH vpo29

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000106

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000107

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000108

3.2 BIODEGRADATION REMEDY SELECTION ASSESSMENT

3.2.1 Introduction

Biodegradation is typically conducted due to its potential to treat large quantities of low to moderatelycontaminated sludge/sediment cost-effectively. Moderate to good success in biodegradation of PAHs byother biodegradation practitioners support the use of this technology for removal actions. Field conducteddegradation trials in general yield better results than bench scale treatability testing due to a variety offactors. These factors include optimized microbiological conditions, dilution by excavation and mixingwith clean soil, photochemical effects, and climatic conditions. In addition, larger scale reactors ascompared to bench scale are more resistent to upset conditions. A feasibility assessment conducted inthe field enables a more realistic estimate of full scale costs. The biodegradation work plan was preparedby the Ecology & Environment Technical Assistance Team (TAT), and with review and commentsprovided by Edward Opatken (U.S. EPA Office of Research and Development START Leader) and JohnGlaser (U.S. EPA - Risk Reduction Engineering Laboratory).

3.2.1.1 Biodegradation Remedy Selection Assessment Goals

Biodegradation is being considered as a removal action option for the reasons stated in the previoussection. The agencies policy of preference for treatment (i.e., for technologies that will permanently andsignificantly reduce toxicity, mobility, or volume of hazardous substances as their principal element)requires evaluation based upon the following subfactors for a particular alternative:

1. The treatment process(es) employed and the materials) it will treat.

2. The amount of the hazardous materials to be destroyed or treated.

3. The degree of reduction expected in toxicity, degradation into less complex compoundsand volume reduction.

4. The degree to which the treatment will be irreversible.

5. The type and quantity of residuals that will remain after treatment.

000109

6. Whether the alternative will satisfy the preference of treatment.

More specifically, the objectives of the EE/CA biodegradation remedy selection feasibility assessment areto:

1. Significantly and permanently reduce the volume, toxicity, and mobility of hazardouscompounds present in the remedy selection treatment units.

2. Evaluate the ability of ex-situ (landfarm) arTd in-situ slurry biodegradation to degradearomatic and polycyclic aromatic hydrocarbons present, in a petroleum hydrocarbonmatrix in the contaminated lagoons at the SSC site under field conditions.

3. Collect kinetic data on which to base conclusion of biodegradation efficiency includingrate of biodegradation and final contaminant concentrations.

4. Evaluate the capability of biodegradation technologies and use the data generated toevaluate this technology for site removal actions.

5. Refine the technology necessary for implementation of biodegradation of contaminatedsludge at the site.

6. Identify potential problems in implementing a biodegradation project and estimatedproject duration.

3.2.1.2 Rational for Remedy Selection Ex-Situ Sediment Biodegradation

Ex-situ biodegradation is typically conducted due to its potential to convert large quantities of low tomoderately contaminated sludge/sediment into innoxius products cost-effectively. It is typically the mosteconomical ex-situ technology. As previously mentioned, field conducted degradation results in generalyield better results than treatability testing due to a variety of factors. These factors include optimizedmicrobiological conditions, dilution by excavation and mixing with clean soil, photochemical effects, andclimatic conditions.

000110

3.2.1.3 Ex-Situ Sludge (Landfarm) Biodegradation

One limiting factor for landfarm biotreatment is the availability of the contaminants to the bacteria. Thisis due to a combination of factors which include proximity of bacteria to contaminants, soil aggregatesize, adsorption and absorption of contaminants to the soil, and the solubility of the contaminants. Thebiodegradation remedy selection assessment is designed to optimally control each of these effects in amanner which is both economical and practical.

Sludge and sediment excavated for the treatability assessment 'will be placed in the Land Treatment Unit(LTU), any material which would interfere with tilling will be removed. Contaminated sand may beadded during excavation of the sample to assist in material handling. Soil amendments will be addedduring the tilling/mixing operation. Amendments may include nitrogen and/or other cofactors and pHadjustments (lime) if needed. The soil in the LTU will probably contain indigenous hydrocarbondegrading bacteria and will be stimulated by the addition of nutrients. A surfactant may be added toincrease the liquid-solid interface by solubilizing the contaminants, making them more available to thebacteria. Moisture content will be monitored to optimize this parameter.

3.2.1.4 Rational for In-Situ Slurry Biodegradation

Soil slurry biodegradation is being conducted at the bench, pilot and full scale by many practioners, dueto its enhanced capability to degrade recalcitrant organic compounds (over ex-situ treatment). Biologicalreactions can proceed at an accelerated rate in a slurry system because limiting nutrients can be supplied,oxygen can be maintained and contact between contaminates and microorganisms can be increased byeffective mixing and maintenance of relatively high bacterial populations. This technology is appropriatefor soils having a low sand content and small particle size composition. Results from other practitionersof slurry biodegradation indicate that this method of biotreatment is appropriate for PAHs.

3.2.1.5 In-Situ Slurry Biodegradation

In-situ biodegradation is generally seen as a cost-effective means of contaminant reduction without theexpense of material handling associated with excavation and treatment of ex-situ soil. From a technicalpoint of view, this approach represents a situation with less degree of process control or ability to

000111

manipulate the conditions to achieve removal goals. Most in-situ biodegradation projects are conductedto lower costs, to avoid excavation, thereby imposing Land Disposal Restrictions (LDRs), or because theremoval goal is obtainable under less than optimum conditions. Simulated in-situ biodegradation remedyselection assessment will be undertaken on the site assess in the removal of lagoon sludge by reducingthe toxicity, mobility and volume of contaminant through microbial treatment.

000112

3.2.2 DESIGN CONSIDERATION: MOISTURE CONTROL

Moisture control in a landfarm style biodegradation project is of paramount importance, particularly withthe soil matrices which were addressed earlier. Microbial activity in soil is directly related to soilmoisture content. Too little or too much water inhibits microbial activity and therefore degradation.Proper leachate control also prevents contamination from migrating out of the treatment area. Thissystem is designed for the maximum amount of water control and flexibility of water usage.

The LTU has been designed to accommodate the flow of water from a two year, 24 hour maximumrainfall event. This is equivalent to six inches of water. The'leachate drainage, collection and dischargesystem has been designed to maximize return to optimum soil moisture content as soon as possible aftera rainfall event. This is achieved by construction of the system addressed in Section 3.2.3. A sourceof water will be provided by restoration of on-site utilities.

Water collected in the leachate trench will flow via a PVC pipe to a sludge lagoon with ample capacityto contain it. The LTU sump is designed to contain rainfall in excess of that which is immediatelyabsorbed into the soil. The water will flow over the soil retaining berm and into the sump which mayserve as water storage for use in landfarm operations. An overflow pipe will lead to the lagoon whichserves as water storage for use in landfarm operations.

000113

3.2.3 CONSTRUCTION OF THE LAND TREATMENT UNITAND ASSEMBLY OF THE SIMULATED IN-SITU TREATMENT UNIT

Figure 3.2-1 illustrates the design and construction of the biodegradation LTU. EPA proposed UniversalTreatment Standards (UTS) has defined the magnitude of remedy selection as > 1 kilograms and <1000kilograms. The Federal Register, February 18, 1994 increase the treatability studies sample exclusionfrom 1,000 kg to 10,000 of non-acute hazardous waste. In order to simulate full-scale treatment aminimum of five cubic yards of sludge/sediment is recommended. The LTU will have interiordimensions of 9 x 15 feet. This assumes a generally accepted optimum sediment depth of nine to twelveinches. Nine inches is the approximate maximum tilling depth using conventional apparatus. Sedimentexceeding this depth becomes increasingly difficult to oxygenate, hence delaying the biodegradationprocess. The proposed depth also facilitates water retention, which aids in maintaining the propermoisture content.

The delineated LTU area will be graded to facilitate gravitational drainage toward the leachate collectionsystem. Berms may be constructed high enough to exclude potential of a 100-year flood event. Materialrequired to construct the berms will be obtained from suitable on or off-site locations.

A 30 mil LDPE liner will be installed over indigenous soil, including the leachate collection trench andthe leachate sump. The liner edges will be anchored into the perimeter berm to make the LTU leakproof.A perforated PVC pipe will be installed in the lined trench.

Sixteen inches of sand will be placed on the liner. This layer will serve to create a buffer and drainingzone between the liner and the contaminated sediment. Although the tilling implement should notpenetrate to this layer, it will provide a comfortable safety margin. Construction equipment such as abackhoe will be used to place the sand over the LDPE.

The leachate collection system is designed to accommodate severe precipitation conditions expected atthe site, as previously addressed. Some precipitation will dram through the sand layer, and into theleachate collection trench and then to a lagoon. Precipitation in excess of the percolation rate will runoff of the contaminated soil into the LTU sump without significant contact with the soil. The sump isdesigned to serve as holding capacity for severe rainfall, which will prevent all of the precipitation fromhaving to percolate through the contaminated soil. This sump water can be used for the preparation of

000114

1bacterial cultures and possible irrigation as well. Water in excess of the holding capacity of the sumpwill flow out of the sump and through a PVC conduit to an existing lagoon with sufficient capacity toavoid discharge.

Figure 3.2-2 illustrates the simulated in-situ slurry treatment design. A cylindrical 2000 gallonpolyethylene tank will be used to simulate the south impoundment. Mixing of contaminated matrices(LNPL, water, DNPL) will be achieved by use of an aspirating mixer. This equipment will introduceair (oxygen) into the slurry as well as facilitate mixing of bacterial amendments added to stimulatemicrobial growth and chemical degradation. An air compressor will be used to provide additional oxygenrequired by the microbial population.

This equipment will be staged in a location between the north and south impoundments and will beoperated using a generator for electrical power.

000115

I .

PLAN VIEW

COMTMJMAIED SOIL

1C COMBE sum——— IX SLOPE

SECTION

12" COHTMWU1QI SON.

SECTION

m

ecology and environment, inc.SOUTHERN SHIPBUILDING CORPORATON

«Ti-9307-015«*ELA0240FAAI

BIODEGRAnATlON REMEDY SELECTIONAND LAND TREATMENT UNIT

SUDELL. LOUISIANA

FIGURE000116

1

ASPIRATING AERATOR

POLYETHYLENETANK

4ecology andenvironment, inc.Dallas, TexasSptdrifati in the Entrapment

SOUTHERN SHIPBUILDING CORPORATIONSLIDELL, LOUISIANA_______TOfT06-9507-015|»|ELAO24OSAA

BIODEGRADATION REMEDYSELECTION SIMULATEDIN-SITU TREATMENT

FIGURE 32-2

000117

3.2.4 HEALTH AND SAFETY3.2.4.1 Site Safety Plan

The SSC Site Safety Plan has been amended to address the scope of work to be performed during thebiodegradation remedy selection assessment.

3.2.4.2 Air Monitoring

Air sampling with summa canisters has been conducted while the impoundments were being agitated witha track-hoe. This has provided an estimate of volatile emissions anticipated during excavation of thesludge. An air monitoring program will be conducted prior to, and concurrently with, sludge excavationand treatment unit loading. This program is designed to achieve the following air data quality objectives(DQOs):

1. To provide real-time ambient air quality data for accurateemission rate estimates under undisturbed conditions.

2. To provide real-time air quality data suitable forassessing whether concentrations exceed on-site and off-site health criteria levels.

3. To provide air contaminant data suitable for generatingaccurate emission rate estimates during biodegradationactivities.

Air monitoring will be conducted with a total vapor analyzer (TVA) and/or an organic vapor analyzer.Standard operating procedures for air monitoring are included in the Quality Assurance Sampling Plan.

000118

3.2.5 SLUDGE/SEDIMENT EXCAVATION OPERATIONS

The LTU is designed to accommodate approximately five cubic yards of soil. Excavation will proceedin an area of each lagoon visually identified by the EPA-OSC.

E & E will monitor the excavation, using survey and air monitoring and sampling equipment, andsludge/sediment soil deposition into the slurry tank and LTU respectively.

The sludge/sediment excavated from the north lagoon will be placed in a lined dump truck, transportedto, and dumped into the LTU. Upon completion of the excavation and LTU loading, the sediment willbe graded to the uniform recommended depth.

Tilling of the sludge/sediment will be required for homogenization, distribution of nutrient and bacterialamendments and oxygenation of the material. This operation is very important for the achievement ofbiodegradation objectives. Oxygen, which is used as a terminal electron acceptor during contaminantdegradation, is a biologically limiting factor. The ability to perform this task is also a function of themoisture content of the soil. Since newly excavated sediment will be approximately saturated, there islittle likelihood of tilling the soil during the initial nutrient and bacterial applications. The sediment willdrain by gravity, and eventually will become workable. A garden tiller is recommended for the tillingoperation.

The sediment should be tilled all week, beginning as soon as possible. After initial homogenization, thetilling will take place as necessary to achieve optimal degradation. The tiller should remain on-site tofacilitate its access and use, and to reduce the amount of decontamination.

Sludge excavated from the south lagoon will be similarly transported to the slurry tank. Contaminatedwater will be added to the treatment tank then sludge will be added to a ratio as close as possible to 15-30% solids. This is in the range of aerating/mixing equipment and a range recommended for slurrybiodegradation. The sludge should be mixed and aerated continuously. Air monitoring will be conductedduring slurry biodegradation start up.

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3.2.6 BIODEGRADATION OPERATIONS

3.2.6.1 INITIAL MICROBIOLOGICAL CHARACTERIZATION

Initial microbiological characterization is being performed concurrently with site assessment activities andconcurrently with mobilization for remedy selection ex-situ landfarm and simulated in-situ biodegradation.If it is determined that a significant level of microbiological activity is present in the sludge/sediment (asexpected) mobilization will continue and the remedy selection assessment will proceed. If a low levelof microbiological activity is seen, then provisions will be made to enhance that microbial activity bynutrient addition and allow five days for acclimation or to determine the cause(s) of the low level ofactivity.

3.2.6.2 Ex-Situ Landfarm Nutrient and Bacterial Application

After initial placement of the sediment into the LTU, and tilling to homogenize the soil, initial samplingwill begin. Application of nutrient and bacterial preparations may then begin.

The applications will be divided into phases: initial applications subsequent to LTU loading forapproximately one week, and approximately four applications per month as weather conditions permit.

3.2.6.2.1 Nutrient Application

Nutrients will be applied initially based upon initial characterization results. A blend of nutrients will beapplied to provide sufficient amounts of these macronutrients, as well as micronutrient, to facilitatemicrobial degradation initially and on an as needed basis. The desired cinip ratio is 100:52:2 ammoniumchloride and disodium phosphate will be used as nutrient amendments.

Samples will be taken for nutrient concentrations and bacterial population analysis. The method ofnutrient application will be dictated by the moisture content of the sediment. If the moisture content isdeficient or within the optimal range for maximum degradation to occur (50 to 70 percent of fieldcapacity), the nutrients will be prepared by dissolution in water, and applied via a small pump, gardenhose, and a garden sprinkler.

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3.2.6.2.2 Bacterial Application

A bacterial culturing bioreactor will be assembled to enhance the population of indigenous bacteria. Thiswill consist of a polyethylene drum and an air compressor to provide aeration to developing cultures.The bacteria will be reared using a carbon source provided by site sediments and a nutrient solution toserve as metabolic cofactors. The bacteria will be applied to the soil using a small pump. The LTU wasdesigned to facilitate the maintenance of the desired water content in the soil. Commercially availablebacteria, cultured for their hydrocarbon degrading ability, may be added during the second half of theassessment to expedite TPH degradation. Field modifications to this methodology may be afterconsultation and approval from the OSC.

3.2.6.3 Biological Monitoring

Table 3.2-2 lists the microbiological, nutrient and analytical testing program for the ex-situ landfarmbiodegradation assessment. Table 3.2-3 lists the tests for in-situ slurry biodegradation operations.Standard operating procedures (SOPs) will be used for all of the testing conducted. Testing for nutrientsand moisture content will be conducted initially on a daily basis. Nutrient and moisture testing will occurthereafter on a weekly basis at a minimum. This monitoring assures that concentrations of nitrogen andother cofactors necessary for the degradation of the contaminants are sufficient. The testing will beconducted on-site to provide real-time feedback, and the results will be used to supplement thoseparameters found to be deficient.

Bacterial enumeration (CPUs) on the landfarm soil will be taken initially and on a weekly basis. Bacterialpopulation levels in the slurry reactor will be monitored using oxygen utilization rates. This monitoringof the biological health of the slurry is crucial to objectives of the assessment. Identification of bacterialstrains will occur for both treatments initially and at the conclusion of the assessment. Microbiologicaland analytical testing will be performed at E & E's analytical services center (ASC).

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TestParameters/TestingSchedule

SUMI

BacterialIsolationand I.D.a

BIODEGRAMARY OF MICF

(5(

Total ColonyFormingUnits"(TCFUs)

DATION REIOBIOLOGIC:ubic Yard EJ

NutrientsbN, P, pH

Table 3.2-1MEDY SELE:AL, NUTRI1(-Situ Landfamm~mmmm~————SSS

ToxicityLeachingProcedure(TCLP)

CTION ASSESSMEIENT AND ANALYTrm Treatment)

TotalPetroleumHydrocarbons0(EPA Method418.1)

S(T[C TESTING

VolatileAromaticCompounds(EPA Method8020)

' ' M i ' ' ' " •"""-=' " "J

Semi-VolatileCompounds(EPA Method8270)

Initial Testing1 3 3 3 3 3 3

InterimTesting

--

33

33

--

33

33

33

Final Testing

Total Tests12

312

312

36

312

312

312

"-Composite samplesb-0n-site testing - as performed as necessaryc-Grab samples

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Table 3.2-2BIODEGRADATION REMEDY SELECTION ASSESSMENT

SUMMARY OF MICROBIOLOGICAL, NUTRIENT AND ANALYTIC TESTING(Simulated In-Situ Slurry Treatment)

TestParameters/TestingSchedule

BacterialIsolationand I.D.a

Total ColonyFormingUnits"(TCFUs)

Nutrients6N, P, pH

ToxicityLeachingProcedure(TCLP)

TotalPetroleumHydrocarbons'(EPA Method418.1)

VolatileAromaticCompounds(EPA Method8020)

Semi-VolatileCompounds(EPA Method8270)

*Initial Testing1 3 3 3 3 3 3

InterimTesting

--

33

33

--

33

33

33

Final Testing

Total Tests12

312

312

36

312

312

312

"-Composite samplesb-On-site testing - as performed as necessaryc-Grab samples

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3.2.7 SAMPLING AND ANALYSIS

There are two principle objectives for the sampling and analysis of the sludge and sediment being treatedin the treatment units: monitoring the biological parameters to optimize biological degradation of thetargeted compounds, and monitoring the degradation of chemical contaminants.

3.2.7.1 Ex-Situ Sediment Sampling

A sampling grid will be superimposed over the LTU to facilitate representativeness, to increase samplinglocation reproducibility, and to enable the reporting results In an organized manner. Sampling will beconducted on the grid nodes (or grid intersections). This facilities description of sample locations andrepeatability. The LTU will be divided into 15 grids. This produces 8 internal potential sampling nodes.The 8 locations will be sampled in varying combinations depending on the objective of the sampling task.

SOPs to be used for soil sampling are included in the QASP. In an effort to control the cost of analyticaltesting, composite samples will be used whenever possible. Samples to be analyzed for volatile organiccompounds will be collected in VOA bottles.

3.2.7.2 Contaminant Biodegradation Monitoring

3.2.7.2.1 Sludge Characterization After Placement Into Treatment Areas

In addition to the initial nutrient and microbiological characterization previously addressed, the sludgewill be sampled and analyzed for chemical contaminant concentrations. These samples will be takenimmediately after the soil has been leveled to the specified depth. Total Petroleum Hydrocarbon (TPH),volatile and semi-volatile analysis will occur initially to obtain average contaminant loading and to serviceas a baseline from which to track results of the biological treatment. A sample from the sedimenttreatment will also be tested using the Toxicity Characteristic Leaching Procedures (TCLP) to ascertainthe contaminant potential for mobility. As shown in Table 3.2-2, three composite samples, eachcomposed of grab samples from three different grid nodes, will be collected and analyzed for TPH.

Three samples will be collected for analysis of volatile compounds. These samples will be taken fromrandomly selected grid nodes. Random locations will be chosen using a random number generating table

000124

or a random number generating calculator. Similarly, three samples will be collected for semivolatileanalysis.

3.2.7.2.2 Interim Monitoring

Monitoring for microbiological parameters will occur on a daily, weekly or monthly schedule dependingon which parameter is being monitored. TPH, volatile aromatic and semivolatile compoundconcentrations will be monitored during the tilling, nutrient and bacterial application phase. Samples willbe collected as described when work begins, and weekly thereafter, to ascertain contaminantconcentrations and that chemical degradation that has occurred. Analysis of the sludge for volatilearomatics (or any analyte) may be discontinued if it is shown that there are non-detectable concentrationsin the previous tests.

3.2.7.2.3 Final Sampling

When the treatment period has been completed, there will be a final round of sampling and analysis.Three samples will be collected, analyzed for volatile and semivolatile compounds, and compared to theremoval criteria. Three composite samples will also be collected for TPH analysis. A TCLP test toascertain if there has been a reduction in mobility and/or toxicity in contaminants only if the initial TCLPtest failed.

3.2.7.3 Sample Analysis

The methods used for sludge analysis are summarized in Table 3.2-3. Moisture content will bedetermined using a moisture meter while in the field, and by a gravimetric method as part of theanalytical testing protocol. Samples collected nutrient analyses will be tested on-site using a soil nutrienttest kit from SOILTEST, INC. Bacterial enumeration will be performed using an adaption for soil ofthe standard plate count from the Standard Methods for the Examination of Water and Wastewater.Bacteria will be identified using a system from BIOLOG, INC.

Chemical analyses will be conducted by EPA SW-846 Methods. Method 8020 will be used to analyzesamples for volatile organic compounds. Method 8270 will be used for analyses of semivolatilecompounds. TPH analysis provides a degradation tracking mechanism, is useful in the feasibility

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TABLE 3.2-3

SUMMARY BIODEGRADATION OF TEST METHODS

ANALYTE

Moisture contentAmmonia nitrogen

Orthophosphate

Heterotrophic bacterial populations (CPUs)

Bacterial Identification (Typing)

Total recoverable petroleum hydrocarbons

Volatile aromatic compounds (BTEX)

Base neutral/acid extractable compounds

Volatiles, semivolatiles, metals

TEST METHOD

Moisture meter calibrated 1-10

SOILTEST combination soil testSOILTEST combination soil testr-.

kit

kit

Standard Methods for the Examination ofWater and Wastewater. Method 907 (modifiedfor soii)(15th Edition, 1980)

Biolog, Inc. Manual Bacterial IdentificationSystem

SW-846 418-1

SW-846-8020

SW-846 8270Toxicity Characteristic Leachate Procedures

000126

assessment, and is good indicator of total or gross contamination. Therefore, TPH will be measured bythe relatively inexpensive Method 418.1 . These tests will allow documentation of degradative results.

3.2.7.4 Quality Assurance/Quality Control

Quality Assurance/Quality Control (QA/QC) is incorporated into the removal biodegradation project andspecific subtasks. Use of SOPs and the data reporting format are the key to QA/QC. Field collectionof sludge/sediment samples will be conducted under the QA/QC guideline listed in the QASP. Nutrient,microbiological and target compound analysis will be conducted according to SOPs.

QA is ensured by specification in this work plan of the following: specification of number, type andlocation of samples to be collected; identification of treatment conditions; target compounds; and numberand time of each sampling. Other design components of QA/QC include the clear statement of theobjectives of the biodegradation assessment.

Laboratory chemical analysis of target compounds by the ASC will include matrix spikes, matrix spikeduplicates, and method blanks as a measure of percent recovery. Additional QA/QC procedures areincluded in the E & E Master Quality Assurance Plan (MQAP).

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3.2.8 REFERENCESAmerican Petroleum Institute. Landfarm Air Emissions. API Publication No. 4500, March,

1989.Ecology and Environment, Inc. Aerobic Biodegradation Remedy Screening Treatability Study

Report. RAB Valley Wood Preserving Prepared for EPA Emergency Response Branch - Region6. March 31, 1994.

Ecology and Environment, Inc. Quality Assurance Sampling Plan for Southern ShipbuildingCorporation, LA. Prepared for EPA Emergency Response Branch - Region 6. June 1994.

Ecology and Environment, Inc. Remedy Selection Pilot Biodegradation Report for MacmillanRing-Free Oil Company. September 30, 1993.

Ecology and Environment, Inc. Site Assessment Final Interim Report for Southern ShipbuildingCorporation, LA. Prepared for EPA Emergency Response Branch - Region 6. November, 1993.

Ecology and Environment, Inc. Site Inspection Report for Southern Shipbuilding Corporation, LA.Prepared for EPA Preremedial Branch - Region 6. February, 1994 (LAD008149015)

Matthews, J. E. Evaluation of Full-Scale In-Situ and Ex-Situ Bioremediation of Creosote Waste,U.S.E.P.A.O.R.D., Ada. Oklahoma. Bioremediation of Hazardous Wastes EPA/600/R-92/126,August, 1992.

Myers, J. M. Macmillian Ring-Free Oil Biodegradation Project. Presented at the Hazardous MaterialsControl Research Institute, Washington, DC, November 30, 1993.

Pope, D.F. and S. E. Matthews. Bioremediation Using the Land Treatment Concept. U.S.E.P.A.O.R.D., Ada, Oklahoma. EPA/600/R-93/164, August, 1993.

Sims, J. L., R. C. Sims, and J. E. Matthews. Bioremediation of Contaminated Surface Soils.U.S.E.P.A.O.R.D., Ada, Oklahoma. EPA/600/9-09/073, August, 1989.

Sims, R. C. Evaluation of Full-Scale In-Situ and Ex-Situ Bioremediation of Creosote Wastesin Soils and Groundwater. U.S.E.P.A.O.R.D. Symposium and Bioremediation of HazardousWastes. EPA/600/R-93/054, May, 1993.

Stoo, H.F. et al. Remediation Technologies, Inc. Bioremediation of Hydrocarbon ContaminatedSolids Using Liquids/Solids Contact Reactors. Presented at HMCRI Superfund Conference.December, 1989.

U.S. Environmental Protection Agency Engineering Bulletin. Slurry Biodegradation. ORD Cincinnati,Ohio. EPA/540.2-90/016, September, 1990.

U.S. Environmental Protection Agency Office of Research and Development. Bioremediation in theField. EPA/540/N-93/001, No, 8, May, 1993.

U.S. Environmental Protection Agency. Bioremediation of Hazardous Wastes. EPA/600/R-92/126,1992.

000128

U.S. Environmental Protection Agency. Guidance for Conducting Remedial Investigations andFeasibility Studies Under CERCLA: Interim Final. EPA/540/G-89/004, 1988.

U.S. Environmental Protection Agency. Guide for Conducting Treatability Studies UnderCERCLA: Final. EPA/540/R-92/071a, 1992.

U.S. Environmental Protection Agency. Guide for Conducting Treatability Studies Under CERCLA:Aerobic Biodegradation Remedy Screening: Interim Guidance. EPA/540/2-91/013A, 1991.

U.S. Environmental Protection Agency. Guide for Conducting Treatability Studies UnderCERCLA: Biodegradation Remedy Selection: Interim Guidance. EPA/540/R-93/519 a+bAugust, 1993.

U.S. Environmental Protection Agency. Obtaining a Sjoil and debris Treatability Variance forRemoval Actions. Superfund LDR Guide #6B. Superfund Publication 9347.3-06BFS,September, 1990.

U.S. Environmental Protection Agency. On-Site Engineering Report of the Slurry-Phase BiologicalReactor for Pilot-Scale Testing on Contaminated Soil. Risk Reduction Engineering Laboratory.EPA/600/SR-93/066, June, 1993.

U.S. Environmental Protection Agency. Pilot-Scale Demonstration of a Slurry-Phase BiologicalReactor for Creosote Contaminated Soil. Superfund Innovative Technology Evaluation.EPA/540/55-91/009, September, 1993.

Zappi, M. E. et al. USAE Waterways Experiment Station, MS Remediation of Petroleum FuelContaminated Soils Using an Innovative Bioslurry System. Presented at HMCRI SuperfundConference, December, 1993.

000129

3.3 SOLIDIFICATION/STABILIZATION (SS)3.3.1 IntroductionThe solidification/stabilization treatability study is being conducted to test the ability of this technologyto remedy the wastes at the Southern Shipbuilding Corporation into a substance which will be acceptablefor landfill disposal.

The primary screening criteria is the ability to have acceptable RCRA characteristics including TCLPresults for landfilling. Not having this ability will eliminate the technology from further consideration.A secondary criteria is for the treated sample to have adequate compressive stress. The adequacy is tobe determined by the intended location within a landfill. It is not expected that this secondary criteriawill in fact eliminate any technologies.

Tertiary screening criteria are cost and percentage volume of swell. The percentage volume of swellaffects transportation and landfill costs. The comparative cost of implementing a particular technologymust include the differential costs for transporting and landfilling the stabilized volume. Although aranking by this cost will be established, all these technologies will have passed primary and secondarysolidification/stabilization screening criteria. If the abatement action is bid, all technologies passingprimary and secondary screening criteria should be considered acceptable. If one technology is to bedesignated for implementation, then the most cost-effective as determined by the third screening criteriashould guide the selection.

Complete physical and chemical characterization of the wastes, including those parameters deemed to berelevant to solidification/stabilization, is currently being conducted. The parameters which are beinganalyzed for are being presented in the EE/CA work plan. SS treatability samples are being collectedconcurrently with sample collection for physical/chemical characterization. Collection methodology andhealth and safety considerations are presented in the EE/CA QASP (Appendix A).

3.3.2 Treatability Study Contractor

The solidification/stabilization treatability study will be conducted by Kiber Associates, 3786 DekalbTechnology Parkway, Atlanta, GA. under contract with the U.S.E.P.A. Risk Reduction Engineering

000130

Laboratory, Cincinnati, Ohio. Patrick Erikson through Edward Opathen is the primary contract for thisstudy. Refer to Section 4 for more information of the organization of this study.

3.3.3 Statement of Work

Following is a "Statement of Work" prepared by the RREL for the treatability contractor.

000131

SOUTHERN SHIPBUILDING CORPORATION SITETREATABILITY STUDY

Quality Assurance Project PlanREVISION 1

PREPARED FOR:

U.S. ENVIRONMENTAL PROTECTION AGENCYOffice of Research and Development

Contract No. 68-CO-0047

October, 1994

000132

QUALITY ASSURANCE PROJECT PLAN APPROVAL FORMfor

RREL Conttcls/IAQdCacparaiive Agteement^dn-haae Projects

RRELQAIDNo: A-940-B RREL Project Category: IV Revision Date:PRC Environmental Management, Inc.

QAPrtjectPIaiTifle: Southern Shipbuilding Corporation Site Treatabtltty Study

IbjpLEMENT THE ABOVE QA PRQJECTPLAN:

(ognaion) Other ai Appropriate* - Affilanon

as Appropriate* - Affiliaiion

Print Date

Pom Dateg support

provided by aaibcontracar or

APPROVAL TO PROCEED IN ACCORDANCE TO THE ABOVEQA PROJECT PLAN:

(agnannt) RREL reqxmabie person - contractually

CONCURRENCES:

(signamn}jlREL responsible pcnoo- technically

Print Date

Print Date

(dpjttorc) RBEL QA Maftagti/Cooidinator Print Date

SignamrcGoflimenc

TJUc Date

MffiL(QAPPAP)(Ape. 1993)

000133

Southern Shipbuilding Corporation SiteQuality Assurance Project PlanRevision No. 117 October 1994Pagei

TABLE OF CONTENTS

1 .0 PROJECT DESCRIPTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11 . 1 INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.2 GENERAL PROJECT OVERVIEW . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.3 PROJECT BACKGROUND . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21.4 TREATABILITY STUDY OBJECTIVES . . . . . . . . . . . . . . . . . . . . . . . 21 .5 TREATABILITY STUDY DESIGN . . . . . . . . . . . J . . . . . . . . . . . . . . . 4

1 .5. 1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41 .5.2 Data Quality Objectives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51 .5.3 Treatability Study Work Plan . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

1 .6 PROJECT RESPONSIBILITIES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 121.7 PROJECT COMMUNICATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181.8 PROJECT SCHEDULE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

2.0 QUALITY ASSURANCE OBJECTIVES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 202.1 INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 202.2 QUALITY CONTROL EFFORT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 202.3 ACCURACY, PRECISION, AND SENSITIVITY . . . . . . . . . . . . . . . . 222.4 COMPLETENESS, REPRESENTATIVENESS AND

COMPARABILITY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 232.5 IMP ACT OF NOT MEETING QA OBJECTIVES . . . . . . . . . . . . . . . . 25

3.0 SAMPLING SELECTION AND PROCEDURES . . . . . . . . . . . . . . . . . . . . . . . . 263.1 OVERVIEW . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 263.2 FIELD OPERATIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

3.2.1 Sample Collection and Preparation . . . . . . . . . . . . . . . . . . . . . . 263.2.2 Transportation / Chain-of-Custody Record . . . . . . . . . . . . . . . . 273.2.3 Receipt of Untreated Materials by Kiber . . . . . . . . . . . . . . . . . . 27

3.3 MATERIAL SAMPLING AND PREPARATIONS . . . . . . . . . . . . . . . 283.3.1 Untreated Sample Homogenization and Collection . . . . . . . . . . 283.3.2 Treated Material Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

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Southern Shipbuilding Corporation SiteQuality Assurance Project PlanRevision No. 117 October 1994Page ii

3.3.3 Site Water Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 293.3.4 Organic Emissions Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

3.3.5 Sample Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 293.3.6 Receipt of Samples by Analytical Laboratory . . . . . . . . . . . . . . 29

3.4 SAMPLE EQUIPMENT DECONTAMINATION . . . . . . . . . . . . . . . . 313.5 SAMPLE CONTAINERS AND PRESERVATION . . . . . . . . . . . . . . . 313.6 CHAIN-OF-CUSTODY RECORDS . . . . . . . . . . . . . . . . . . . . . . . . . . 33

3.6.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 333.6.2 Field Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 333.6.3 Internal Tracking . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 333.6.4 Shipment of Samples to Subcontract Laboratory . . . . . . . . . . . . 34

3.7 DOCUMENTATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

4.0 TESTING PROCEDURES AND CALIBRATION . . . . . . . . . . . . . . . . . . . . . . . 354.1 OVERVIEW . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 354.2 LABORATORY TESTING PROCEDURES . . . . . . . . . . . . . . . . . . . . 35

4.2.1 Analytical Methodologies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 354.2.2 Physical Properties Methodologies . . . . . . . . . . . . . . . . . . . . . . 364.2.3 Treatability Methodologies . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

4.3 CALIBRATION PROCEDURES AND FREQUENCY . . . . . . . . . . . . 38

5.0 DATA REDUCTION, VALIDATION AND REPORTING . . . . . . . . . . . . . . . . . 405.1 STANDARD RECORD MAINTENANCE . . . . . . . . . . . . . . . . . . . . . 405.2 LABORATORY DATA VALIDATION . . . . . . . . . . . . . . . . . . . . . . . 405.3 DATAREPORTING . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 415.4 DATA STORAGE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41

6.0 INTERNAL QUALITY CONTROL CHECKS . . . . . . . . . . . . . . . . . . . . . . . . . . 43

7.0 PERFORMANCE AND SYSTEM AUDITS . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45

8.0 CALCULATION OF DATA QUALITY INDICATORS . . . . . . . . . . . . . . . . . . . 478.1 OVERVIEW . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

000135

8.28.38.48.5

Southern Shipbuilding Corporation SiteQuality Assurance Project PlanRevision No. I17 October 1994Page iii

P R E C I S I O N . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47ACCURACY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . . . . . 47COMPLETENESS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48SENSITIVITY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

9.0 CORRECTIVE ACTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 499.1 TREATABILITY CORRECTIVRACTION . . . . . . . . . . . . . . . . . . . . 499.2 ANALYTICAL LABORATORY CORRECTIVE ACTION . . . . . . . . 51

10.0 QUALITY ASSURANCE REPORTS TO MANAGEMENT . . . . . . . . . . . . . . . 53

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Southern Shipbuilding Corporation SiteQuality Assurance Project PlanRevision No. 117 October 1994Page 1

1.0 PROJECT DESCRIPTION

1.1 INTRODUCTION

The United States Environmental Protection Agency (U.S. EPA) requires participation ofail U.S. EPA contractors in a centrally managed Quality Assurance (QA) program. Thisrequirement applies to all environmental monitoring and measurement efforts mandatedor supported by the U.S. EPA. This document is the Quality Assurance Project Plan(QAPP) for the Remedy Screening Treatability Study for Solidification/Stabilization ofSemivolatile Organic Compounds in Sludge from the Southern Shipbuilding CorporationSite. This QAPP was developed in accordance with the procedures and requirementsestablished in the following document:

U.S. EPA, February 1991, Preparation Aids for the Development of Category HIQuality Assurance Project Plans, EPA/600/8-91/005.

This document specifies the procedures that must be implemented to ensure the datagathered for the treatability study of soils and sludges at Southern Shipbuilding Site areconsistent with specific quality goals of accuracy, precision, completeness, andrepresentativeness.

1.2 GENERAL PROJECT OVERVIEW

The remedy screening treatability study for the Southern Shipbuilding Site will beperformed under the direction of PRC Environmental Management, Inc. (PRC) for theU.S. EPA, Office of Research and Development. The treatability study will beperformed under Contract Number 68-CO-0047 in support of the Superfiind TechnicalAssistance Response Team (START) program. Kiber Environmental Services, Inc.(Kiber) will be responsible for implementing the treatability study as a subcontractor to

000137


PRC. The remedy screening treatability study is being performed to determine theeffectiveness of solidification/stabilization treatment for immobilization of the organicsludges and reduction in the teachability of semivolatile organic compounds.

1.3 PROJECT BACKGROUND-*••«v.

The Southern Shipbuilding Corporation Site is located in the State of Louisiana. Theprincipal waste consists of a tarry sludge produced by barge cleaning operations.Adjacent soils and sediments have been affected. Contaminants of concern aresemivolatile organic compounds (SVOC). There is little evidence of SVOCs leaching tothe groundwater. There is evidence, however, of bulk movement of organics through thedikes separating the sludge pits from adjacent surface water. Volatile organiccompounds and metals are generally absent or present at low concentrations. MaximumSVOC concentrations in the sludge media are in the maximum range of 102 to 10* mg/kg.The two waste samples, to be provided by Region 6, for remedy screening are expectedto contain SVOC concentrations significantly lower than the maximum range presented.

1.4 TREATABILITY STUDY OBJECTIVES

The overall objective of the project is to perform a remedy screening treatability study toevaluate the effectiveness of solidification/stabilization treatment for semivolatilecontaminated materials at the Southern Shipbuilding Site. Although preliminaryremediation goals have not been specified for the Southern Shipbuilding Site, thefollowing objectives have been established for the treatability study:

1. Evaluate the chemical and physical characteristics including total and leachableSVOC concentrations, total organic carbon, pH, moisture content, bulk densityand specific gravity of the two contaminated sludges.

2. Perform all testing in accordance with methods approved by U.S. EPA SW-846 orthe American Society for Testing and Materials (ASTM), when available. Theteachability evaluations will be performed using a modified ToxicityCharacteristic Leaching Procedure (TCLP). The modification includes the

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substitution of upgradient site water for the extraction fluid specified in the testmethod.Identify one candidate mixture for treatment of the materials at the SouthernShipbuilding Corporation Site. Each candidate mixture will be selected based onevaluation of approximately 20 to 30 potential solidification/stabilizationmixtures applied to the contaminated soils and sludges. The mixtures will bedeveloped using proprietary reagents developed by International WasteTechnologies, Inc.; Rheox, Inc.; and Hazco Division of Fluidtech, Inc.; and non-proprietary reagents including Type I Portland cement, cement kiln dust, lime anda mixture of cement and fly ash. Preliminary screening tests will includequalitative emissions and temperature testing, volumetric expansion, andleachability evaluations.Perform qualitative monitoring of air emissions resulting from the treatmentprocess using a Photolonization Detector (PID), and evaluate the effect of thetreatment process on the material temperature using a laboratory-calibratedthermometer for all mixtures developed including preliminary screening mixturesand the final candidate mixture.Eliminate the presence of free liquids to ensure compliance with landfillrestrictions. Preliminary mixtures will be screened based on visual observationsof the mixtures. Compliance of each candidate mixture will be assured throughliquid release testing.Evaluate the ability of the treated material to support a protective cap byexhibiting an unconfmed compressive strength of greater than 50 pounds persquare inch (lb./in2). Preliminary mixtures will be screened based on review ofpenetrometer strength data. Compliance of each candidate mixture will bequantitated using unconfmed compressive strength testing.Determine SVOC concentrations for all target compounds through Total WasteAnalysis (TWA) of the candidate mixture, and evaluate the reduction of SVOCconcentrations for the most significant contaminants, primarily those present inthe untreated sludge at concentrations greater than 50 mg/kg.Determine the leachability in both the untreated and treated materials for allSVOC target compounds. Specifically, evaluate the contaminant reduction forcontaminants present in the untreated waste at leachable concentrations greaterthan three times the quantitation limited for each respective compound.

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9. Evaluate the effects of reagent dilution for all teachability and TWA evaluationsusing the following equation:Percent Reduction = [1 - (1+Additive Ratio) x (Cone. treated)/(Conc. Untreated)] x 100

where, the additive ratio is the amount of treatment reagents added as a weightratio relative to the waste; Cone, treated and Cone, untreated are theconcentrations of the contaminants of concern measured in treated and untreatedmaterials respectively.

10.. Determine the teachability of SVOCs for each candidate mixture in accordancewith TCLP regulatory procedures.

Again, the treatability study is being performed to support remedy screening; therefore,remediation goals have not been specified. The results of the study will be used toevaluate the chemical and physical characteristics of the treated material, and thechemical reductions achievable for each solidification/stabilization mixture developed.

1.5 TREATABILITY STUDY DESIGN

1.5.1 OverviewThe treatability study has been designed as five, distinct activities in order to achieve theproject objectives presented in Section 1.4, and to maintain the quality and integrityoutlined within this QAPP. The following summarizes the five activities of thetreatability study:

Activity No. 1Activity No. 2Activity No. 3Activity No. 4Activity No. 5

Work Plan / QAPP DevelopmentUntreated Waste CharacterizationPreliminary Treatment EvaluationsCandidate Treatment EvaluationsProject Reporting

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Southern Shipbuilding Corporation SiteQuality Assurance Project PlanRevision No. 117 October 1994PageS

The following subsections present the chemical and physical measurements to beperformed during the treatability study, and the Work Plan developed for remedyscreening of the solidification/stabilization technology.

1.5.2 Data Quality ObjectivesA series of critical and non-critical chemical and physical measurements will beperformed within activities numbered 2 through £, The critical measurements have beensegregated into primary and secondary critical measurements. The primary criticalmeasurement includes the modified leachability evaluations for S VOCs. Secondarycritical measurements include traditional TCLP regulatory testing and total wasteanalyses. Non-critical measurements are screening tests performed throughout thetreatability study to provide continual supporting information and qualitativeassessments. The non-critical measurements include organic emissions using a PID,temperature measurements, volumetric increase, bulk density, moisture content, pH andpenetrometer strength. In addition, the unconfined compressive strength and free liquidevaluations are non-critical measurements.

For each critical and non-critical measurement, a data quality objective (DQO) has beenassigned based on the intended use and interpretation of the resulting data. Thefollowing DQOs are applicable to the Southern Shipbuilding treatability study:

DQO Level I provides the lowest data quality but the most rapid results. It isoften used for health and safety monitoring at a site, preliminary comparison toARARs, initial site characterization to locate areas for subsequent and moreaccurate analyses, and for remedy screening of treatment alternatives. All non-critical measurements will be performed as screening measurements; therefore,DQO Level I will be implemented.DQO Level n provides an minimum level of quality and is used for laboratory orfield screening. This level may include mobile laboratory generated datadepending on the level of quality control exercised. DQO Level n is notapplicable to the Southern Shipbuilding study.DQO Level HI provides an intermediate level of data quality and is used forlaboratory measurements requiring complete data analyses including QAspecimens. All chemical characterizations associated with this treatability studywill be performed to achieve DQO Level IE.

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DQO Level IV provides the highest level of data quality and is used for purposesof risk assessment, and optimization of remedial alternatives. These analysesrequire full Contract Laboratory Program (CLP) analytical and data validationprocedures in accordance with a EPA recognized protocol. DQO Level IV is notapplicable to the Southern Shipbuilding study.

A summary of the analyses to be performed during each activity of the treatability studyis presented oh Table 1-1. A detailed presentation of the scope of work will be presentedin Section 1 .5.3. Table 1-1 includes an outline of the physical and chemicalmeasurements to be performed, the specified test method, the untreated sample type (i.e.,soil or sludge), measurement classification (i.e., primary critical, secondary critical ornoncritical), the specified DQO level, and the number of analytical, duplicate and qualitycontrol samples to be performed.

1.5.3 Treatabilitv Study Work PlanActivity No. 1 included development of the scope of work and this QAPP; no furtherdiscussion is included. Activity No. 2 includes untreated material characterizations.Upon receipt of the untreated materials, Kiber will gently homogenize each sludge tobetter ensure a uniform material. For bench-scale testing, Kiber will remove all materialgreater than 0.5 inches in size prior to initiation of the testing program outlined herein.Complete information pertaining to material sampling, receipt and preparation ispresented in Section 3.0. Representative aliquots of each waste will be sampled forcharacterization testing. The establishment of-the baseline level of contamination isimportant for comparing and determining the effectiveness of solidification/stabilizationtreatment. The results of the soil characterization will also allow Kiber to estimate thereagents and reagent concentrations necessary for effective treatment. The followinganalytical characterization testing will be conducted on duplicate samples of each sludgein accordance with the referenced test method:

Total SemivolatilesTCLP Semivolatiles (Modified)Total Organic CarbonMaterial pH

SW-846 3550 7 8270SW-846 1 3 1 1 / 3 5 1 0 7 8270SW-846 9060 (Modified)SW-846 9045

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SOUTHERN SHIPBUILDING CORPORATION SITEQUALITY ASSURANCE PROJECT PLAN

TABLE 1-1Summary of Chemical and Physical Measurements

LaboratoryParameter

I. Untreated Waste CharacterizationTWA SemivolatilesTWA SemivolatilesTCLP Semivolatiles (Modified)Total Organic CarbonMaterial pHMoisture ContentBulk Density / Specific Gravity

n. Preliminary Treatment Evaluations1

Mixture PreparationOrganic EmissionsTemperature MonitoringPenetrometer AnalysesVolumetric ExpansionTCLP Semivolatiles (Modified)

ffl. Candidate Treatment EvaluationsMixture PreparationTWA SemivolatilesTCLP SemivolatilesTCLP Semivolatiles (Modified)Unconfined Compressive StrengthLiquid Release Testing

MaterialMatrix

Site WaterSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / Sludge

Soil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / Sludge

Soil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / Sludge

MeasurementClassification

Secondary CriticalSecondary CriticalPrimary CriticalNon-criticalNon-criticalNon-criticalNon-critical

•

Non-criticalNon-criticalNon-criticalNon-criticalNon-critical

Primary Critical

Non-criticalSecondary CriticalSecondary CriticalPrimary CriticalNon-criticalNon-critical

DQO AnalyticalLevel

mmmIIII

IIIIIffl

. Ifflmffl.ii

Number of MeasurementsAnalysis

1222222

26: 262626

. , 26. 10

111111

Duplicate

1222222

M' 4

•A44442

111111

OA/OC

122----

-----

2

.111-

- Not applicable974202

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Southern Shipbuilding Corporation SiteQuality Assurance Project PlanReyision No. 117 October 1994PageS

Note that the total organic carbon (TOC) will be performed using a modified method9060. Kiber's subcontract laboratory will analyze the soil samples using a ShimadzuModel 5050 TOC Analyzer,Duplicate characterization of the upgradient site water will also be performed. Totalsemivolatile and leachability evaluations will be performed using particle sizes less than3/8 inch. This maximum particle size was selected to parallel recommendationspresented in the TCLP methodology. Also, modiSed TCLP semivolatile analyses will beperformed by substituting upgradient site water for the leaching fluid during theextraction procedure.

Physical properties characterization provides basic information on the handlingproperties of the contaminated soil. These properties are used to prepare cost estimatesand design specifications with regard to treatability testing, material excavation,transport, storage and treatment. The information generated is used in making soundengineering decisions. The following analyses will be conducted in duplicate for eachsludge in accordance with the referenced test methods:

Moisture ContentBulk Density / Specific Gravity

ASTMD2216ASTM D 698/2937

Activity No. 3 includes preliminary solidification/stabilization treatment evaluations.Preliminary evaluations will include treatment with both non-proprietary and proprietaryreagents. The non-proprietary reagents may include, but are not limited to Type IPortland cement, cement kiln dust, lime and a mixture of cement and fly ash. Severalproprietary reagents and treatment processes have demonstrated effective treatment forwastes containing high concentrations of both organic and inorganic contaminants. Theproprietary processes may include reagents developed by the following vendors:

International Waste Technologies, Inc.Rheox, Inc.Hazco Division of Fluidtech, Inc. ' .

The treatability laboratory has considerable experience evaluating the processes marketedby each of the above vendors.

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A total of 15 mixtures will be developed for each untreated sludge during preliminarysolidification/stabilization treatment. The blending process to be implemented for thetreatability study is a cost-effective process intended to mimic full-scale processes asmuch as possible on the laboratory scale. Specifically, the process is intended to providea basis for valid comparison between the different treatment options. Included as part ofthe 15 total mixtures are two duplicates which will be generated to determine thereproducibility of the treatment process. The duplicate mixtures will be selected atrandom during development of the treated mixtures.

Each mixture will be developed by placing aliquots of the untreated material into ablending chamber. To the untreated material, a reagent slurry will be added and blendedat a rate of approximately 30 to 60 rotations per minute (rpm) until visuallyhomogeneous, approximately 2 to 3 minutes. Throughout the treatment process, organicemissions as measured by a PID and temperature as measured by a digital temperatureprobe will be monitored for each mixture. The organic emissions will be determinedby mounting the PID probe to the run of the blending chamber. Initial readings willbe recorded prior to initiation of the treatment process in order to estimate thebackground levels. Monitoring will then be performed and recorded at regularintervals throughout the blending process. Initially, readings will be taken at veryclose intervals of 10 seconds. The intervals may be gradually increased to 20 to 30seconds between readings, if deemed appropriate by the task manager. Also,although readings will be taken at regular intervals, the PID will be monitored for themaximum reading. If the maximum reading, is achieved between readings, themaximum or peak value will be recorded. Temperature readings will be recorded inparallel with the organic emissions monitoring.

Sufficient material will be developed for each mixture in order to perform all analysesoutlined herein. The treated material will be compacted into cylinders measuringapproximately 2.0 inches in diameter by 4.0 inches in height and allowed to cure atambient humidity and a temperature of approximately 24 degrees Celsiu for a period of14 days. During the 14-day cure, the penetrometer strength analyses will be determinedfor each mixture to estimate the setting and strength properties of the treated materials atcure times of 4 hours, 1 day, 2 days, 3 days, 7 days, and 14 days. A Brainard-Kilman S-170 Pocket penetrometer or similar will be used for the penetrometer strength data. The

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pocket penetrometer is a hand held instrument commonly used during field drilling teststo estimate the unconfined compressive strength of soils. The penetrometer is calibratedby the manufacturer in increments of 0.25 tons per square foot (tsf) with a maximumreading of 4.5 tsf (63 psi).

Upon completion of the 14-day cure, the volumetric expansion due the addition of thetreatment reagents will be determined for each mixture. The volumetric expansion due toaddition of the treatment reagents is performed by compacting a pre-weighed aliquot ofsoil into a cylindrical sample mold. The volume of the untreated soil will be measuredand recorded. The soil will then be removed from the mold, and treated in accordancewith the protocols outlined above. Upon completion of the treatment process, thematerial will again be compacted into the same type of sample moid and allowed to curefor a period of 14 days. After completion of the 14-day cure, the volume of the treatedmaterial will be measured and recorded. The percent volumetric expansion or shrinkagewill be determined based on the following equation: [(Final Volume - Initial Volume) /Initial Volume]* 100.

Upon completion of the 14-day cure, a review of the test results will be performed inorder to identify potential reagent and reagent addition rates effective forsolidification/stabilization treatment of the Southern Shipbuilding materials. Theseevaluations will include review of organic emissions and temperature data, penetrometerstrength versus cure time, volumetric expansion, reagent cost, visual assessments ofmaterials both during treatment and after curing, and experience implementing full-scalesolidification/stabilization technology. Mixtures which appear to yield favorablecharacteristics based on these properties will be identified for teachability evaluations.The following guidlines will be used by EPA, PRC and Kiber in evaluating eachcriterion:

1. Organic emissions should be low. If the values cover a wide range, preferencewill be given to mixtures having emission rates in the lower half of the measuredvalues.

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2. Temperature increases should be low. Preference will be given to mixtureshaving temperature increases less than 10 degrees Celsius over ambienttemperature.

3. Strength should be high. Preference will be given to mixtures having highstrength or a trend showing continued or increased strength development duringcuring. Samples that do not set or develop.measurable strength will be excluded.

4. Volumetric expansion should be low. Preference will given to mixtures in thelower half of the range of measured values.

5. Visual assessments should show good mixing and blending, incorporation of thewaste throughout the treated matrix, uniform physical appearance, and minimaldefects such as bubbles, cracks, and so forth. Defects would result in mixtureexclusion. Preference will be given to a uniform appearance indicative of goodmixing and waste incorporation.

A total of 10 mixtures will be identified for modified TCLP semivolatile analyses. Twomixtures will be randomly selected for duplicate leachability testing. If 10 mixturescannot be identified as producing favorable properties based on review of the preliminaryresults, additional mixtures may need to be developed prior to completion of Activity No.3. These leachability analyses will provide the quantitative data necessary to identifycandidate treatment processes which achieve the project and QA objectives. Based on areview of the leachability analyses, one mixture will be selected for each waste materialfor additional treatment characterization.

Activity No. 4 will include treatment evaluations of a selected candidate mixture. Basedon review of the Activity No. 3 leachability analyses, one candidate treatmentformulation will be recommended for the candidate treatment evaluations. Activity No. 4will include evaluation of the candidate treatment.formulation in duplicate. Thecandidate mixture will be blended according to the protocols outlined for the preliminarystabilization treatment phase. A laboratory-scale Hobart-type mixer will be used totreated bulk aliquots of each material. Sufficient material will be treated in order toperform all of the specified analyses outlined for the candidate stabilization treatment

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Southern Shipbuilding Corporation SiteQuality Assurance Project PlanRevision No. I17 October 1994Page 12

phase. All monitoring and testing activities will be identical to those presented for thepreliminary evaluations presented above.

The treated specimens will be cured for a period of 14 days. At completion of the 14-daycure, the following analyses will be performed on each mixture:

Total SemivolatilesTCLP Semivolatiles (Modified)TCLP SemivolatilesUnconfined Compressive StrengthLiquid Release Testing

SW-8463550/8270SW-846 1 3 1 1 / 3 5 1 0 / 8 2 7 0SW-846 13 1 1 /35 10/8270ASTMD2166SW-846 9096

Traditional TCLP semivolatile analyses have been included in the final phase forcomparison of the treated materials to established regulatory values.

Activity No. 5 includes project reporting. Throughout the duration of the project, thetreatability laboratory will submit telefaxed memorandums to PRC and the U.S. EPA asresults become available. At the completion of the treatability study, a comprehensivereport will be submitted presenting all the applicable testing protocols and the test results.The U.S. EPA has indicated that publication of the report is not anticipated; therefore,U.S. EPA format requirements for research reports need not be met.

1.6 PROJECT RESPONSIBILITIES

The Southern Shipbuilding treatability study was designed based on a combined effort ofU.S. EPA, PRC and Kiber, as a subcontractor to PRC. Representatives of each groupwill be closely involved with the treatability study throughout the duration of the project;however, Kiber will be responsible for implementing the study at Kiber's laboratoryfacilities located in Atlanta, Georgia under the direct supervision and guidance of PRC.

The PRC SITE team personnel are dedicated to maintaining the quality of the SouthernShipbuilding project and the data generated as a result of the project activities. Figure 1-1 and the following sections provide an overview of the PRC SITE team employees whowill be responsible for the daily activities of the study.

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PRC PROJECT MANAGER: Mr. Paul Dean jThe PRC project manager, Paul Dean, or his designee is responsible for effectiveday-to-day management of the entire project staff, as well as for directcommunication with EPA. He is also responsible for ensuring that all PRC SITEteam personnel understand and comply with the QA/QC plans.

PRC SITE PROGRAM QA MANAGER: Dr. Kenneth Partymiller

The PRC SITE program QA manager, Kenneth Partymiller, will support the PRCproject manager, Paul Dean, and will coordinate QA technical operations amongproject staff. His specific responsibilities include the following:

Providing assistance and guidance in developing and revising the QAproject plan.Performing system audits of QA/QC for the work assignment team,standard operating procedures, and operations manuals to determinewhether the defined practices are appropriate.Auditing operations of the work assignment team to determine whetherthe defined operations are performed properly.Providing guidance and coordination to rapidly resolve any QA/QCproblems.Maintaining all QA records and QA data for inspection by programmanagers and EPA.Providing QA of the program data and document control and securitysystem that ensures chain-of-custody and confidentiality protection forprogram data and documentation.

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SOUTHERN SHIPBUILDING CORPORATION SITEPROJECT ORGANIZATION

FIGURE 1-1

EPAQAOFFICER

Ann LeitzingerEPA PROJECTMANAGER

Trish Erickson

PRC SITE PROGRAMMANAGERRobert Foster

START WORKASSIGNMENT MANAGER

JimRomine

PRC SITE QAMANAGER

Ken Partymiller

PRC PROJECTMANAGERPaul Dean

KJJ3ERPROJECTTEAM

PRCPROJECTSTAFF

PROJECTDIRECTOR

Tracv Bergquist

TECHNICALDIRECTOR

Neville KinghamQA/QC

DIRECTORCy Sharp

PROJECTMANAGER

Stephen Zarlinski

TREATABJLITYTASK MANAGERRobert Semenak

ANALYTICALTASK MANAGER

Cathi Sharp

TOC SUBCONTRACTLABORATORY

AES

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Kiber's personnel are dedicated to maintaining the quality of the Southern Shipbuildingproject and the data generated as a result of the activities. The following sections providean overview of the Kiber employees who will be responsible for the daily activities of thestudy.

PROJECT DIRECTOR: Ms. Tracy BergquistThe Project Director is responsible for verifying that the Southern Shipbuildingtreatability study meets EPA objectives and Kiber's quality standards. Inaddition, she is responsible for technical quality control and project oversight, andwill provide the project manager with access to corporate management.

TECHNICAL DIRECTOR: Mr. Neville W. KinghamAs Technical Director, Mr. Kingham is responsible for the direction of theSouthern Shipbuilding treatability study. The Technical Director has the overallresponsibility for verifying that the project meets EPA objectives and provides alltechnical oversight as to the application of the treatment process. The individualquality-related responsibilities of the Technical Director include:

Assignment of the Project Manager.Participation in the project review.Approval of project-specific QA documents, as required.Selection of the QA/QC Manager.Stopping work on a project if the project cannot be completed to requiredquality levels, if the quality requirements cannot be met, or if the scheduleor budget does not permit successful completion.

PROJECT MANAGER: Mr. Stephen J. ZarlinskiAs Project Manager, Mr. Zarlinski is responsible for implementing the project,and has the authority to commit the resources necessary to meet project objectives

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and requirements. The project manager's primary function is to see that technical,financial and scheduling objectives are achieved successfully. The projectmanager will provide the major point of contact and control between PRC, U.S.EPA and Kiber for matters concerning the Southern Shipbuilding treatabilitystudy. The individual responsibilities will include:

Define project objectives and develop a detailed work plan schedule.Establish project policy and procedures to address the specific needs ofthe project as a whole, as well as the objectives of each task.Acquire and apply technical and corporate resources as needed to performthe work within budget and schedule constraints.Develop and meet on-going project and/or task staffing requirements,including assignment of Task Managers and mechanisms to review andevaluate each task product.Review the work performed on each task to verify its quality,responsiveness, and timeliness.Review and analyze overall task performance with respect to plannedrequirements and authorizations.Ultimately be responsible for the preparation of all interim and finalreports.

QA/QC MANAGER: Mr. Cy SharpAs QA/QC Manager, Mr. Sharp will remain separate and distinct from any otherproject-related duties. The QA/QC Manager is responsible for maintainingconformance with this project-specific QAPP, Kiber's Corporate QA/QC Plan,and EPA-related methodologies. The following lists several specific duties of theQA/QC Manager:

Tracking validation data and ensuring adherence to published guidelines.Determining if the levels of QA/QC are being achieved.Certifying the level of QA/QC for each analytical project.

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Maintaining QA/QC procedures.Assuring the continuity of chain-of-custody evidence.Initiate and overseeing audit functions.Submittai of QA reports to Project Director.

•*••Supervisory training of new and current personnel.Implementation of corrective actions.

TASK MANAGERS: Mr. Robert K. Semenak and Ms. Cathi SharpThe project Task Managers will provide support to the Project Manager. TheTask Managers will lead and coordinate all day-to-day activities associated witheach of the resources under his or her supervision. The Task Managers areexperienced environmental professionals who report directly to the ProjectManager or Project Director. Mr. Semenak will serve as Task Manager for alltreatability and physical properties evaluations, while Ms. Sharp will serve asTask Manager for analytical services. The individual responsibilities of the TaskManagers will include:

Day-to-day coordination with the Project Manager on technical issues andscheduling of project tasks.Oversight of laboratory services, scheduling compliance and adherence tostudy requirements as developed by either the Project Manager orTechnical Director.Authorship and review of text, graphics and data reduction required forthe treatability study.Oversight of final report preparation.

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1.7 PROJECT COMMUNICATION

Kiber has outlined a scope of work which includes five separate activities associated withthe treatability study. During each of these activities, PRC will maintain continuouscommunication between U.S. EPA and Kiber. Communications between Kiber, PRC andthe U.S. EPA will ultimately be the responsibility of the appointed Project Manager foreach group. These communications will includenveekly and bi-weekly conference calls,telefaxed memorandums presenting interim test results, and a comprehensive report uponcompletion of the treatability study.

Kiber will be responsible for all critical and non-critical testing, except for the totalorganic carbon (TOC) analyses. Kiber will subcontract these analyses to AnalyticalEnvironmental Services, Inc. (AES). Kiber routinely subcontracts these additionalservices to AES. The QA/QC program implemented by AES is evaluated by Kiber'sQA/QC Manager to ensure the quality of testing. Any additional QA protocols outlinedon a project specific basis are transmitted to AES prior to initiation of the testingprogram. Kiber's QA/QC Manager will confirm implementation of any additionalprotocols requested prior to any sample submittal. In addition to the regular QA/QCaudits, Kiber's personnel will review each set of analyses performed by AES to ensureconformity with Kiber's QA/QC requirements and any requirements specific to theSouthern Shipbuilding project. Only data that meets Kiber's QA/QC requirements willbe reported for the treatability study. Any discrepancies in the data will be resolved, and,if necessary, the sample will be reanalyzed prior to data reporting.

1.8 PROJECT SCHEDULE

Kiber is expected to receive the material for testing during the week of 5 September1994. The testing portion of the treatability study will begin immediately after receipt ofthe samples. Once initiated, the study is expected to last approximately 12 weeks

000154


including project reporting and review. More specifically, the projected completion ofeach activity is presented below:

Activity No. 1Activity No. 2Activity No. 3Activity No. 4Activity No. 5

Work Plan / QAPP Development Aug 31Untreated Waste Characterization Sep 16Preliminary Treatment Evaluations Oct 14Candidate Treatment Evaluations Nov 4Project Reporting Dec 1

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2.0 QUALITY ASSURANCE OBJECTIVES

2.1 INTRODUCTION

The overall QA objective is to develop and implement procedures that produce test datathat can be used to make sound technical decisions. Specific procedures for sampling,chain of custody, laboratory instrumentation calibration, laboratory analysis, internalquality control, audits, preventative maintenance, and corrective actions are described inother sections of this QAPP. This section defines the quality assurance objectives foraccuracy, precision, and sensitivity of analyses, and for completeness, representativeness,and comparability of reported data from all analytical laboratories.

2.2 QUALITY CONTROL EFFORT

The analytical QA/QC program established for the Southern Shipbuilding treatabilitystudy includes a series of duplicates and matrix spike samples. These selected samplesare analyzed to assess the quality of data resulting from the treatability study program.Duplicate samples are analyzed to check for reproducibility. Matrix spikes provideinformation about the effect of the sample matrix on the extraction and measurementmethodology. All matrix spikes are performed in duplicate and are hereafter referred toas MS/MSD samples. MS/MSD samples are only designated for the S VOC analyses.MS/MSD analyses will be specified for all S VOC analyses; however, experienceindicates that a matrix effect may be observed for the treated materials. The reason forthe potential matrix interferences after treatment is attributed to the fact that the goal ofthe solidification/stabilization technology is to chemically bind organic compounds intothe sample matrix. Therefore, disqualification of treated data based on a matrix effectwould be improper since the treatment is designed to result in a matrix effect. Thesuccess of the treatment will often depend on the matrix effect. The effect of the matrixwill therefore be evaluated based on review of both the MS/MSD and duplicate analyses.Upon review of the data by Kiber's QA/QC Manager, additional analyses may beperformed if warranted. The modified TCLP procedure will include one TCLP blank in

000156


order to assess any problems or contamination induced during TCLP set-up, rotating andfiltering. Upon completion of TCLP procedure, this blank will be handled as anadditional sample with regards to the S VOC analyses. TCLP blanks will be performed ata rate of one blank for every 20 analyses, or one blank per day whichever is greater.These blanks are intended to observe any contamination or problems resulting from theTCLP preparation, extraction fluid, and extraction procedure. The modified TCLPprocedure will only use the modified leachate consisting of site water. If a regulatoryTCLP is performed, a corresponding blank of the acid leachate will also be performed. Ifboth modified and regulatory TCLP analyses are performed, one blank of each will beperformed.

During performance of the SVOC extraction procedure in accordance with SW-846method 3550 or 3510, an extraction blank spike (BBS) will be performed in order toevaluate any potential problems or contaminated resulting from the SVOC extractionprocedure. A minimum of one set of QA samples will be analyzed per waste stream foreach set of samples submitted for analyses. Surrogate recoveries will be performed forevery sample analyzed including samples, duplicates, MS/MSD, and blanks. Surrogaterecoveries are performed to detect any problems resulting from the analyticalinstrumentation.

The non-critical TOC analyses will include analysis of 1) replicate samples in addition tothe duplicate samples specified in the work plan, and 2) laboratory blank. Because of thepotential for interferences and the gross nature of the TOC analyses, MS/MSD samplesare not recommended for soils and sludges unless the matrix has exceedingly low organiccontent. Experience indicates that considerable variability of the TOC measurements isanticipated due to the heterogeneity of the waste materials.

The remaining non-critical measurements include physical properties measurements andqualitative assessments performed during the treatment and curing stages. The primaryQA associated with these analyses include equipment calibration, and training andsupervision of laboratory operations by personnel experience both in laboratory testingand full-scale implementation of the solidification/stabilization technology. Whenappropriate, duplicate samples will be analyzed to evaluate the potential variation andreproducibility of the test data.

000157


2.3 ACCURACY, PRECISION, AND SENSITIVITY

The U.S. EPA recognizes three levels of treatability studies designed to evaluate and,ultimately, to implement one or more technologies for treatment of waste materials.These levels of treatability testing are generally undertaken as part of the remedyselection and implementation process, including i-) laboratory or remedy, screening, 2)bench-scale testing, and 3) pilot-scale testing (EPA/540/2-89/058, December 1989). TheSouthern Shipbuilding Site is being performed as a Level 1 study. The treatability studydata will be used to establish the validity of solidification/stabilization technology to treatcontaminated materials at the site. The test results are only to be used as indicators of theeffectiveness of the treatment technology. Although remediation goals have not beenestablished for the Southern Shipbuilding Site, a series of treatability study objectiveshave been established for evaluation of the solidification/stabilization treatment. Thesegoals are presented in Section 1.4. Based on these goals, fundamental QA objectives,with respect to accuracy, precision, and sensitivity of laboratory analytical data, havebeen established for the critical chemical testing. Table 2-1 summarizes the accuracy,precision and sensitivity requirements for each measurement test to be performed.

A series of non-critical measurements will be performed to provide additionalinformation as to the effectiveness of the solidification/stabilization technology. Theseanalyses are being performed simply to provide additional information which may provebeneficial in the evaluation of the solidification/stabilization remedy. Ifsolidification/stabilization is selected as a potential remedy, a second level, or bench-scale treatability study will need to be performed to verify that the technology can meetestablished remediation goals, to support remedy evaluation criteria, and to providenecessary cost and design information. Therefore, precision and accuracy beyond thatdiscussed herein have not been established for this phase of treatability testing.

The non-critical physical measurements include moisture content, bulk density,volumetric expansion, and unconfined compressive strength. These measurements willbe performed using DQO Level I. The equipment associated with these measurementswill be calibrated on yearly basis, or more if deemed necessary by the appropriate taskmanager. In addition, the calibration of the ovens, balances and pH meters are verified

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on a daily basis. The pH meter is calibrated daily using a two-point calibration procedureas recommended by the manufacturer. The balances are calibrated every six months withdaily verification using a three-point range of calibration weights. The oventemperatures are monitored daily, and the temperatures verified using a calibratedthermometer on a weekly basis.

The PID will be used to monitor for organic emissions during the treatment process. TheFDD will be serviced by a manufacturer-authorized service representative prior toinitiation of the treatability study. The accuracy of the Pro meter will be assessed bydaily calibration with isobutylene, a standardized reference gas.

The thermometers used to monitor temperature increases during the treatment processwill be compared to a certified thermometer at two temperatures prior to initiation of thetreatability study.

2.4 COMPLETENESS, REPRESENTATIVENESS AND COMPARABILITY

Completeness is a measure of the amount of valid data obtained from a measurementsystem compared to the amount that was expected to be obtained under normalconditions. It is expected that the critical measurements will meet the QC acceptancecriteria of 90 percent or more for all samples. Upon completion of the analytical testing,the percent complete will be calculated by determining the percentage of valid dataversus the total number of samples collected for analysis.

Representativeness expresses the degree to which data accurately and preciselyrepresents a characteristics of a population, parameter variations at a sampling point,process conditions, or an environmental condition. Representativeness is a qualitativeparameter which is dependent upon the proper design of the sampling program andproper laboratory protocol. The sampling and-analysis program outlined in the scope ofwork was designed to provide representative data necessary for evaluation of the

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TABLE 2-1Summary of QA Objectives

LaboratoryParameter

I. Critical MeasurementsTWA SemivolatilesTWA SemivolatilesTCLP Semivolatiles (Modified)TCLP Semivolatiles

II, Non-critical MeasurementsTotal Organic CarbonMaterial pHMoisture ContentHulk Density / Specific GravityMixture PreparationOrganic Emissions MonitoringTemperature MonitoringVolumetric ExpansionUnconfined Compressive StrengthLiquid Release Testing

MaterialMatrix

WaterSoil / SludgeSoil / SludgeSoil / Sludge

Soil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / Sludge

TestMethod

SW-846 35 10/8270SW-846 3550/8270

SW-846 131 1/3510/8270SW-846 13 11/3510/8270^

SW-846 9060SW-846 9045ASTMD2216

ASTM D 698/2937-(See Note 1)

Photoionization DetectorThermocouple- (Sec Note 1)ASTM D 2 166SW-846 9096

ReportingUnits

ug/Lmg/kgug/Lug/L

mg/kgs.u.°/°Ib. per cubic ft.

-(See Note 1)Parts per millionDegrees Celsius

%Ib. per square in.

Pass / Fail

MethodDetection Limits

10101010

10- (See Note 1)-(See Note 1)-(Sec Note 1)- (See Note 1)-(See Note 1)- (See Note 1)- (See Note 1)- (See Note 1)- (See Note 1)

Precision(RPD)

<30<30<30<30

4 35* 20-(See Note 2)- (Sec Note 2)-(See Note 2)-(See Note 2)-(See Note 2)- (See Note 2)- (See Note 2)- (See Note 2)

Accuracy(% Recovery)

(See SOP O-02)(See SOP O-02)(See SOP O-02)(See SOP 0-02)

- (See Note 2)-(See Note 2)-(See Note 2)- (Sec Note 2)-(See Note 2)- (See Note 2)-(See Note 2)- (See Note 2)-(See Note 2)-(See Note 2)

Completeness(%)

100100100100

100 *10 :0100100100100100100100 :.

100

(1) Not applicable(2) Due to the screening nature of the remedy screening, precision and accuracy levels have not been specified for many of the non-critical analyses. Also, the majority of the analyses will only include one-point analysis.

Although precision and accuracy measurements will no be obtainable for single determinations, differences between similar treatment mixtures within a series of reagent concentrations will be sufficient to make sound

974 203

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solidification/stabilization technology as a potential remedy for the SouthernShipbuilding Site. During development of the treatability study, consideration was givento existing chemical and physical characterizations, proposed treatment reagents andprocesses, potential remedial objectives, and experiences of U.S. EPA, PRC and Kiber atimplementing and troubleshooting full-scale solidification/stabilization treatmentprocesses. Representativeness will be satisfied by ensuring that proper samplingtechniques are used, proper analytical procedurescand DQOs are followed and specified,and holding times of the samples are not exceeded in the laboratory. Representativenesswill be assessed by the analysis of duplicate samples, when appropriate.

Comparability is the confidence with which one data set can be compared with anotherdata set. The extent to which existing and planned analytical data will be comparabledepends on the similarity of sampling and analytical methods. The procedures used toobtain the planned analytical data, as documented in the QAPP, are expected to providecomparable data. The analytical data, however, may not be directly comparable toexisting data because of differences in procedures and QA objectives.

2.5 IMPACT OF NOT MEETING QA OBJECTIVES

The QA/QC objectives should be met completely without any outliers. However, ifunforeseen conditions or data mishandling results in failure to meet the objectives, re-analysis will occur if possible. If the QA/QC manager believes that re-analysis is notnecessary or possible, the result will be flagged and a case narrative written regarding theimpact and the potential usability of the data. The severity of the impact will depend onthe specific occurrence and the corresponding QA objective. Regardless of severity, anyimpact or unacceptable test data will be reported by Kiber directly to PRC uponoccurrence.

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3.0 SAMPLING SELECTION AND PROCEDURES

3.1 OVERVIEW

This section addresses the sampling procedures to.be followed during all laboratoryportions of the treatability study. Information discussed herein will include samplingplan rationale, sample identification, sample container and preservation, chain of custody,and documentation. Sample types and matrices which will be included as part of thetreatability study will include untreated soil and sludges, treated soil and sludges, organicemissions during the treatment process, and upgradient site water to be used during themodified TCLP testing. The scope of work associated with the sampling protocols isaddressed in Section 1 .5.

3.2 FIELD OPERATIONS

3.2.1 Sample Collection and PreparationU.S. EPA Region 6 personnel, or appointed representatives, are to collect samples fromthe Southern Shipbuilding Site which are representative of the average site materials.Collected materials are to be carefully transferred to containers which meet all regulatoryrequirements. Each container should be completely filled to minimize headspace. Thesample containers are to remain tightly closed and stored in a cool, shaded area betweensampling episodes. In order to complete the treatability study outlined, approximately 60pounds of each the contaminated soil and sludge will be required. To complete themodified TCLP testing, approximately 35 gallons of upgradient site water will also berequired.

Field sampling personnel must properly identify all samples collected for the treatabilitystudy. The sample label must contain the following information:

Site nameSample identification number

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Date and time of collectionLocation of sample collection

The sample identification information must be printed in a legible manner using indelibleink. The field identification information must be sufficient to enable cross-reference withthe field notebook and chain-of-custody record.

3.2.2 Transportation / Chain-of-Custody RecordChain-of-custody records are to be included in each sample shipment. The custodyrecord is to be completed by the designated site personnel, in duplicate. The informationspecified on the chain-of-custody records will contain the same level of detail asmaintained by the field personnel, with the exception that the on-site measurement dataneed not be recorded. The custody record will include, at a minimum, the followinginformation:

Name of person collecting the sampleSample identification numberDate and time of sample collectionNumber and size of containers usedType of preservation materialsSignature of site personnel relinquishing the samplesName of overnight courier used to ship the materials and the airbill numberDate and time of custody transfer to overnight courier

The duplicate records are to be placed in plastic bags and attached to each container oradhered to each lid. Each container should then be tightly bound with filament tape.Finally, at least two custody seals are to be signed by the individual relinquishingcustody, and affixed in such a way that the container cannot be opened without breakingthe seal.

3.2.3 Receipt of Untreated Materials by KiberU.S. EPA Region 6, or appointed representatives, will be responsible for shipment of theuntreated soils to Kiber's facilities located in Atlanta, Georgia. Once the materials havebeen received by Kiber, the samples will be placed in a secured, temperature-controlledrefrigerator maintained at 4 degrees Celsius (°C).

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3.3 MATERIAL SAMPLING AND PREPARATIONS

3.3.1 Untreated Sample Homogenization and CollectionPrior to initiation of the treatability testing, each waste material (i.e., the soil and sludge)will be separately homogenized in order to create more uniform materials for treatabilitytesting. Homogenization will involve emptying the drum for one of the materials into alarge mixing pan and blending with stainless steel mixing instruments. In order tominimize potential loss of contaminants through volatilization, the homogenizationprocess will be performed using the chilled materials and low energy hand mixing.During the homogenization process, organic emissions will be monitored using a PID.The highest reading obtained, as well as periodic readings, will be recorded. When eachwaste appears visually homogeneous, representative aliquots of the homogenizedmaterial will be transferred into the respective sample container, using stainless steelspoons, in the following order for analysis: S VOCs, TOC, pH and physicalmeasurements. The remaining material will be placed back into the original container inwhich it was received. All materials will be kept in refrigerated storage.

3.3.2 Treated Material SamplingThroughout the duration of the treatability study, samples of treated material will becollected for analysis of the various critical and non-critical parameters. The samplingmethod will be dictated by the physical or chemical measurement performed. As afunction of the treatment process outlined in Section 1.5, each untreated material will beblended with various treatment reagents. Once blended, the treated material will becompacted into cylindrical molds and allowed to cure for a specified time period. Oncethe materials have cured, the mold for each mixture is cut away from the sample. Exceptfor the unconfmed compressive strength (UCS) testing, representative samples will becollected from the molded sample by cutting each mold into a number of subsections andtransferring the subsections from the top, middle and bottom of each mold to a mortar forpreparation for analysis. The sample is crushed with a mortar and pestle and thentransferred to the appropriate sample container. The sample is then transferred to theanalytical laboratory under internal chain-of-custody tracking. The entire samplingprocess is accomplished as quickly as possible to minimize contaminant loss throughemissions.

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The UCS determinations are performed using the entire cylindrical mold. Therefore,once the treated sample has cured and the mold is cut away, the sample remains intact forUCS testing. This sampling process is only used for specimens subjected to UCS testing.

3.3.3 Site Water SamplingThe upgradient site water will need to be sampled prior to each round of modified TCLPtesting. The water will be homogenized by first-gently stirring the water. Aliquots of thewater will then be transferred between two containers in an effort to create a morehomogeneous sample. The U.S. EPA has indicated that the upgradient site water has notbeen contaminated from the site soils and sludges; however, care will be taken during thewater homogenization to minimize any potential contaminant loss through volatilization.As such, all homogenization will be performed on refrigerated water using low energymixing and stirring methods. PID monitoring will be performed in order to evaluate anyorganic emissions resulting from the homogenization process. No treatability testing willbe performed on the site water. The water will be used as the leaching fluid for themodified TCLP analyses. The homogenized water will be gently stirred prior to eachsampling episode throughout the treatability study.

3.3.4 Organic Emissions SamplingThe only air sampling will be the qualitative organic emissions monitoring performedduring material homogenization and treatment. The organic emissions will be monitoredusing a PHD manufactured by HNu Model PI-101. The organic emissions will bedetermined by mounting the PID probe to the rim of the blending chamber. Initialreadings will be recorded prior to initiation of the treatment process in order to estimatethe background levels. Monitoring will then be performed and recorded at regularintervals throughout the blending process. Initially, readings will be taken at very closeintervals of 10 seconds. These initial readings are intended to characterize thevolatilization occurring upon initiation of the mixing process. The intervals may begradually increased to 20 or 30 seconds between readings; if deemed appropriate by thetask manager. Also, although readings will be taken at regular intervals, the PID will bemonitored for the maximum reading. If the maximum reading is achieved betweenscheduled readings, the maximum, or peak, value will be recorded.

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3.3.5 Sample LabelsA sample label will be attached to each sample container collected for physical andchemical testing. The treatability study log book and the sample label will contain thefollowing information:

Laboratory project numberSample identification number -^Date and time of collectionDescription of sampleName of sampling personnel

3.3.6 Receipt of Samples by Analytical LaboratoryA detailed discussion of the sample receiving and storage protocols are presented as astandard operating procedure contained in Appendix A. Generally, laboratory personnelwill proceed with the following protocols prior to initiation of each respective analysis:

1. Verify the integrity of the samples and containers. This verification includeschecking for leakage, cracked or broken closures, obvious odors, and grosslycontaminated exteriors.

2. Check to confirm that the Work Order Request Form (WORF) contains all of therequired information. If the form does not, the project manager or appointedrepresentative should be notified immediately.

3. Once all samples and corresponding paper worked has been verified, the samplecustodian will execute the WORF indicating acceptance.

4. Each sample should be checked for proper preservation (pH and temperature).5. The WORF is placed in the laboratory project file with one copy submitted to the

project manager.6. The samples should be placed directly into the refrigerated storage marked

"Samples Only", except samples being evaluated for UCS, pH and free liquids.Detailed discussions of sample containerization and preservation are presented inSection 3.5.

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3.4 SAMPLE EQUIPMENT DECONTAMINATION

All sampling equipment and utensils are thoroughly cleaned and decontaminated prior toeach sampling or treatment episode utilizing accepted procedures for cleaning laboratoryglassware and equipment. Cleaning procedures differ based on intended use, but alwaysinclude washing in analyte-free detergents and tap water rinses, followed by triplicaterinses of deionized or laboratory grade water. Laboratory glassware and equipment ismanually washed until all signs of visible discoloration and/or any materials that mayhave been present are eliminated. If necessary, the process is repeated. All chipped,cracked, visually discolored, or fractured equipment is discarded or repairedimmediately. Also, heavy sludge contamination may require an additional stage ofwashing with a weak nitric acid solution followed by several rinses with deionized water.

All containers used to hold samples for analytical characterization are provided byEnvironmental Sampling Supply (ESS). The containers are purchased as precleaned,certified containers. The containers used are chemically cleaned by the specified U.S.EPA cleaning procedure for low level chemical analysis. Each container shipment isreceived with a Certificate of Compliance verifying that the containers achieve thedetection limits established by the U.S. EPA in the specifications and guidance forobtaining contaminant-free sample containers.

3.5 SAMPLE CONTAINERS AND PRESERVATION

All samples collected for chemical and physical analyses will be containerized andpreserved according to the requirements presented on Table 3-1. All samples, exceptthose for UCS, density, pH, and moisture content, will be containerized in glass jars withTeflon-lined lids. As stated hi Section 3.4, the glass containers will be precleanedcertified. All samples will be collected in accordance with/the appropriate procedurespresented in Section 3.3 . All samples, except those to be analyzed for pH, UCS, moisturecontent, density, and free liquids, will be held for no more than 28 days and preserved bychilling to 4 °C. These samples will be analyzed immediately and with no preservative.

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TABLE 3-1Summary of Sample, Containers, Volumes, Preservation, and Holding Times

LaboratoryParameter

I. Critical MeasurementsTWA SemivolatilesTWA SemivolatilesTCLP Semivolatiles (Modified)TCLP Semivolatiles

II. Non-critical MeasurementsTotal Organic CarbonMaterial pHMoisture ContentBulk Density / Specific GravityVolumetric ExpansionUnconfined Compressive StrengthLiquid Release Testing

MaterialMatrix

Site WaterSoil / SludgeSoil / SludgeSoil / Sludge

Soil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / SludgeSoil / Sludge

TestMethod

SW-846 35 10/8270SW-846 3550/8270

SW-846 131 1/3510/8270SW-846 13 1 1/35 10/8270

SW-846 9060SW-846 9045ASTMD2216ASTMD698

-ASTMD2166SW-846 9096

Container

Glass, 1 liter with teflon-lined capGlass, 8 oz widemouth with teflon-lined capGlass, 8 oz widemouth with teflon-lined capGlass, 8 oz widemouth with teflon-lined cap

Glass, 4 oz widemouth with teflon-linejd capPlastic or Glass • 'Plastic or GlassPlastic or GlassPlastic or Glass

-

Preservation

Cool, 4 °CCool, 4 °CCool, 4 °CCool, 4 °C

Cool, 4 °C-

.---

MaximumHolding Time?

14 Days14 Days14 Days14 Days

28 DaysAnalyze ImmediatelyAnalyze Immediately .Analyze ImmediatelyAnalyze ImmediatelyAnalyze ImmediatelyAnalyze Immediately

• Not applicable974 204

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Chilling these specimens may impact the representativeness of the test results. Samplecontainer size, preservation, maximum holding time, and analytical technique for eachanalysis is presented on Table 3-1.

3.6 CHAIN-OF-CUSTODY RECORDS' f.

3.6.1 OverviewThe chain-of-possession, or custody must be maintained for any samples submitted to thetreatability and analytical laboratories, or any sample generated as part of the treatmentevaluations. Written procedures must be available and followed whenever samples aretransferred, stored, analyzed or destroyed. The primary objective of these procedures areto create an accurate written record which can be used to trace possession of the samplesthroughout the duration of the treatability study. The following sections outline thechain-of-custody procedures to be implemented for the Southern Shipbuilding treatabilitystudy.

3.6.2 Field SamplingRequirements for chain-of-custody records for shipment of untreated soil, sludge andwater materials from the Southern Shipbuilding site to Kiber's facilities located inAtlanta, Georgia were previously presented in Section 3.2.2.

3.6.3 Internal TrackingSample possession within Kiber's facilities between the treatability and analyticallaboratories will be monitored utilizing a Work Order Request Form (WORF). TheWORF is similar to a chain-of-custody record, except that it is used only byrepresentatives of Kiber for internal tracking of samples. Each WORF is reviewed andauthorized by the project manager, or an appointed representative.. In addition to trackinginternal sample possession, the WORF provides laboratory personnel with the necessaryauthorization to proceed in accordance with the protocols outlined herein. Each WORF,at a minimum, contains the following information:

Project name and numberSample number

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Sample preservationDate and time of sample collectionName of samplerSignatures and dates of all persons involved in sample possessionAnalyses to be performedComments about each sampleProject manager's authorization

3.6.4 Shipment of Samples to Subcontract LaboratoryAs indicated in Section 1 .7, Kiber will be responsible for all critical and non-criticaltesting, except for the TOC analyses. Kiber will subcontract these analyses to AnalyticalEnvironmental Services, Inc. (AES). In preparation for shipment to the subcontractlaboratory, all samples will be packaged by securely sealing the lids with tape andverifying that the sample labels are securely attached to each container. Each sampleshipment will be performed under chain-of-custody record via overnight courier. Thechain-of-custody protocols outlined in Section 3.2.2 will be followed for shipment ofsamples to the subcontract laboratory.

3.7 DOCUMENTATION

To properly document all aspects of the treatability study, a log book is used to record allpertinent project information. The log book is a bound ledger, preferably withconsecutively numbered pages, that is maintained for each single treatability study.Information pertaining to all aspects of the study will be recorded in this document. Allcorrespondences, laboratory reports, and data will be maintained in the project files. AHoriginal laboratory reports are maintained in the original format and stored separatelyfrom working copies of these reports. The appointed project managers for eachrespective party will be responsible for maintaining the project files. Upon completion ofthe treatability study, the files will be stored in a centralized project file storage area, ortransferred to a secure document storage facility.-

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4.0 TESTING PROCEDURES AND CALIBRATION

4.1 OVERVIEW

The testing procedures specified for the Southerns-Shipbuilding remedy screeningtreatability study consist of known, tested and approved EPA and/or ASTMmethodologies. Standard operating procedures (SOPs) have been developed for each ofthe approved methodologies. Copies of the applicable SOPs developed by Kiber arepresented in Appendix A. For solidification/stabilization treatment and evaluations, suchas mixture preparation, curing, organic emissions, temperature monitoring, andvolumetric expansion, the procedures outlined within the scope of work presented inSection 1 .5 .3 will be followed. This section presents the procedures specified in thereferenced scope of work and an overview of the calibrations for any associatedequipment.

4.2 LABORATORY TESTING PROCEDURES

4.2.1 Analytical MethodologiesAs outlined in the scope of work presented in Section 1.5.3, all analytical testing, exceptfor TOC analyses, will be performed by Kiber.. The analytical testing will be conductedhi accordance with SW-846 methodologies. The following analyses have been specifiedin accordance with the referenced test methods:

Total Semivolatiles SW-846 3550 / 8270TCLP (modified) Semivolatiles SW-846 1 3 1 1 / 3 5 1 0 7 8270Total Organic Carbon SW-846 9060 (mod.)Material pH SW-846 9045

A brief description of each analytical method is presented below. A copy of Kiber's SOPfor each analysis is included in Appendix A.

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Semivolatile Organics include acid and base-neutral organic compoundsrecommended in SW-846 method 8270. Materials are prepared using a solventextraction. Soils are prepared in accordance with SW-846 method 3550, whileliquids are prepared in accordance with SW-846 method 3510. In accorance withthe SOP, extraction blank spikes and extraction blanks will be performed. Theseextraction blanks will be performed using water and methylene chloride for liquidsamples. For soil samples, 30 grams of sodium sulfate will be extracted. Theextracts generated are concentrated, then-injected directly into the GC/MS forquantitation.The Toxicity Characteristic Leaching Procedure (TCLP) is used by the U.S.EPA as the basis for promulgation of best demonstrated available technologies(BDAT) treatment standards under the land disposal restrictions program. Forthis remedy screening treatability study, the TCLP extraction process will bemodified to use upgradient site water as the extraction fluid. The SOP presentedin Appendix A covers complete TCLP testing. Upon initiation of the treatabilitystudy, a procedure deviation will be completed and approved by Kiber's QA/QCManager prior to implementation of the modified TCLP extraction.Total Organic Carbon (TOC) is measured using a carbonaceous analyzer. Thisinstrument converts the organic carbon in a sample to carbon dioxide by eithercatalytic combustion or wet chemical oxidation. The carbon dioxide formed isthen either measured directly by an infrared detector or converted to methane andmeasured by a flame ionization detector. The amount of carbon dioxide ormethane in a sample is directly proportional to the concentration of carbonaceousmaterial.

4.2.2 Physical Properties MethodologiesAs outlined in the scope of work presented in Section 1.5.3, all physical measurementswill be performed by Kiber. The physical measurements will be performed inaccordance with methodologies approved by the U.S. EPA and/or ASTM. The followingphysical properties analyses will be performed in accordance with the referenced testmethods:

Unconfined Compressive StrengthLiquid Release Testing (Free Liquids)Moisture ContentBulk Density / Specific Gravity

ASTM D 2166SW-846 9096ASTM D 2216ASTM D 698 72937

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1Southern Shipbuilding Corporation SiteQuality Assurance Project PlanRevision No. I17 October 1994Page 37

Physical properties testing is an essential element in the effective evaluation of thematerial handling characteristics. These particular tests were selected due to theirrecognition as viable testing methods, their availability, and their suitability forevaluating waste and waste-like materials. A copy of Kiber's SOPs for each analysis arepresented in Appendix A. A brief description of each test method is presented below.

Unconfined Compressive Strength (UCS) testing measures the shear strength ofcohesive, soil-like material in unsaturated, undrained conditions without lateralconfinement of the sample. UCS tests for unstabilized materials have limitedapplication. The U.S. EPA considers a stabilized material to have a satisfactoryUCS with a strength of 50 pounds per square inch (psi) or greater (U.S. EPAOWSER Directive No. 9437.00-2A).Liquid Release Testing (LRT) is a laboratory test designed to determine whetheror not liquids will be released from materials when subjected to overburdenpressures in a landfill. The liquid release testing is intended to provide similarinformation to the paint filter test. This testing is performed in strict accordancewith SW-846 method 9096. "Moisture Content testing determines the amount of free water or fluid in a givenamount of material.Bulk Density is the ratio of the total weight (solids and water) to the totalvolume. Bulk density values are used to convert weight to volume for materialshandling calculations. The sample is compacted, as received, using standardproctor compaction energy in accordance with ASTM D 698. The bulk density isthen determined in accordance with ASTM D 2937.The Bulk Specific Gravity is simply the density of the as-received material (i.e,bulk density) relative to the density of water.

4.2.3 Treatability MethodologiesAll treatability methodologies will be performed by Kiber and includesolidification/stabilization treatment, curing, organic emissions and temperaturemonitoring, penetrometer strength, and volumetric expansion. These measurements ortreatment technologies are non-routine analyses and are developed on a project and wastespecific basis. The procedures to be implemented for each phase are included in the

000173


scope of work presented in Section 1 .5 .3.

4.3 CALIBRATION PROCEDURES AND FREQUENCY

The primary objectives of the QA program for the Southern Shipbuilding treatabilitystudy is to validate the quality of each measurement and treatment evaluation, and toevaluate the effectiveness or variability of the solidification/stabilization treatmenttechnology for the contaminated soils and sludges. The objectives are achieved through1) calibration of the associated equipment, and 2) supervision and review by qualifiedtechnical personnel. The remaining discussions provide an overview of calibrationpolicy for the general laboratory equipment. Any calibration protocols specific to aparticular test method are discussed in the SOPs presented in Appendix A.

Kiber's QA/QC practices include regular calibrations of all general equipment. The QCprogram includes regular professional calibration of equipment as determined necessaryby the QA/QC Manager, Project Manager, or manufacturer-developed specifications ofall equipment. Calibrations records are maintained which can be traced to the NationalInstitute of Standards and Technology (MIST). All equipment associated with the UCStesting is calibrated on an annual basis by the manufacturer, in accordance with Kiber'smaintenance plans. Laboratory balances are calibrated on a 6 month basis; however, thebalances are checked daily using a three-point range of calibration weights.Thermometers and thermocouples are calibrated every 6 months versus an NIST-traceable thermometer at a minimum of two temperatures. Laboratory ovens andrefrigerated storage facilities are monitored and recorded daily to ensure that a constantand acceptable temperature is maintained. The temperatures are verified on a weeklybasis using calibrated digital thermometers.

The pH meter is calibrated on a daily basis using a two-point calibration method asrecommended by the manufacturer. If acceptable tolerances cannot be achieved, the pHmeter is returned to the manufacturer for further service and calibration. Organicemission will be monitored using a photoionization detector (PID) manufactured by HNuModel PI-101. The PID will be serviced by a manufacturer-authorized servicerepresentative prior to initiation of the treatability study. The accuracy of the PID meter

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1Southern Shipbuilding Corporation SiteQuality Assurance Project PlanRevision No. 117 October 1994Page 39

will be assessed by the daily verification and calibration with isobutylene, a standardreference gas.

All data and calculations are checked by a secondary source, preferably an individual notinvolved with the testing, and then by QA personnel to ensure that no errors are included.In addition, testing is supervised by personnel experienced in both laboratory evaluationsand full-scale application of the solidification/stabilization technology.

Again, specific calibration protocols required for each individual analysis aresummarized in the SOPs presented in Appendix A.

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5.0 DATA REDUCTION, VALIDATION AND REPORTING

5.1 STANDARD RECORD MAINTENANCE

This section summarizes the types of bound log books maintained by Kiber's treatabilityand/or analytical personnel:

Daily Log - A bound document of all laboratory activities; equipmentmaintenance, chemists/scientists that are working in the laboratory, samplesreceived, testing performed; problems encountered and solutions found; and QCsample preparation. This log is maintained on a daily basis by the laboratorypersonnel involved with the testing.QA/QC Log - A bound laboratory log book recording all QC data and results forall samples analyzed.Extraction Log - A bound laboratory log book recording all samples and theextraction method used, including the extraction date, sample and run number,initial and final volumes, matrix, and cleanup procedures.Standards Log - A bound laboratory log book for recording manufacturer's lotnumbers, preparation procedures, and preparation date for all standards used inthe laboratory.Data Spreadsheets - Individual spreadsheets used in raw data calculations.These are kept in files separated by day along with supporting documentation.Most data outputs are generated through computer systems that have beenvalidated by the appropriate task manager and reviewed by the QA/QC Manager.

5.2 LABORATORY DATA VALIDATION

All data generated within the treatability laboratory is extensively checked for accuracyand completeness. The data validation process consists of data generation, reduction, andthree levels of review. The chemist/scientist who generates the raw data has the primeresponsibility for correctness and completeness of the data. All data generated and

000176


reduced follows protocols specified in each SOP. Each analyst reviews the quality of hiswork based on the following set of guidelines:

1. Verify informal chain of custody2. Sample preparation and log information is correct and complete3. Study information is correct and complete4. The appropriate SOPs have been followed5. Analytical results are correct and complete6. QC samples are within appropriate QC limits7. Special sample preparation has been met8. Documentation is complete

The next level of review is performed by the QA/QC Manager and the Task Manager forthis project. The review is structured to ensure that:

1. QC samples are within established limits2. Quantitative results are correct '3. Documentation is complete4. The data is ready for incorporation into the final report5. The data is complete and ready for data archive6. Calculations are reviewed and confirmed7. Obvious or anomalous data are investigated and clearly documented

The final level of review by the laboratory comes from the Project Manager. The ProjectManager reviews the reports to ensure that the data meets the overall objectives of theproject. All logs and chain of custody records-are checked by the Project Manager.

5.3 DATA REPORTING

Once the data has been validated, the results can be used to evaluate the potentialeffectiveness of solidification/stabilization treatment and included hi the final treatability

000177


study report. The report will follow closely the guidelines presented in the document"Guideline to Conducting Treatability Studies Under CERCLA." The report will containthe following:

1. Original chain-of-custody forms2. Description of sample types3. Tests performed, problems encountered during testing4. Dates sampled5. Date received6. Date the study was conducted7. Study results8. QC information, including:

- Relative percent difference- Any other special QC information

9. Methodology10. Conclusions and recommendations as to the effectiveness of solidification/

stabilization as a remedial alternative for the Southern Shipbuilding site

All data is entered and checked by the project personnel. The hard copy report ischecked by the Task Manager, and approved by the Project Manager before sufamittal.Prior to submittal to the U.S. EPA, all submittals generated by Kiber will be reviewed byPRC. Data reports will be turned over to the Kiber Project Manager and released to therespective clients and/or governmental agencies requesting copies.

5.4 DATA STORAGE

Typically, all documentation used and generated for a treatability study is turned over tothe Project Manager at the completion of a project. All log books, spreadsheets andsupport documentation are then archived. The final report is usually generated by use ofcomputer. A back-up copy of the report on diskette is filed and sent off-site to secure,fire-protected storage facility. All information under the corresponding project number ismaintained in the archive system for five years. All archives are accessed by the archivesfile master list which is maintained in a separate location from the archives.

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6.0 INTERNAL QUALITY CONTROL CHECKS

The primary objective of the QAPP is to assure that the laboratory generates data ofknown quality, that achieves the QA/QC criteria, and that records necessary to documentlaboratory performance are maintained. Quality assurance oversight is performedthroughout the sample process from initial sampling, through treatability and analyticalsystems, to the final report. The QA/QC manager and project manager for each party isresponsible for monitoring compliance of the QAPP. The QA program presented isintended to safeguard against deficiencies during all aspects of the treatability study.

The treatability and physical properties measurements are performed to evaluate theeffectiveness and/or variability of the solidification/stabilization treatment on thechemical and physical characteristics of the waste materials. Experience indicates thatwaste materials similar to those at the Southern Shipbuilding site exhibit considerablevariability; therefore, duplicate analyses have been specified for the untreated chemicaland physical characterizations. These duplicate analyses will better ensure the quality ofthe data and the representativeness of the data. All non-critical physical and chemicalmeasurements will be assessed through the performance of duplicate testing, except forthe UCS tests. There are no standard materials that can be used to determine theaccuracy of the UCS test, because the test involves a simple application of steadilyincreasing known pressures to a standard-sized cylindrical sample until the sample failsor is deformed to 15 percent of its original size. The UCS test simply determines themaximum load, or pressure that can be placed upon a given material type. The UCS testis being performed only to provide additional qualitative information pertaining theeffectiveness of solidification/stabilization treatment using candidate treatment processes.The testing will be performed as non-critical testing with DQO Level I. Because it isimpossible to re-analyze, corrective action and data review and usage will involve anassessment of the data generated and a visual evaluation of the material by experiencedpersonnel.

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A preliminary discussion of the quality control samples associated with the criticalSVOC analyses has been presented in Section 2.2. Detailed protocols for each analysisare included in the SOPs presented in Appendix A. In general, the QC samples willinclude the following:

DuplicatesMatrix Spikes / Matrix Spike Duplicates _Extraction BlanksExtraction Blank SpikesTCLP Extraction BlanksSurrogate Recoveries

A detailed presentation of the acceptance criteria for each are included within the SOPspresented in Appendix A.

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7.0 PERFORMANCE AND SYSTEM AUDITS

An audit is defined as a systematic check to determine the quality of operation oflaboratory activities. The purpose of conducting audits is to monitor and verifycompliance of the testing program with the protocols presented in the QAPP. The auditsgenerally include a detailed review of each operating component of the network.Communication of audit findings to management is required for timely consideration andimplementation of corrective actions.

The laboratory system audit is a review of laboratory operations conducted to verify thatthe facility maintains the necessary equipment, staff, and procedures required to generateacceptable data. Also, an audit serves as a determination that each element within anactivity is functioning appropriately and within the guidelines established by theappropriate methodology, approved procedures, and this QAPP.

System audits of laboratory activities are accomplished by an inspection of all laboratoryactivities by the QA/QC Manager. Internal audits are planned and conducted inaccordance with a schedule developed by the QA/QC Manager. Unscheduled audits orsurveillances are also conducted as necessary. This audit is composed of a comparisonbetween current practices and standard procedures. The following is a list of criteria tobe used in the evaluation of laboratory activities:

1. Organization and responsibilities - Determine whether the qualityassurance organization is operational.

2. Collection of samples - Ensure that written procedures are available andare being followed.

3. Chain-of-custody program - Ensure that the appropriate steps have beenfollowed in the traceability of sample origin.

4. Implementation of the operational procedures - Ensure that the appropriateQC checks are being made and records are maintained of these checks.

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5. Equipment - Determine whether the specified equipment is available,calibrated, and in proper working order.

6. Training - Ensure that personnel conducting the treatability study areadequately trained.

7. Records - Ensure that recordkeeping procedures are operational and thatfield notebooks, log sheets, bench.scale sheets, and tracking forms areproperly prepared and maintained.

Laboratory system audits often include analysis of blind samples, split samples,additional quality control samples, standardized performance evaluation samples, andadditional blank spikes. Performance evaluation samples are routinely provided byexternal professional organizations.

Kiber's laboratories participate in Wastewater Pollution (WP) studies conducted by theU.S. EPA each year. Results of these audits, or other U.S. EPA audits or otherperformance evaluation studies are available for review.

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8.0 CALCULATION OF DATA QUALITY INDICATORS

8.1 OVERVIEW

Laboratory results will be assessed for compliance with required precision, accuracy,completeness, and sensitivity. The targets for each of these parameters were presentedon Table 2-1 . The following presents the calculations required for each of theseparameters.

8.2 PRECISION

Precision of laboratory analyses will be assessed by comparing the analytical resultsbetween matrix spike and matrix spike duplicates for the S VOC analyses, and laboratoryduplicates for the non-critical analyses. The relative percent difference (RPD) will becalculated for each pair of duplicate analyses using the following equation:

RPD = (S-D)/ {(S+D)/2}*100

where, S = First sample value (original or MS value)D = Second sample value (duplicate or MSD value)

8.3 ACCURACY

Accuracy of laboratory results will be assessed for compliance with the established QCcriteria using the analytical results of method blanks, reagent/preparation blanks, matrixspikes, and matrix spike duplicates. The percent recovery (R) of matrix spike sampleswill be calculated using the following equation:

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Southern Shipbuilding Corporation SiteQualify Assurance Project PlanRevision No. 117 October 1994Page 48

R= (A-B)/C*100

where, A = The analyte concentration determined experimentally from thespiked sample.

B = The background level determined by a separate analysis of theunspiked sample. -;..

C = The amount of spike added.

8.4 COMPLETENESS

The data completeness of laboratory analyses results will be assessed for compliancewith the amount of data required for decision-making in remedy screening. Thecompleteness is calculated using the following equation:

Completeness = (Valid Data Obtained )/(Total Data Planned)* 100

8.5 SENSITIVITY

The achievement of method detection limits depends on instrumental sensitivity andmatrix effects. Therefore, it is important to monitor the instrumental sensitivity to ensurethe data quality through constant instrument performance. The instrumental sensitivitywill be monitored through analysis of method blanks, calibration check samples,laboratory control samples, and detection limit studies.

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1Southern Shipbuilding Corporation SiteQuality Assurance Project PlanRevision No. 117 October 1994Page 49

9.0 CORRECTIVE ACTION

9.1 TREATABILITY CORRECTIVE ACTION

The results of the following Quality Assurance activities may initiate a corrective action:

1. Internal and external performance audits2. Systems audits3. Inter-laboratory comparison study4. Failure to adhere to Quality Assurance Plan5. Failure to adhere to standard operating procedure

A detailed discussion of the laboratories corrective action procedures are presented in thecorresponding standard operating procedure presented in Appendix A. The followingdiscussions present an overview of these procedures. Upon notification of a problem orwhen a potential problem is identified and documented, the Project Manager notifies theQA/QC Manager. The client will then be notified and asked for their recommendations.At this time, a thorough investigation of the reported problem is immediately performedto determine if corrective action should be initiated. The problem is reviewed with theQA/QC Manager. Corrective actions will be initiated by treatability laboratorypersonnel, as well as the QA/QC Manager. The Task Manager for treatability testing willbe responsible for approving the corrective action and will call upon the QA/QCManager to ensure the corrective action is carried out. Follow-up procedures for eithercase will not be considered complete until the problem has been effectively andpermanently solved. These procedures will consist of, but not be limited to, thefollowing:

1. Determining when the problem occurred and which systems were affectedby the problem.

2. Assigning responsibility and time schedule for implementing thecorrective action.

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3.

4.


Determining the desired effectiveness and implementability of thecorrective action.Verifying and documenting that the corrective action has eliminated theproblem.

The Treatability Task Manager has the authority to require that all measurementsthreatened by the problem be stopped or limited until the corrective action is complete.The QA/QC Manager also has the authority to order a new study to be initiated after thecorrective action is complete. Formal notification to laboratory management, the QA/QCManager, and incorporation into the project file will be the ultimate disposition of anycorrective action.

If, during system or performance audits, weaknesses or problems are uncovered,corrective action will be initiated immediately.

Whenever a long-term corrective action is necessary to eliminate the cause of non-conformance, the following closed-loop corrective-action system will be implemented.As appropriate, the Kiber project scientist, QA/QC Manager, Task Manager, and ProjectManager will ensure that each of these steps is followed:

1. The problem will be defined.2. Responsibility for investigating the problem will be assigned.3. The cause of the problem will be investigated and determined.4. A corrective action to eliminate the problem will be determined.5. Responsibility for implementing the corrective action will be assigned and

accepted.6. The effectiveness of the corrective action will be established and the

correction implemented.7. The fact that the corrective action has eliminated the problem will be

verified.

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9.2 ANALYTICAL LABORATORY CORRECTIVE ACTION

When non-conformance occurs, analysts should notify the Task Manager immediately.The Task Manager and the QA/QC Manager will evaluate the problem and decide whatcorrective action is required. Once a non-conformance is identified, a corrective actionform (CAP) is issued in order to document the deficiency and track the corrective action.The CAP is issued by the QA/QC Manager to th£ responsible Task Manager. A copy ofthe CAP is maintained in the QA files. The following guidelines are used to validatedata, and determine what, if any, corrective action is necessary.

1. Verify all calculations which use raw laboratory data, including samplealiquots, dilution factors, linear regression calculations, etc.

2. Verify that method specific matrix interference procedures were followed.3. Review the analytical procedure with the analyst to make certain that the

required procedures and sample preparation techniques were performedcorrectly.

4. Check the initial calibration data to verify that instrumental operatingrequirements were met prior to starting sample analysis.

5. Verify that quality control sample checks were analyzed at the properfrequency and that quality control sample performance criteriarequirements were met.

6. Determine if an alternative method would have been more appropriate forsample analysis.

7. Review log-in and chain-of-custody information to determine if sampleconditions may have been affected between sampling and receipt ofsample.

When a definitive explanation for the problem cannot be determined, sample reanalysis isrequired. All non-conformance and corrective action procedures taken to correct theproblem must be documented and included with the project files. If the non-conformance

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has not been corrected and the validity of the data is in question, the Project Managermust contact the client. All client contact should be documented and included in the jobfile.

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10.0 QUALITY ASSURANCE REPORTS TO MANAGEMENT

Kiber's Task Manager, the Project Manager and the QA/QC Manager willregular basis to ensure that all QA/QC practices-are being carried out and

converse on aregular basis to ensure that all QA/QC practices^re being carried out and to reviewpossible or potential problem areas. It is important that all data abnormalities beinvestigated to ensure that they are not a result of operator or equipment deviation, butare a true reflection of the methodology or task function. External reporting for theare a true lenecuon 01 me iiiemuuoiugy ui UISK. uuiuuun. rproject final report, prepared for the Southern Shipbuilding project, will contain aseparate section that covers the data quality and validity, and will be made available tothe client. At a minimum, the following information will be included in the report:

1. Title Page / Table of Contents.2. Performance audits will include: date, parameters and systems tested,

person performing audit, reported results, summary of any problems thatoccurred, and corrective action taken.

3. System audits will include: date and agency performing audit, system andparameters tested, results of tests, parameters for which results wereunacceptable and an explanation of these results.

4. Copies of documentation such as memos or reports will be included asapplicable.

5. Significant QA/QC problems, including: identifying the problem,identifying the individual who reported the problem, source of problemand corrective actions that need to be taken.

QA reports will be included with the final report.. In addition, a monthly report will besubmitted which will include any QA reports. Verbal reports will be made on a morefrequent basis. If no project audits are performed for that particular project, and nosignificant QA/QC problems occur, a letter stating these facts will be submitted to thereferenced parties in lieu of a QA Report.

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3.4 SOIL WASHING TREATABILITY STUDY

3.4.1 Introduction

During the identification and classification of OUs at the SSC facility in Slidell, Louisiana, contaminatedsoils and sediments were identified that are candidates for treatment using the separation technology, soilwashing. Soil washing is a physical/chemical treatment technology which utilizes washing fluids tofacilitate the transfer of contaminants from the soils/sediments to the wash fluids or to a concentrate thesmaller grain size fraction where most contaminants are present. The resulting chemical concentrate(either the washing fluid or particulate fraction) can then befiirther treated to destroy or permanentlystabilize the contaminant matrix.

Soil washing is a proven technology which is capable of treating both organic and metal contaminantswith a soil/sediment matrix. The technology is capable of handling large volumes of contaminatedmaterial and has been applied at numerous NPL sites by the EPA with success as described in InnovativeTreatment Technologies: Annual Status Report (Fifth Edition), EPA/542/R-93/003, September 1993.

The soil washing remedy screening treatability study will be performed by Ecology and Environment,Inc. (E & E) in the treatability facility in Buffalo, New York. The study will be conducted accordingto "Screening Protocol for Evaluating Soil Washing Potential of Contaminated Soils" provided by theRisk Reduction Engineering Laboratory (RREL) hi Cincinnati, Ohio.

3.4.2 Site Characteristics and Process Description

3.4.2.1 Site Characteristics

Two of the five matrices to be addressed under this EE/CA and CD, have materials which couldpotentially be addressed with a soil washing pre-treatment technology: lagoon sediments (oily solids) andsandy soils. Depending on the results of the field investigation, a decision will be made concerning theapplicability of soil washing techniques to these two matrices.

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The sandy soils matrix is includes berm material, naturally occurring sand deposits associated with theproperty, and imported sand utilized for roads, fill, sand blasting, and other site activities. The lagoonsediment sample will be collected neat the bottom of the impoundment and will consist of soil and clay.The soil to be used is a coarse sand, believed to be deposited by barge cleaning and sand blastingoperations. This sample will be obtained adjacent to the north impoundment. The second sample to betested will be more of a silty clay and will be collected from the south impoundment.

The contamination associated with the waste consists mainly of volatile organics, semi-volatile organics(predominantly PAHs), and metals. This contaminant suite has been successfully treated at other NPLsites. The final disposition of the cleaned sediments will Be made in accordance with accepted siteARARs and TBCs.

3.4.2.2 Process Description

Soil washing remedy screening treatability design considerations are driven by the contaminants present,the grain size distribution of the soils/sediments, anticipated removal action levels and the total projectedvolume of soils to be treated.

Characterization of each operable unit with regard to information important to the application of thistechnology is being collected and is addressed in the EE/CA and CD work plan QASP.

The protocol used was developed by the EPA Risk Reduction Engineering Laboratory. This protocolsuggests that the Remedial Project Manager (RPM) or specify the wash solution to be used in the study.Since the EE/CA is being conducted as a non-tune critical removal, the On-Scene Coordinator (OSC) hasdiffered the recommendations to the treatability contractor. A several surfactant solutions will bescreened to evaluate which one causes the greatest removal of contaminant from the soil matrix.

The contamination to be targeted are the polycyclic aromatic hydrocarbons (PAHs). Focusing on thisclass of compounds rather than all semivolatile compounds, greatly reduce the analytic costs involved hithe study.

Total Recoverable Petroleum Hydrocarbons (TRPH) will also be analyzed as they provide a goodindicator of total petroleum content.

000191

The pages that follow are the laboratory protocol by which the soil washing treatability will be conducted.Table 3.4-1 presents a summary of analytic testing to be performed on the resultant products of the soilwashing process.

3.4.2.3 Quality Assurance/Quality Control

E & E will implement established quality assurance and quality control practices to permit the evaluationof the removal efficiency and reproducability of the test results. EPA guidance has suggested QualityControl (QC) procedures including:

1. Triplicate samples of both reactor and controls;2. The analysis of surrogate spike compounds in each sample;3. The extraction and analysis of a method blank with each set of samples; and,4. The analysis of a matrix spike in approximately 10 percent of the samples.

As indicated in the EPA guidance, the analysis of triplicate samples provides for the overall precisionmeasurements that are necessary to determine whether the difference is significant at the chosenconfidence level. The analysis of the surrogate spike will determine if the analytical method performanceis consistent. The method blank will determine if laboratory contamination has effected the results.

3.4.2.4 References

U. S. Environmental Protection Agency. Engineering Bulletin - Soil Washing Treatment, EPA/540/2-90/017, September, 1990.

U. S. Environmental Protection Agency. Guide for Conducting Treatability Studies under CERCLA(Final) EPA/540/R-92/071 October 1992.

U. S. Environmental Protection Agency. Guide for Conducting Treatability Studies under CERCLA:Soil Washing, EPA/540/2-91/020B, September 1991

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Soil Washing ProtocolRevision: 1

Date: 3/17/94

SCREENING PROTOCOL FOR EVALUATING SOIL WASHINGPOTENTIAL OF CONTAMINATED SOILS

By

University of CincinnatiDepartment of Civil & Environmental Engineering

Center Hill FacilityCincinnati, Ohio 45224

Contract 08-09-0031 WA #3-9

Work Assignment ManagerEugene Harris

RISK REDUCTION ENGINEERING LABORATORYOFFICE OF RESEARCH AND DEVELOPMENTUS ENVIRONMENTAL PROTECTION AGENCY

CINCINNATI, OHIO 45219

March 1993

This document was duplicated exactly from a facsimile provided by the Agency above.

06:WPUZD:Zn061_DTOO«_SOIL_WASHING_PROTOCOM)9/26/94-Dl

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Date: 3/17/94

CONTENTS1. Test Purpose2. Limitations3. Cautions and Warnings4. Reference Documents and Procedures5. Reagents and Supplies6. Test Equipment7. Calibration of Equipment8. Sample Characteristic Requirements9. Test Sample Preparation10. Test Procedure11. Calculation/Data Reduction12. Data Reporting13. Waste/Decontamination14. Cost ProjectionAppendix A Physical/Chemical Measurement MethodsAppendix B ASTM Procedures

Page33344566789101010

06:WPUZD:ZT2061 DTOMO SOIL WASHING PROTOCQL-09/2&94-D1

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Date: 3/17/941. Test Purpose

This laboratory-scale screening protocol is to determine the potential applicability ofthe soil washing technology for remediation purposes.1.1 This test procedure describes washing of contaminated soils with specified

reagents and equipment under standard operating conditions. Contaminantconcentration in the washed soil and the resulting washing liquid indicate thepotential of removing the contaminants from the soil by washing.

1.2 Separation of the soil, prior to washing, into preselected fraction concentrates thecontaminants into specific size fractions.

1.3 The qualitative nature of information obtained from this procedure is used todetermine whether further testing of this technology, for example bench scalestudy should be pursued.

2. Limitations2.1 Tests are carried out at atmospheric pressure and at temperatures not exceeding

150°F. These tests only show the potential application of the technology for thesite under consideration. For design purposes, bench and pilot scale studies arenecessary.

Note: DI water is used for both wash solution preparation and rinsing of soil.2.2 This screening protocol does not provide either a procedure for the selection of

appropriate washing liquids or their compositions.2.3 The identities and concentrations of contaminants of interest present in the soil

should be provided by the RPM.3. Supplied Information

The following information and material is needed along with the request for screeningtest• The identities and concentrations of contaminants of interest present

in the soil• Representative disturbed soil of at least 2 kg.

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Date: 3/17/944. Cautions and Warnings

• This protocol may involve hazardous materials, operations, andequipment. This standard does not purport to address all of thesafety problems associated with its use. It is the responsibility of theuser of this standards to establish appropriate safety and healthpractices and determined the applicability of regulatory limitationsprior to use.

• EPA regulations for shipping containers, methods of preservation,and storage of the sample need to be scrupulously observed (49 CFRSubchapter C, Parts 100-199).

• Shipping regulations provide some information as to the chemicalcomposition of the sample. For example, whether the sample con-tains acute toxic compounds such as dioxins, PCBs, etc.

• When receiving shipment of soils and samples from the field, ob-serve whether sample labels, seals, and chain of custody records arein order.

• Note whether proper containers and preservation methods (AppendixA) have been observed and the shipping container is at propertemperature.

• Identity (Identities) and concentrations) of the contaminants) presentin the soil sample(s) should be provided by the shipper.

• Mention of trade names or commercial products does not constituteendorsement or recommendation for use.

5. Reference Documents and Procedures5.1 Documents• ASTM D421 - Practice for Dry Preparation of Soil Samples for

Particle Size Analysis and Determination of Soil Constants• ASTM D2216 - Standard Method for Laboratory Determination of

Water (Moisture) Content of Soil, Rock, and Soil - AggregateMixtures

• ASTM Ell-Sieve Specifications• 49 CFR Subchapter C. Parts 100 through 199 - The Hazardous

Materials Regulations

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Date: 3/17/94• 40 CFR 261 4(1) - Samples Undergoing Treatability Studies at

Laboratories and Testing Facilities.5.2 Physical/Chemical Measurements MethodsAll physical, chemical measurement methods are from USEPA SW-846 - TestMethods for Evaluating Solid Waste and are listed in Appendix A.

6. Reagents and SuppliesReagents and supplies necessary for the screening of one soil hi triplicate:• 1 Aggregate scoop pan with tapered design to transfer soil into

splitter, sieves, graduated cylinders, and jars. Soiltest model CL-292or equivalent

• 2 Appropriate container with spigot for storing wash and rinse fluids.Two gallon (8 L) capacity. Fisher model 02-963-6A or equivalent.

• 2 Washing bottles (500 ml) for washing/rinsing of soil. Fishermodels 03-409-10E or equivalent.

• 1 Each graduated cylinders, 1L, 500 ml, 250 ml capacity for themeasurement of liquids.

• 3 1.5 L heavy duty graduated pyrex beakers.• 18 Wide mouth glass sample bottles (4 oz., 144 ml) with teflon lined

screw caps for analysis of organic and inorganic contaminants insoils and for inorganic contaminants in liquids.

• 12 Boresilicate glass vials (40 ml capacity) with black phenolic teflonlined screw cap for organic contaminants in liquids.

• 3 Rubber policemen/scrapers with angled or wing-shaped edge toscrape solids from beakers, sieves, etc. Fisher model 14-105A orequivalent.

• 3 Buchner funnels with fixed perforated filter plate (25 cm diameter)with glass filtering flask (100 ml capacity) with tabulation.

• 1 box filter paper suitable for Buchner funnel filtration. Particle sizeretention up to 2.5 /am and good wet strength (Whatman #5 orequivalent).

• 1 Mercury thermometer from 20 to 150°C with 1/5°C subdivisionprecision grade. Fisher model 15-043C or equivalent.

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Date: 3/17/94• 1 Stop watch or timer (digital with alarms) capable of measuring time

in seconds.• 2 Wide mouth glass or plastic funnels for pouring the soil slurry into

filtering device.• 1 bottle each standard buffer solutions pH 4, 7, and 10.• 6 Aluminum weighing dishes, 300 ml to 500 ml capacity.• 2 Heavy-duty canvas or plastic sheets (1.5 m X 1 m: 5 ft. X 3 ft.).• 2 Trowels. Soiltest model CN-840 or equivalent.• 1 Hydrometer. Soiltest model CL-277 or equivalent.• 1 Pycnometer.• 1 box. Phosphate free laboratory detergent.• 1 5-gallon pail with lid.• 1 roll, Aluminum foil.• 2 55-gallon disposal drums.

7. Test Equipment• 1 Top loading balance, readability 0.1 g; reproducibility ± 0.1 g;

and linearity ± 0. Ig. Capacity 4 kg.• 1 Set of National Institute of Science and Technology (NIST) Class F

standard weights, 500 mg., Ig., 2g., 5g., lOOg., 200g., 500g., 1 kg.and 2 kg.

• 3 Sets of screening sieves (US Standard per ASTM EM) with pans(204 mm, 8 inch diameter) each set containing following:

No. 10 (2 mm)No. 60 (250 mm)No. 80 (180 mm)No. 200 (75 mm)

• 3 204 mm (8 inch) diameter pans.• 1 Sieve shaker with timer. Tyler Ro-Tap sieve shaker or equivalent.

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Date: 3/17/94• 1 Mechanical sand equivalent shaker. Soiltest model CL-232C or

equivalent.• 1 Drying oven., forced air, automatic temperature control (accuracy

± 5°C) from ambient to at least 150°C. Two cubic feet capacity.• 1 pH meter with glass electrode, accuracy ± 0.05 pH. 0-14 pH .

range.• 1 Standard single head vacuum pump or aspirator filter pumps.

Fisher model 13-875-220 or equivalent.• 1 Sample splitter (riffle) with 14 chutes, 13 mm (1/2 inch) wide.

Soiltest model CL-280 or equivalent.8. Calibration of Equipment

Record and calibration data in laboratory note book used for the screening study.Balance Calibrate the top loading balance using NIST Class F weights. For small weights

(e.g., filter paper), calibrate the balance using 500 mg. 1 g. 2 g. and 5 g. Forlarge weights (e.g., sieves), calibrate the balance using 100 g. 200g. 500 g. and 1kg. Balances are checked monthly and recalibrated or serviced, if needed.

pH meter Calibrate the pH meter, after washing the electrodes thoroughly with distilledwater using the three buffer solutions, pH 40., 7.0, and 10.0. Follow theinstructions supplied with the instrument and electrode. Keep the pH electrodesoaked in either distilled water or in the pH buffer 4.0 when not in use.

Oven Checked whether the temperature controller of the oven is working properly. Thetemperature should be within ± 5°C of the setting.

9. Sample Characterization RequirementsThis test requires 1.5 kg of soil sample passing through 3/8" sieve to conduct each set of testsin triplicate.- The soil sample shipped to the laboratory should be in airtight containers to preserve theoriginal moisture content.- Chemical composition of the soil, even when available from the shipper, should beconfirmed by the laboratory performing the screening test.1.0 Test Sample and Wash Solutions PreparationRecord all data in the laboratory note book.

06:WPUZD:ZT2061 DT0040 SOIL WASHING PROTQCOL-09/2«94-DI

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Date: 3/17/9410.1 Well mix the 1.5 kg of soil by shaking and tumbling in a 5 gallon pail fitted with a

lid.10.2 Pour the content of the pail on a clean heavy-duty quartering canvas.

Remove (hand picking) all large (6.4 mm or 0.25 in) gravel and stones and all otherforeign materials. For example, pieces of cloth, plastics, tree parts, and other debris.Place all rejects in the disposal drum.Determine the weight of the debris-free soil

10.3 A procedure similar to ASTM D2216 is used for moisture content determination asfollows:• Weigh close to 300 g of the debris-free soil with an accuracy of ± 1

g, in a preweighed aluminum weighing dish and dry at 110+5°C inthe oven overnight to constant weight (< 5% weight change)

• Record the weights of the sample before and after drying.• Determine the moisture content of the soil as follows.• % moisture content = wt. of wet soil - wt. of dry soil X 100

wt. of dry soil10.4 Sieve the debris-free soil through a 3/8" sieve

Collect all soil passing through the 3/8" sieveWeigh on the top loading balanceRecord the weight

10.5 Riffle the screened sample (ASTM D4210 close to 1000 gReserve 50 g for chemical analysis of contaminants of interest.Note: If the soil characteristics prevent screening through the 3/8" screen, follow. Step 10.6 instead of Steps 10.4 and 10.5.

10.6 Pour the debris-free soil (from Step 10.2) on a clean quartering canvas and reduce thevolume of the soil sample weighing approximately 1000 g, using a clean trowel.

10.7 Prepare 1.8 L of the wash solution according to the direction provided by RPM.Store in appropriate container.

06:WPUZD:Zr2061jyrQQ40_SOIL_WASHING_PROTOCOL-09/26/94-Dl 8

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Date: 3/17/94Record the pH of the wash solution.

10.8 Store rinse fluid in a separate container (generally Dl water).11. Test ProcedurePreliminary Density Separation should be performed on samples containing large pieces ofcontaminant in order to make the sample homogeneous.11 .1 Laboratory Scale Soil Washing

The attached flow diagram (Figure 1) summarized the laboratory scale soil washingprotocol. These screening tests are carried out in triplicate and in sequence.1 1 . 1 . 1 Thoroughly clean the sieves using a phosphate free laboratory detergent

followed by distilled water.Make sure that no solids remain adhered to the screens.Dry the screens to constant weight at 110±5°C.Record the weights of each screen and mark the screens for identification.Note: Special precautions should be taken when using corrosiveliquidsforexample, acidic, basic, or highly concentrated salt solutions. Incase of corrosive liquid, it may be necessary to use sieves made of eitherstainless steel or polyethylene instead of brass.Note: Do not force lodged soil particles through the screen either by aspatula or brush or water stream. Place the screen upside down in the sinkand then pour water over the screen to dislodge any soil particles from thescreen.

11 .1 .2 Weigh with an accuracy of ±0.1 g of the well mixed, air dried, andrepresentative soil (from Step 10.5 or 10.6), close to 200 g in an aluminumdish.

1 1 . 1 .3 Stack the three sets of marked sieves and the collection pans in the ordershown in Figure 1.Place the whole assembly securely on the shaker.

11 .1 .4 Transfer the weighed soil from the weighing dish to the top sieve.11 . 1 .5 Using a sieve shaker, shake the sample for at least 10 min. to separate the

soil into the fractions.

06:WPUZD:ZT2061 DT0040 SOIL WASHING PROTOCOL-09/26#4-Dl

000201


Date: 3/17/9411 . 1 .6 Weigh the sieve and sample with aluminum foil underneath.1 1 . 1 .7 Determine weight of sample/sieve.1 1 . 1 .8 Measure wash solution using a graduated cylinder (normal soil/wash

solution 1.6 (w/v)).11 . 1 .9 Place on a vibrating table and shake for 2 hours at low speed.

Allow the sample to settle, followingjhe 2 hours, for 10 minutes.1 1 . 1 . 10 Weigh a filter paper.

Filter sample using Millipore filtering system or equivalent.1 1 . 1 . 1 1 Place a new clean container under filter and rinse sample with 100 ml DI

water.1 1 . 1 . 12 Measure and record total volume of each of the wash and rinse water.

Weigh and record the wet sample on the filter paper.1 1 . 1 . 13 Dry the soil and filter paper to a constant weigh at 110°C and record

weight.Difference between dry and wt weight is the weight of rinse water attachedto sample.

1 1 . 1 . 14 Submit wash solution, sample, and rinse water for analysis of targetcontaminants.

1 1 . 1 . 15 Decontaminate all equipment and glassware by washing with a phosphatefree laboratory detergent and then rinsing with Dl water.Store all the washings in the disposal drum.

1 1 . 1 . 16 Analyze all samples as soon as possible.Consult USEPA SW-846 guidelines for sample preservation technique,holding time, and analytical procedures (Appendix A).

12. Calculation/Data Reduction12.1 Soil Washing

06:WPU2D:ZT2061_DT0040_SOIL_WASHING_PROTC)COW)9/26/94-Dl 10

000202

SOIL WASHING TREATABIUTY STUDY SCHEMATICSOUTHERN SHIPBUILDING CORPORATION

# 10SOIL

DRY SOIL(200g)

SIEVE #10SIEVE #60SIEVE #80

SIEVE #200PAN

#60SOIL

RINSE

#I200\

/WASH\'SOL'N 1

#80SOIL

#200SOIL

FIGURE 1

SOURCE: SCREENING PROTOCOL FOR EVALUATING SOIL WASHING POTENTIALOF CONTAMINATED SOILS, MARCH, 1993, USEPA-ORD-RREL

000203

Table 3.4-1SOIL WASHING TREATABELITY STUDY

SUMMARY OF ANALYTIC TESTINGSouthern Shipbuilding Corporation

Operation

Initial Sample AnalysisWash Solution PretestsSoil Washing Solution/Sample #1Soil Washing Solution/Sample #2TOTAL ANALYSES

Total RecoverablePetroleum Hydrocarbons

(EPA Method 418.1)310'452

45103

Semivolatile Compounds(EPA Method 8310)

•i 3-454593

1 Five wash solutions x two duplicates2 Five sieve sizes x wash, rinse, soil x three replicates

000204


Date: 3/17/9412.1 .1 Record the volumes of wash and rinse solutions for each

sieve during the particle separation process.12.1.2 Calculate moisture contents of initial sample to determine dry

weights.12.1.3 Record the dry weight (g) of soil retained on each sieve.12.1.4. Calculate the mass of contaminant (jig) in sample, wash, and

rinse solutions by multiplying concentration obtained fromanalysis (/tg/g or jttg/ml) by the weight retained (g) on eachsieve.

12.1.5 Total mass (/ig) of sample, wash, and rinse solutions for eachsieve to determine the percent removed.

NOTE: Due to small sample size and number, the mass balance maynot be 100%.

13. Data Reporting13.1

13.2

Initial concentrations in the soil are determined through analysis. Thesevalues are used to determine the percent removal of the contaminant whencompared to final concentrations.Concentrations of the contaminants) in bulk soil and in the washed soilfractions are displayed in tabular form.

13.3 Report the results based on mass balance.14. Waste/Decontamination

The entire sample generated from the testing protocol is either submitted for analysisto the analytical laboratory or archived. All excess wash solutions, rinse solutions, orsoil as well as wash water used to clean any excess solids from any laboratoryequipment shall be placed in a properly labeled 5 gallon bucket for subsequentdisposal.All remaining wastes are either returned to the site or removed by a certified wastecollector for proper repository.

15. Cost ProjectionLabor

06:WPUZD:ZT2061_DT0040 SOIL WASHING_PROTOCOL-09/26/94-Dl 11

000205


Date: 3/17/94Approximately 16 hours each of two technicians' time will be needed to run the soilwashing laboratory scale screening study in triplicate.Transportation/DisposalDisposal costs are dependent on the nature of the washing fluids for example,acidic/basic/presence of surfactants or chelating agents, etc. used. Conventionalwastewater treatment such as granular activated carbon, chemical precipitation maynot work.

r--The total volume of the waste (including the amount of soil received) generated hithis test procedure will be approximately 17 L or 4.5 gallons. However, any unusedsample can be according to 40 CFR Chapter 1 .261.4 (1). returned to the originator.In that case, the volume of the waste generated will be reduced.Also, the transportation cost, the major item in the disposal of wastes, dependslargely on the location of the disposal site.In general the wastes in the treatability facility are stored either in 55 gallon drums orin larger containers and cost of disposal of larger containers are less on per volumebasis than those of drums. Assuming total disposal cost of $250/drum, the cost ofdisposal of 4.5 gallons of waste will be approximately $21.00.UtilitiesUtilities such as chemicals, water and electricity needed for the triplicate tests areminimal and should be included in the laboratory overhead.

06:VWnjZD:ZT2061_DT0040_SOIL_WASHING_PROTOCOL4»/26/94-Dl 12

000206

4.0 TREATABILITY STUDIES MANAGEMENT AND SCHEDULE

To facilitate organization, quality control, and communications each treatability study has anorganizational structure. These are depicted on the following pages.

Gary Moore, EPA On-Scene Coordinator ultimately makes the decision of which treatability studies areperformed and on which contaminants/matrices.

Robert Giswold, EPA Remedial Project Manager for the Bayou Bonfouca site, coordinated the SSC siteneeds with the START program in Cincinatti. He also has imput as to which technologies would betested in treatability studies. -

John Mueller, E & E Project Manager acts as a liaison between Gary and E & E's treatabilitystudies coordinator Julian Myers.

Mr. Myers will interface with each of the treatability testers to assure they have adequate amounts ofsamples on which to run their respective tests and they are committed to the schedule of site activities.He will also be responsible for collecting treatability information into a format which is understandableand which facilitates comparisons between potential removal technologies. In order to meet the draftEE/CA report due date of December 15, it had been agreed upon by all treatability testers to submit theirrespective results by mid November.

Field sampling activities for both site characterization and treatability sample collection is occurringduring August with a projected treatability sample shipping date the last week of August.

This essentially gives the treatability testers two and a half months to perform their tests and submit the

000207

results. Tables 4-1 and 4-2 illustrate the projected schedule of events.

000208

THERMAL TREATMENT REMEDY SCREENING TREATABBLITY STUDYORGANIZATION CHART

Southern Shipbuilding Corporation

CONTRACTOR/WORK ASSIGNMENT MANAGER

• Coordinate Site Activity with TreatabilityTesting

• Collate Study Results with EE/CA reportJulian Myers, CHMMTreatability Coordinator

CHEMICAL/ENGINEER• Regional Support Section• Technical Support Branch

Edward Opatken, START LeaderU.S.E.P.A.O.R.D.

QUALITY ASSURANCE MANAGER

• Oversee Quality Assurance• Report to EPA On-Scene Coordinator

John Mueller, P.E.Project Manager

THERMAL TREATMENT SPECIALIST

Review Treatability Work PlanReview Treatability ResultsReview Treatability Report

Mark Schneckenberger

LABORATORY SUPERVISORACUREX ENVIRONMENTALCORPORATION

• Prepare Treatability Work Plan• Perform Treatability Study• Prepare Treatability Report

Dennis Tabor

Modified From: Guide for conducting treatabiliry studies under CERCLA: Aerobic Biodegradation RemedyScreening Interim Guidance EPA/540/2-91/013. July 1991

06:WPUZD:ZT2061 ELA0240SBA SS F412-10/19/94-D1

000209

BIODEGRADATION REMEDY SELECTION FEASIBILITY ASSESSMENTORGANIZATION CHART



• Prepare Work Plan and Study Report• Implement Biodegradation Treatability

Julian Myers, CHMMBioremediation Specialist

CHEMICAL/BIOENGINEER

Review of Work Plan and Report

Ton Sundquist, Ph.D.Edward Opatken, U.S.E.P.A.O.R.D.


Oversee Quality AssuranceReport to EPA On-Scene Coordinator


STAFF CHEMIST

• Oversee Sample Collection and Analysis• Perform Field Analysis

MICROBIOLOGISTPerform Microbiological Testing

Paul Azzopardi

Modified From: Guide for conducting treatability studies under CERCLA: Aerobic Biodegradation RemedyScreening Interim Guidance EPA/540/2-91/013. July 1991

06:WPUZD:ZT2061 ELA0240SBA SS F421-08/11/94-D1

000210

SOLIDIFICATION/STABILIZATION REMEDY SCREENING TREATABILITY STUDYORGANIZATION CHART



• Coordinate Site Activity with TreatabilityTesting

• Collate Study Results with EE/CA Report

Julian Myers, CHMMTreatability Coordinator

CHEMICAL/ENGINEERRegional Support SectionTechnical Support Branch

Edward Opatken, Start LeaderU.S.E.P.O.R.D.


• Oversee Quality Assurance• Report to EPA On-Scene Coordinator


CONTRACTOR MANAGEROversee Work Plan preparationOversee Treatability ExecutionOversee Report Preparation

Patricia EricsonU.S.E.P.A.R.R.E.L.

KIBER ASSOCIATESPrepare S/S Work PlanPerform Treatabiity StudyPrepare Treatability Report

Modified From: Guide for conducting treatability studies under CERCLA: Aerobic Biodegradation RemedyScreening Interim Guidance EPA/540/2-91/013. July 1991

Q&ZT206! ELAQ240SBA SS F431-Q8/I1/94-D1

000211

SOIL WASHING REMEDY SCREENING TREATABBLITY STUDYORGANIZATION CHART



• Coordinate Site Activity with TreatabilityTesting• Review Work Plan and Study Report

Julian Myers, CHMMTreatability Coordinator

CHEMICAL/BIOENGINEER

Supervise Treatability ImplementationPrepare Work Plan and Report

Jon Sundquist, Ph.D.


Oversee Quality AssuranceReport to EPA On-Scene Coordinator


STAFF CHEMIST

Oversee Sample Collection and AnalysisPrepare Applicable Sections ofWork Plan and Report

MICROBIOLOGIST/TECHNICIAN• Perform Treatability Testing• Coordinate with Staff Chemist

Paul Azzopardi

^Modified From: Guide for conducting treatability studies under CERCLA: Aerobic Biodegradation RemedyScreening Interim Guidance EPA/540/2-91/013. July 1991

0&WPUmZT206I_EUME40SBA_SS_F44208/H/94-Dl

000212

Table 4-1TttEATABILITY TESTING SCHEDlll.K

SOUTHERN SHIPBUILDING CORPORATION(Revised K-I-'M)

U-litil)

1 . Field Sample Collection

2. Siimpli! Shipping

3. THERMAL TREATMENT:a. Wink I'lan huparaiiini

h. TiLMIahilily Hxecmion

c. Dala Analysis

d. Rqmrl Picparatiiiii

4. BIODE«RAI)ATION:;i. Wink 1'lan I'rcpaniiinn

h. Miihili/aiiiin/Conslruclion

u: 'I'leatabilily lixeculion

il. Dalci Analysis

u. Ru|)or[ Preparation

August1-5

-

8-12 15- 19

i

-

•

22-26 29-2H September6-9 12-16

-

19-23 26-30

-JL

October3-7

_

10-14 17-21

4

24-28

-

November31-4 7-11 14-19 21-26

1

(Mi WI- l i/D /| Ml MU KS V.i KM A t 'HAKl IW > I2 <M Ul

000213

Table 4-21 KKATAIHI.I'l V TKSTINC; SrilKDIII.lt

SOIJTIIKRN SHIPBUILDING CORPORATION(conlinucd)

Activity

5. SOLIDIFICATION/STABILIZATION

u. Wink 1'ljii 1'icpaialinn

h. Trealahiliiy l:xt:aitkmand Sample Curing

c. Daia Analysis

d. Rcpmi Preparation

6. SOIL WASIIINC:a. Wink I'kin I'lcparaiiiin

h, Mohili/aii i iu

c. TaMlahilily Mxeculinn

i\. Dau Analysis

u. Rqiml I'rcparaluin

August1-5

•••I

8-12

•Ml

15-19

!

•••

22-26

-

-

29-2September

6-9 12-16

•••

19-23 26-30October

3-7

4

-,

10-14 17-21

?

24-28November

314 7-11 14-19

i—m^Mi. •——•».. I"

•

21-26

———^.iii i J

] MM us ssr kSi-A < MAKI tN'JJ-yj DI

000214

5.0 DATA ANALYSIS AND INTERPRETATION

The data obtained and described in section 3 of this work plan will be analyzed and interpreted for usein assessment of the site removal actions identified in section 2 of this report. The data quality objectives(DQO's) have been established prior to the actual implementation of the TS's. These DQO's will alsoinclude QA/QC requirements. The EE/CA work plan attached QASP and this TS protocol documentdepict most of the general and some of the more detailed DQO's and QA/QC requirements andprocedures to be followed during implementation of the TS's.

The data will be assessed for precision, accuracy, and completeness; the total error will be determinedin this process.

The interpretation of data will include evaluation/assessment criteria listed in section 1 of this document.The results of the TS analysis will be included in a report shown as Task 6 of the EE/CA and CD workplan.

000215

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