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MRIgH REPORT

Test Report for Risk Burn No. 2on the Drake Chemical Superfund Site's

Mobile On-site Hazardous Waste Incinerator

Volume I—Technical Report

For OHM Remediation Services Corp.180 Myrtle Street

Lock Haven, PA 17745

Attn: Mr. Gary JonesTechnical Manager

OHM Subcontract No. 292521-02 ooUD—»%•

MRI Project No. 3620-28 ^or

September 4,1997

MIDWEST RESEARCH INSTITUTE 425 Volker Boulevard, Kansas City, MO 64110-2299 • (816) 753-7600

Preface

Midwest Research Institute (MRI) conducted sampling and analysis for the Risk BurnNo. 2 testing at the Drake Chemical superfund site's mobile on-site soil incinerator locatedat Lock Haven, Pennsylvania. The Risk Burn No. 2 consisted of three runs (numbered asRuns 5, 6, and 7) and was conducted during the period of February 7-9, 1997. This reportpresents the results for these three test runs.

Mr. Gary Jones was the technical manager for OHM Remediation Services Corp. andMr. Paul Gorman was the project leader for MRI. Dr. Greg Jungclaus was the analyticaltask leader and Mr. Jim Surman was the field sampling task leader.

Approved for:

MIDWEST RESEARCH INSTITUTE

Thomas J. Grant, Ph.D., P.E.DirectorApplied Engineering

September 4, 1997

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Contents

Preface .............................................................. iiTables ............................................................... vNomenclature ......................................................... viii

1 Introduction ..................................................... 1-1

2 Operating Data ................................................... 2-1

3 Test Results ..................................................... 3-13.0 Procedures Used for Handling of Data and Calculation of

Emission Rates ........................................... 3-13.1 Method 5 Sampling Data Summary and Particulate Emissions ........ 3-53.2 HC1 and C12 Emission Results ................................ 3-83.3 VOCs and V-TIC Emissions Results .......................... 3-103.4 SVOCs Emissions Results .................................. 3-293.5 PCDD/PCDF Emissions Results ............................. 3-503.6 PCB Emissions Results .................................... 3-573.7 Metals Analysis Results for MM5-MM Samples ................. 3-663.8 Hexavalent Chromium Emissions Results ...................... 3-783.9 Volatile Organic Analysis Results for Feed, Bottom Ash, and

Fly Ash ................................................ 3-803.10 Semivolatile Organic Analysis Results for Feed, Bottom Ash, and

Fly Ash ................................................ 3-833.11 PCDD/PCDF Analysis Results for Bottom Ash and Fly Ash ........ 3-893.12 Herbicides Analysis Results for Feed, Bottom Ash and Fly Ash ...... 3-953.13 Metals Analysis Results for Feed Samples and TCLP Metals in

Bottom Ash, Fly Ash, and Scrubber Water Samples .............. 3-993.14 Feed Characteristics ..................................... 3-1023.15 Continuous Emission Monitoring Results for SO2 ............... 3-104

4 Quality Assurance Report ........................................... 4-14.1 Discussion .............................................. 4-24.2 Audit Samples ........................................... 4-64.3 Data Quality Objectives (DQO) .............................. 4-84.4 Data Review ............................................. 4-8

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Appendices

Volume 2A List of Samples CollectedB Field Sampling Data and Sample TraceabilityC Process and Feed Data

Volume 3D Modified Method 5 Calculations and Laboratory Paniculate ResultsE Calibration Data for Sampling EquipmentF Report on Chemical Analysis Results for Semivolatile OrganicsG Report on Chemical Analysis Results for PCDDs/PCDFsH Report on Chemical Analysis Results for HerbicidesI Report on Chemical Analysis Results for VOCsJ Report on Chemical Analysis Results for MetalsK Report on Chemical Analysis Results for Hexavalent ChromiumL Report on Chemical Analysis Results for PCBsM Report on Chemical Analysis Results for ChloridesN Continuous Emission Monitoring Data for SO2O Example Calculations

MRI.ApplicdMUSlCKZS.sl IV

Tables

1-1. Risk Burn No. 2—Sampling and Analysis Protocols .................... 1-22-1. Summary of Incinerator Process Operating Data ...................... 2-22-2. Waste Feed and Sampling Interruptions—Risk Burn No. 2 .............. 2-33.0-1. Quantification and Data Qualification Procedure for Estimated and

Non-detect Analytical Results .................................... 3-33.1-1. MM5 Summary Data ........................................... 3-63.1-2. Particulate Test Results (Method 0050) ............................. 3-73.2-1. Hydrogen Chloride and Chlorine Emission Results ..................... 3-93.3-1. VOCs in VOST Traps—Run 5 .................................. 3-123.3-2. VOCs in VOST Traps—Run 6 .................................. 3-133.3-3. VOCs in VOST Traps—Run 7 .................................. 3-143.3-4. Condensate Analysis Results—Run 5 .............................. 3-153.3-5. Condensate Analysis Results—Run 6 .............................. 3-163.3-6. Condensate Analysis Results—Run 7 .............................. 3-173.3-7. Summary of VOST Traps and Condensate Analysis Results—Run 5 ...... 3-183.3-8. Summary of VOST Traps and Condensate Analysis Results—Run 6 ...... 3-193.3-9. Summary of VOST Traps and Condensate Analysis Results—Run 7 ...... 3-203.3-10A.VOST Average Emission Rates in g/sec ............................ 3-213.3-10B.VOST Average Emission Rates in Ib/hr ............................ 3-223.3-11. Tentatively Identified Compounds (TICs) in Twenty Largest Peaks of Train A

VOST Trap Samples—Run 5 ................................... 3-233.3-12. Tentatively Identified Compounds (TICs) in Twenty Largest Peaks of Train A

VOST Trap Samples—Run 6 .................................... 3-243.3-13. Tentatively Identified Compounds (TICs) in Twenty Largest Peaks of Train A

VOST Trap Samples—Run 7 .................................... 3-253.3-14. Twenty Largest Peaks Identified in VOST Trap Samples—Run 5 ........ 3-263.3-15. Twenty Largest Peaks Identified in VOST Trap Samples—Run 6 ........ 3-273.3-16. Twenty Largest Peaks Identified in VOST Trap Samples—Run 7 ........ 3-283.4-1. MM5-Semivolatile Analysis Results ............................... 3-313.4-2. MM5-Semivolatile Concentrations and Emission Rates ................ 3-333.4-3A. MM5-Semivolatile Average Emission Rates, in g/sec .................. 3-353.4-3B. MM5-Semivolatile Average Emission Rates, in Ib/hr .................. 3-383.4-4. MM5-Pesticide Analysis Results ................................. 3-393.4-5. MM5-Pesticide Concentrations and Emission Rates ................... 3-403.4-6A. MM5-Pesticide Average Emissioin Rates in g/sec .................... 3-413.4-6B. MM5-Pesticide Average Emissioin Rates in Ib/hr ..................... 3-423.4-7. Matrix Spike Recoveries (XAD) for SVOCs ........................ 3-433.4-8. Matrix Spike (XAD) Recoveries for Pesticides and Surrogates .......... 3-453.4-9. MM5-Semivolatile Blank Train Analytes Associated with Twenty

Largest Peaks Identified in Sample Trains .......................... 3-463..4-10. Twenty Largest Peaks Identified in Run 5 MM5-Semivolatile Train ....... 3-47

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3.4-11. Twenty Largest Peaks Identified in Run 6 MM5-Serriivolatile Train ....... 3-483.4-12. Twenty Largest Peaks Identified in Run 7 MM5-Semivolatile Train ....... 3-493.5-1. Dioxin/Furan Results for MM5-M23 Samples ....................... 3-513.5-2 2,3,7,8-Substituted Dioxin/Furan Emissions for MM5-M23 Samples ...... 3-523.5-3. 2,3,7,8-TCDD Equivalents Results (1989 EPA Factors) ............... 3-533.5-4. 2,3,7,8-TCDD Equivalent Average Emission RAtes ................... 3-543.5-5. Surrogate Recovery Results for MM5-M23 Samples .................. 3-553.5-6 QC Resultsfor 2,3,7,8-Substituted Dioxin/Furan Samples ............... 3-563.6-1. PCB Analysis Results for Blank Train and Method Blank............... 3-583.6-2 PCB Analysis Results .......................................... 3-593.6-3 Results for Laboratory Control Spike of XAD ....................... 3-603.6-4. Initial Precision and Recovery (D?R) Results (% Recovery) ............. 3-613.6-5. PCB Emission Rate for Run 5 ................................... 3-623.6-6. PCB Emission Rate for Run 6 ................................... 3-633.6-7. PCB Emission Rate for Run 7 ................................... 3-643.6-8. Average PCB Emission Rate .................................... 3-653.7-1. Analysis Results for MM5-MM (Metals) Train—Blank Corrected ........ 3-683.7-2. Analysis Results for MM5-MM (Metals) Train, Mercury Results— *

Blank Corrected ............................................. 3-753.7-3. Average Metal Emission Rate (Blank Corrected) ..................... 3-763.7-4. Metals Analysis QAResults ..................................... 3-773.8-1. Hexavalent Chromium Emission Results ........................... 3-793.9-1. VOCs in Feed Samples ........................................ 3-813.9-2. VOCs in Ash Samples ......................................... 3-823.10-1. Semivolatile Results in Feed Samples .............................. 3-843.10-2. Semivolatile Organic Compounds in Ash Samples .................... 3-853.10-3. Matrix Spike Recoveries for Feed, Bottom Ash and Fly Ash ............ 3-873.11-1. 2,3,7,8-Substituted Dioxin/Furan Results for Bottom Ash Samples ....... 3-903.11-2. 2,3,7,8-Substituted Dioxin/Furan Results for Fly Ash Samples ........... 3-913.11-3. QC Results for 2,3,7,8-Substituted Dioxin/Furan Samples .............. 3-923.11-4. 2,3,7,8-TCDD Equivalents Results for Bottom Ash Samples

(1989EPAFactors) ........................................... 3-933.11-5. 2,3,7,8-TCDD Equivalents Results for Fly Ash Samples

(1989EPAFactors) ........................................... 3-943.12-1. Summary of Herbicide Results for Feed Samples ..................... 3-963.12-2. Summary of Herbicide Results for Ash Samples ...................... 3-973.12-3. Summary Table for Herbicide Laboratory Control Spike ............... 3-983.13-1. Metal Concentration in Feeds ......................:............ 3-1003.13-2. TCLP Metal Concentrations in Bottom Ash, Fly Ash, and

Scrubber Water ............................................. 3-1013.14-1. Feed Characteristics .......................................... 3-1033.15-1. Summary of SO2 Monitoring Data ............................... 3-1054-0. Summary of Issues/Concerns ..................................... 4-34-1. Performance Audit Sample Results ................................ 4-7

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4-2. Specific Objectives for Measurement Data(Effluent Sample Analyses Except Stack)............................ 4-9

4-3. Specific Objectives For Measurement Data(Stack Gas Organic Emissions) .................................. 4-11

4-4. Specific Objectives for Measurement Data(Stack Gas Metals Emissions) ................................... 4-14

4-5. Matrix Spike Results for TCLP Metals Extract of Bottom Ash .......... 4-164-6. Matrix Spike Recoveries and Precision for SVOCs in Bottom Ash and

Fly Ash .................................................... 4-174-7. 2,3,7,8-Substituted Dioxin/Furan Precision Results for Bottom Ash

Samples .................................................... 4-194-8. 2,3,7,8-Substituted Dioxin/Furan Precision Results for Fly Ash Samples ... 4-204-9. Precision Results for VOCs in Ash Samples ......................... 4-214-10. Surrogate Recoveries and Precision Data for VOST Samples ............ 4-224-11. Recovery and Precision Results for Combined MM5 Semivolatile Train .... 4-234-12. Surrogate Recovery and Precision Results for MM5-M23 Samples ....... 4-244-13. PCB Surrogate Recovery and Precision Results—XAD Samples ......... 4-254-14. Initial Precision and Recovery (IPR) Results for PCBs on XAD Resin ..... 4-264-15. Metals Train Analysis QA Results ................................ 4-27

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Nomenclature

acfm Actual cubic feet per minuteCLP Contract Laboratory Program (EPA)dscf Dry standard cubic feetdscm Dry standard cubic meters at 20°C, 760 mm Hg (68°F, 29.92 in Hg)dscm/min Dry standard cubic meters per minute at 20 °C, 760 mm Hg

(68 °F, 29.92 in Hg)ECC Environmental Chemical Corp.°F Degrees, Fahrenheitgpm Gallons per minuteIQS Internal quantitation standardL.CS Laboratory control spikeLOQ Limit of quantitationMDL Method detection limitMS Matrix spikeMSD Matrix spike duplicateng Nanogram (10"9 g)PADEP Pennsylvania Department of Environmental ProtectionPCBs Polychlorinated biphenylsPCDD Polychlorinated dibenzodioxins (tetra-octa)PCDF Polychlorinated dibenzofiirans (tetra-octa)PQL Practical quantitation limitQAC Quality Assurance CooridnatorSCC Secondary combustion chamberscfh Standard cubic feet per hour (68 °F, 29.92 in Hg)SVOCs Semivolatile organic compoundsTIC Tentatively Identified Compoundug Microgram (10~6 g)VOCs Volatile organic compoundsVOST Volatile organic sampling train for volatile PICsMM5-CR Modified Method 5 sampling train for hexavalent chromium (Cr+6) .MM5-MM Modified Method 5 sampling train for metalsMM5-SV Modified Method 5 sampling train for semivolatile organicsMM5-PCB Modified Method 5 sampling train for PCBsMM5-D/F Modified Method 5 sampling train for PCDD/PCDFMM5-PHC1 Modified Method 5 sampling train for particulate/HCl/Cl2

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Section 1Introduction

Risk Burn No. 2, consisting of three runs (Runs 5-7), was conducted at the DrakeChemical Superfimd site's mobile on-site soil incinerator during the period ofFebruary 7-9, 1997. Table 1-1 summarizes the test matrix for each of the three runs.

A description of the incineration system, and the sampling and analyses, is contained inAppendix G of the "Trial Burn Plan for the Drake Chemical Superfund Site's MobileHazardous Waste Incinerator," dated September 20, 1996, as amended.

Subsequent sections of this report present results for Risk Burn No. 2 as follows:

Section 2 Operating DataSection 3 Test ResultsSection 4 Quality Assurance Report

The appendices, in separate volumes, provide documentation and supporting data,organized as follows:

Appendices

Volume 2A List of Samples CollectedB Field Sampling Data and Sample TraceabilityC Process Data

Volume 3D Modified Method 5 Calculations and Laboratory Particulate ResultsE Calibration Data for Sampling EquipmentF Report on Chemical Analysis Results for Semivolatile OrganicsG Report on Chemical Analysis Results for PCDDs/PCDFsH Report on Chemical Analysis Results for HerbicidesI Report on Chemical Analysis Results for VOCsJ Report on Chemical Analysis Results for MetalsK Report on Chemical Analysis Results for Hexavalent ChromiumL Report on Chemical Analysis Results for PCBsM Report on Chemical Analysis Results for ChloridesN Continuous Emission Monitoring Data for SO2O Example Calculations

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Section 2Operating Data

This section presents incinerator operating data for all of the runs, numbered Runs 5, 6,and?.

The waste feed consisted of contaminated material from the site. Table 2-1summarizes the incinerator operating parameters for all of the runs, presented as averagevalues calculated from process data recorded every 1 min by the control room computerdata system. This data is contained in Appendix C.

Each run consisted of at least 3 hours of actual sampling time for each traversingsampling train, but the actual incinerator operating time was longer due to some differencein the sampling intervals, leak checks, and port changes, etc.

Some waste feed shutdowns and sampling interruptions occurred during the runs, aslisted in Table 2-2.

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Table 2-2. Waste Feed and Sampling Interruptions—Risk Burn No. 2Run 5 (2/7/97)

11:50 Began sampling

13:26 Stop all sampling for scheduled port change14:21 Resume sampling after port change

15:01 Stop all sampling. Ash discharge conveyor kicked out15:04 Resume sampling

16:00 Finish Run 5

Run 6 (2/8/97)11:00 Began sampling


15:14 Finish Run 6

Run 7 (2/9/97)10:45 Began sampling


14:39 Finish Run 7Failed final pitot leak check on SV train. It was decided by EPA et al. to use pitotreadings from the PCB train (done at the same level) and the volume sampledfrom the SV train to calculate isokinetic on the SV train. Result was good (101 %isokinetic) so SV train valid.

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Section 3Test Results

3.0 Procedures Used for Handling of Data and Calculationof Emission Rates

Subsequent subsections of this report present analysis results for many analytes inseveral different matrices. Those results were used to calculate emission rates for theanalytes, for the purpose of risk assessment. Considering that purpose, it was appropriateto develop procedures for handling data that represented values at or below the detectionlimit (i.e., "< values"). Also, some of the analytical results involve multiple samples (e.g., 4VOST trap pairs per run), so procedures were needed for summing values that may involvenoh-detects, estimated values, and quantified values. MRI and OHM cooperated indeveloping procedures for handling the above situations for the Drake Chemical SuperfundSite risk burn stack results for the test reports. Although different variations of theprocedures are certainly possible, it is believed that the procedures developed herein areuseful and also provide rational methods for handling the data and calculating emissionrates.

Procedures developed for calculating emissions that involve summing of results formore than one component, some or all of which may involve non-detect results, aredescribed in Table 3.0-1. That procedure stipulates substituting one-half the detection limitQ/2 DL) for non-detect values, that may then be used in calculating a sum. The procedurealso specifies some specific data qualifiers for data sums, as follows:

XI Indicates that the sum consists entirely of non-detect (ND) values.(Use V4 DL for ND values.)

X2 Indicates that the sum includes ND values that represent more than 20% ofthe total.

X3 Indicates that the sum includes ND values that represent less than 20% of thetotal.

X4 Indicates that the sum includes ND values and estimated values (J) thatrepresent less than 20% of the total.

MRI-Applied\R3«20-28.S3

Indicates an estimated value, above the MDL but below the PQL. Also usedwhen sum includes estimated values but no non-detect values.Applied to all TIC data, since there are no detection limits for thosecompounds that are only tentatively identified and only semiquantitated.

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Table 3.0-1. Quantification and Data Qualification Procedure for Estimated and_____________Non-detect Analytical Results_________ __

1 Where non-detect values are used in a summation or a quantitation, they aretreated as one-half of the stated detection limit (Yz DL). When presenting thequantitated number, it is stated followed by an X1 flag if all values going intothat sum or quantitation are less than the DL.

2 Where non-detect values are used in a summation or quantitation along withquantified numbers, Vs. DL is used in developing the quantity and the data isflagged with one of two following flags:

X2 To signify that 20% or more of the quantity presented is from a non-detect result.

X3 To signify that less than 20% of the quantity presented is from a non-detect result.

3 Where non-detect values are used in a summation or quantitation along withestimated (J flagged) values, 1/£ DL is used in developing the quantity and thedata is flagged with one of the two flags provided in 2 along with the J flag.

4 Where quantified values, non-detect values, and estimated values are allincluded in the summation quantity, 1/£ DL is used in developing the quantityand the data is flagged with one of the two flags provided in 2 along with the Jflag, except when the estimated and non-detect values contribute less than20% of the total. When this is the case, an X4 flag is used.

5 Where quantified values and estimated values (but no non-detect) areincluded in a sum, the data is flagged with the J flag. When J flagged data isused in a sum, the J flag is dropped if the J flagged result(s) contribute lessthan 20% of the total.

6 The B data flag is used if the blank is equal to or greater than 20% of thesample result. When B flagged data is used in a sum, the B flag will bedropped if the B flagged result(s) contribute less than 20% of the total.

(continued on next page)

MRI-AppW\R3620-28.S3 3-3

Table 3.0-1 Continued(Quantification and Data Qualification Procedure for Estimated and Non-detect

Analytical Results)

Data Qualification Flag Definitions:

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Compound not detected.

Estimated value.

Indicates that a measured value is not greater than 5 times the blank value.

100% of this quantity is from non-detect data using 1/z of the detection limit todevelop the quantity.

Greater than 20% of this quantity is from non-detect data using 50% of thedetection limit to develop the quantity.

This data contains non-detect values, but they contribute less than 20% toquantity.

This data contains non-detect values and estimated values, but theycontribute less than 20% to the quantity.

Tentatively identified and semiquantitated.

The < sign will not be applied to values developed using this procedure.

the

This procedure is not to be used where the method has a specific method ofhandling non-detects (e.g., Method 23 for dioxins/furans, where non-detectsare to be treated as a zero for summation purposes).

This method should be employed on method or field blanks whereappropriate.

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3.1 Method 5 Sampling Data Summary and ParticulateEmissions

Each risk burn run included sampling of stack emissions with six EPA modifiedMethod 5 type sampling trains, which provide data on stack velocity, etc., as given inTable 3.1-1. In conjunction with one or more of the sampling trains, a composite bagsample was collected and analyzed for O2 and CO2 by Orsat. Data from the sampling trainsare presented in Table 3.1-1 along with the Orsat results for O2and CO2. The average stackflow rate as calculated from the sampling trains employed during each respective run is alsogiven and was used in later emission rate calculations. Sampling train identifications are asfollows:

MM5-CR Modified Method 5 sampling train for hexavalent chromium (Cr+6)MM5-MM Modified Method 5 sampling train for metalsMM5-SV Modified Method 5 sampling train for semivolatile organicsMM5-PCB Modified Method 5 sampling train for PCBsMM5-D/F Modified Method 5 sampling train for PCDD/PCDFMM5-PHC1 Modified Method 5 sampling train for particulate/HCl/Cl2

Table 3.1-2 provides the particulate test results determined from the EPA Method 0050sampling trains.

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3-7

3.2 HCI and CI2 Emission Results

A 25-mL aliquot of the 0.1 N sulfuric acid impinger samples from the Method 0050sampling train was analyzed for chloride, representing HCI emissions. Likewise, a 25-mLaliquot of the combined caustic impingers samples was analyzed for chloride, consideredattributable to C12 emissions. These aliquots were analyzed by ion chromatography perMethod 9057. The results are shown in Table 3.2-1, where, in all cases, the measuredconcentration was below the detection limit. A value of Vz D.L. was used to calculate theemission rates shown in Table 3.2-1. If the blank values had been used to blank correct thedata, as allowed in Method 0050, the blank corrected emission rates would be zero.

Matrix spike recovery for the acidic impingers was good (97%), but was somewhathigh (128%) for the basic impingers, which is above the method limit of 90-110%. Thiscould indicate that the reported C12 emissions are higher than actual.

Audit samples prepared by the MRI Quality Assurance Coordinator (Q AC) weresubmitted for analysis and those results are discussed in Section 4.

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3.3 VOCs and V-TIC Emissions ResultsVOST trap samples were analyzed for the target volatile organic compounds using

purge and trap GC/MS analysis, specifically as described in SW-846 Method 5041. Thefront trap (Tenax) and back trap (Tenax/charcoal) from each sampling period weredesorbed together and analyzed as a pair.

Two VOST trains were used for sampling in each run, referred to as Train A (4 pair)and Train B (3 pair). VOST trap pairs from Train B were analyzed by selective ionmonitoring (SIM) for all the target compounds (except benzene and 2-butanone), but theSIM results are shown only for those analytes that were not found in full scan analysis ofTrain A samples. The results of the VOC concentrations found in the traps, by full scan orSIM, are given in Tables 3.3-1, 3.3-2, and 3.3-3.

It should also be noted that the high benzene levels in the VOST traps saturated theGC/MS, requiring quantitation by a secondary ion. Since the benzene level was abovethe calibration range, the reported values may not be as accurate as for other analytes. Thebenzene levels also necessitated quantitation of 1,2-dichloroethane using a secondary ion.

Tables 3.3-1, 3.3-2 and 3.3-3 include surrogate recoveries for the VOST trap pairs.Recoveries for two of the three surrogates met the QA objective of 75-125% for all but onepair in Run 5 (153%). Most of the recoveries for the third surrogate (1,2-dichloroethane-d4) were above 125% due to interference from a coeluting benzene peak.

Condensate samples collected in the VOST sampling trains during each run were alsoanalyzed, by full scan and SIM, and those results were used to calculate the correspondingconcentration of each analyte in the gas stream, as shown in Tables 3.3-4, 3.3-5, and 3.3-6.Like the VOST trap samples discussed above, the results for condensate by SIM are shownonly if they were not detected in the full scan analysis. For any values that were below thedetection limit, a value of one-half the detection limit was used in calculating the amountsand concentrations.

The concentrations of each analyte determined from the VOST traps and from thecondensate were added together to determine the total concentration of each analyte, asshown in Tables 3.3-7, 3.3-8, and 3.3-9. Those concentrations were then used to calculate

MRl-Appl*d\R3620-28.S3 3-10

the emission rates for the analytes in g/sec and Ib/hr. Tables 3.3-10A and B show theaverage emission rate for all three runs.

In addition to the specific list of VOCs, the Train A trap pair full scan results wereused to tentatively identify and semiquantitate the V-TICs in the 20 largest peaks. Thoseresults are given in Tables 3.3-11 to 3.3-13. As expected, many of those peaks could notbe specifically identified (e.g., branched alkane, C8-C10). Results in Tables 3.3-11 to 3.3-13 for TICs in the 20 largest peaks and results given in previous tables for target analytes(Tables 3.3-1, 3.3-2, and 3.3-3) were used to compile the list of 20 largest peaks for eachrun, and their emission rates, as shown in Tables 3.3-14 through 3.3-16.

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3-20

AR3U666

Table 3.3-10A. VOST Average Emission Rates in g/sec

Benzene2-ButanoneCarbon TetrachlorideChlorobenzeneChloroform1 ,2-Dichloroethane1,1-DichloroetheneTetrachloroetheneToluene1,1,1 -TrichloroethaneTrichloroetheneVinyl ChlorideBromodichloromethaneBromoformBromomethaneCarbon DisulfideChloroethaneDibromochloromethanet-1 ,2-DichloroetheneEthylbenzene2-HexanoneMethylene Chloride4-Methyl-2-PentanoneStyreneTrichlorofluoromethaneVinyl Acetateo-Xylenem-/p-XyleneTotal Xylene

Run 5EmissionRate8(g/sec)

2.97E-035.91 E-05 J, B5.4E-06 J, X33.6E-056.06E-051.19E-07X14.3E-07 X22.2E-06 J1.6E-05 J, B1.07E-06X31.4E-06 J, X38.5E-07 B, X31.97E-05 X34.2E-06 J, X35.57E-05 J, B, X35.8E-06 J3.2E-07 J, B, X27.6E-06 J, X32E-07 J, X2

2.3E-06 J, B5.3E-06 J, B2.2E-05 J, B5.84E-06 B, X37.5E-06 J, B1.85E-05 B4.66E-06 X32.5E-06 J, B8.0E-06 J, B1.05E-05 J, B


3.77E-035.59E-05 J, B5.2E-064.72E-057.29E-051.97E-07X14.2E-07 X22.4E-06 J, B1.38E-05 J, B9.2E-07 X31.2E-06 J,X28.0E-07 B, X32.27E-054.7E-06 J, X34.65E-05 J, B7.3E-06 J5.2E-07 B, X28.1E-06 X31.2E-07X12E-06 J, B

2.43E-052.02E-05 J, B3.9E-06 J, X21.3E-05X34.8E-064.26E-06 X35.7E-06 J, B1.14E-05 J,B1.8E-05 J, B


3.45E-037.00E-05 J, B6.1E-06 J.X34.29E-056.42E-051.2E-07X13.7E-07 J, X22.6E-06 J, B1.6E-05 J,B9.1E-07X31.3E-06 J6.6E-07 B, X32.02E-05 X35.4E-06 J, X33.82E-05 J, B7.0E-06 J3.0E-07 J, B, X27.6E-06 J, X31.3E-07 J.X22.2E-06 J, B5.0E-06 B2.1 E-05 J, B2.52E-06 X38.7E-06 B, X34.4E-06 B1.94E-05 J

3E-06 J, B8.7E-06 J, B1.22E-05 J, B

AverageEmissionRate(g/sec)3.40E-036.17E-055.6E-064.2E-056.59E-051.5E-074.1E-072.4E-061.5E-059.7E-071.3E-067.7E-072.09E-054.8E-064.68E-056.7E-063.8E-077.8E-061.5E-072.2E-061.2E-052.1 E-054.09E-069.7E-069.2E-069.44E-063.7E-069.4E-061.4E-05

a From Tables 3.3-7 through 3.3-9.

U Indicates compound was analyzed for but not detected.B Indicates that measured value is not greater than 5 times the blank value.J Indicates an estimated value; above the MDL but below the PQL.X1 Indicates that the value consists only of ND values (using one half the DL for ND values).X2 Indicates that the value includes ND values that represent >20% of the total.X3 Indicates that the value includes ND values that represent <20% of the total.X4 Indicates that the value includes ND and J values that represent <20% of the total.

3-21

AR3U667

Table 3.3-10B. VOST Average Emission Rates in Ib/hr

Benzene2-ButanoneCarbon TetrachlorideChlorobenzeneChloroform1 ,2-Dich!oroethane1,1-DichloroetheneTetrachloroetheneToluene1,1,1 -TrichloroethaneTrichloroetheneVinyl ChlorideBromodichloromethaneBromoformBromomethaneCarbon DisulfideChloroethaneDibromochloromethanet-1 ,2-DichIoroetheneEthylbenzene2-HexanoneMethylene Chloride4-Methyl-2-PentanoneStyreneTrichlorofluoromethaneVinyl Acetateo-Xylenem-/p-XyleneTotal Xylene

Run5EmissionRate8(Ib/hr)

2.35E-024.69E-04 J, B4.3E-05 J, X32.8E-044.81 E-049.48E-07 X13.4E-06 X21.7E-05 J1.3E-04 J, B8.53E-06 X31.1E-05 J.X36.7E-06 B, X31.56E-04X33.3E-05 J, X34.42E-04 J, B, X34.6E-05 J2.5E-06 J, B, X26.0E-05 J, X32E-06 J, X2

1.8E-05 J,B4.2E-05 J, B1.7E-04 J, B4.64E-05 B, X35.9E-05 J, B1.47E-04 B3.70E-05 X32.0E-05 J, B6.3E-05 J, B8.37E-05 J, B

Run 6EmissionRate8(Ib/hr)

2.99E-024.43E-04 J, B4.1E-053.75E-045.78E-041.56E-06X13.4E-06 X21.9E-05 J,B1.09E-04 J, B7.3E-06 X39.4E-06 J, X26.3E-06 B, X31.80E-043.7E-05 J, X33.69E-04 J, B5.8E-05 J4.1E-06 B,X26.4E-05 X39.4E-07 X12E-05 J, B

1.93E-041.60E-04 J, B3.1E-05 J,X21.0E-04X33.8E-053.38E-05 X34.5E-05 J, B9.05E-05 J, B1.4E-04 J, B


2.74E-025.56E-04 J, B4.9E-05 J, X33.41 E-045.10E-049.6E-07 X13.0E-06 J, X22.1E-05 J, B1.3E-04 J, B7.3E-06 X31.0E-05 J5.3E-06 B, X31.60E-04X34.3E-05 J, X33.03E-04 J, B5.6E-05 J2.4E-06 J, B, X26.1E-05 J,X31.0E-06 J, X21.8E-05 J.B4.0E-05 B1.7E-04 J,B2.00E-05 X36.9E-05 B, X33.5E-05 B1.54E-04 J2E-05 J, B

6.9E-05 J, B9.65E-05 J, B

AverageEmissionRate(Ib/hr)2.69E-024.89E-044.4E-053.3E-045.23E-041.2E-063.3E-061.9E-051.2E-047.7E-061.0E-056.1E-061.65E-043.8E-053.71 E-045.3E-053.0E-066.2E-051.3E-061.9E-059.2E-051.7E-043.2E-057.6E-057.3E-057.49E-052.8E-057.4E-051.1 E-04

a From Tables 3.3-7 through 3.3-9.


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One of the sampling trains employed (MM5-SV) was used for determining emissions oftarget semivolatile organic compounds, and pesticides, and 20 largest peaks. GC/MS analysis forSVOCs was done full scan and SIM equivalent (i.e. high sensitivity). Analysis results for theSVOCs found in the MM5-SV samples are presented in Table 3.4-1. Table 3.4-1 includes SIMequivalent results whenever the analyte was not detected in the full scan analysis. Whenever ananalyte result was non-detect in the SIM equivalent analysis, a value of !/2 the detection limit wasused in calculating stack gas concentrations.

The concentration results shown in Table 3.4-1 were used to calculate the emission ratespresented in Table 3.4-2. Average emission rates for all 3 runs are presented in Tables 3.4-3Aand 3B.

Besides being analyzed for SVOCs, the MM5-SV extracts were also analyzed for pesticides.Those results are presented in Tables 3.4-4 and 3.4-5, again using l/2 the detection limit for non-detects. The average pesticide emission rates are given in Tables 3.4-6A and 6B.

Recovery results for the surrogates spiked into the samples are included in Table 3.4-1. Allof the surrogate recoveries met the QA objective of 50-150%.

An XAD matrix spike of all SVOCs, except p-naphthylamine, was prepared and analyzedwith results shown in Table 3.4-7. A separate matrix spike of P-naphthylamine was alsoprepared, since the other compounds present in the spike mixture degraded the P-naphthylaminein the spiking mixture. That result is included in Table 3.4-7, which shows recovery of 36%.This is lower than the 50-150% recovery objective, but it is within the 25-100% range set byECC for anatysis of P-naphthylamine in solid matrices as shown in Section 3.10.

Most of the recoveries for the SVOCs were within the QA objective range of 50-150%.Recovery for 5 of the 59 compounds, including P-naphthylamine, was below 50%, as shownbelow:

P-naphthylamine 36%Pentachlorophenol 41%3,3'-Dichlorobenzidine 33%

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Although these are below the 50-150% objective, the recoveries for 3,3'-Dichlorobenzidineand Hexachlorocyclopentadiene are actually above the recovery values shown in Table 11 ofSW846-8270B. Thus, it can be stated that the majority of the compounds (95%) met therecovery objectives or met recoveries expected per Method 8270B.

A matrix spike of the pesticides and S VOC surrogates was also prepared, and those analysisresults are summarized in Table 3.4-8, with all recoveries meeting the QA objective of 50-150%.

The full scan analysis of the MM5-SV samples was also used to tentatively identify andsemiquantitate the SV-TICs in the 20 largest peaks. Those results and associated emission ratesare presented in Tables 3.4-9 through 3.4-12 where the 20 largest peaks includes target analytesand TICs. As expected, several of the TICs could not be specifically identified. It should benoted that the TICs are not necessarily the same between runs, and several of the TICs werepresent in the blank train in approximately the same amounts as in the sample trains, indicatingthat they are not being emitted from the stack. It should be noted that XAD is a synthetic organicresin which can degrade slightly during use. This degradation can result in organic compounds.One example of this is benzoic acid, which may be an XAD degradation product, as evidencedby the fact that benzoic acid was higher in the blank train than in two of the sample trains andover 85% of the amount in the third sample train.


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3-34

AR3U680

Table 3.4-3A. MM5-SemivoIatile Average Emission Rates, in g/sec

Benzo(a)anthraceneBenzo(a)pyreneBenzo(b)fiuorantheneBenzo(k)fluorantheneChryseneDibenz(a,h)anthracene1 ,2-Dichlorobenzene1 ,4-DichlorobenzeneFluorantheneHexachlorobenzenelndeno(1 ,2,3-cd)pyreneNaphthalene

p-Naphthylamine

2-Nitroaniline4-NitroanilineNitrobenzenePentachlorobenzenePentachlorophenolPyrene1 ,2,4-Trichlorobenzene2,4,5-Trichlorophenol2,4,6-TrichlorophenoIAcenaphtheneAcenaphthyleneAnthraceneBenzo(e)pyreneBenzo(g,h,i)peryieneBenzole acidbis(2-Chloroethoxy)methanbis(2-Ethylhexyl)phthalateButylbenzylphthalateCarbazole4-Chloroaniline4-Chloro-3-methyiphenoi2-Chloronaphthalene

Run5EmissionRate3(g/sec)

1.6E-07X11.6E-07X11.6E-07X11.6E-07X11.6E-07X11.6E-07 X11.2E-06 J5.0E-07 J1.6E-07X11.6E-07X11.6E-07X16.9E-06 B

1.6E-07 X1

1.6E-07X11.6E-07X11.7E-051.6E-07X16.1E-07 JB1.6E-07 X11.6E-07X11.6E-07X11.6E-07X11.6E-07X11.6E-07X15.8E-07 JB1.6E-07X11.6E-07X11.9E-03 B1.6E-07X12.7E-05 B2.5E-06 B1.6E-07X11.6E-07X11.7E-06 J1.6E-07X1


1.6E-07 X11.6E-07 X11.6E-07 X11.6E-07 X11.6E-07 X11.6E-07 X14.5E-07 J5.1E-07 J1.6E-07X11.6E-07X11.6E-07X15.7E-06 B

1.6E-07X1

1.6E-07X11.6E-07X11.3E-051.6E-07X11.6E-07X11.3E-06 J1.6E-07X11.6E-07 X11.6E-07X11.6E-07X11.6E-07X15.5E-07 JB1.6E-07X11.6E-07X11.4E-03 B1.6E-07X11.1E-04 B2.4E-06 B1.6E-07 X11.6E-07X11.6E-07X11.6E-07 X1


1.6E-07X11.6E-07X11.6E-07X11.6E-07X116E-07X11.6E-07X16.7E-07 J4.8E-07 J1.6E-07X11.6E-07X11.6E-07X16.2E-06 B

1.6E-07X1

1.6E-07X11.6E-07X11.6E-051.6E-07X11.6E-07X11.6E-07X11.6E-07X11.6E-07 X11.6E-07X11.6E-07X11.6E-07X16.5E-07 JB1.6E-07 X11.6E-07 X11.5E-03 B1.6E-07 X14.0E-05 B2.4E-06 B1.6E-07X11.6E-07X11.6E-07X11.6E-07X1

AverageEmissionRate(g/sec)1.6E-071.6E-071.6E-071.6E-071.6E-071.6E-077.8E-075.0E-071.6E-071.6E-071.6E-076.3E-06

1.6E-07

1.6E-071.6E-071.5E-051.6E-073.1E-075.4E-071.6E-071.6E-071.6E-071.6E-071.6E-075.9E-071.6E-071.6E-071.6E-031.6E-076.0E-052.4E-061.6E-071.6E-076.8E-071.6E-07

3-35

AR3U68

Table 3.4-3A (Continued)MM5-Semivolatile Average Emission Rates, in g/sec

2-ChlorophenolDibenzofuran1 ,3-Dichlorobenzene3,3-Dichlorobenzidine2,4-DichlorophenolDiethylphthalate2,4-DimethylphenoIDimethylphthalateDi-n-butylphthalate2,4-DinitrophenolDi-n-octylphthalateFluoreneHexachlorobutadieneHexachlorocyclopentadieneHexachoroethane2-Methylnaphthalene2-Methylphenol4-Methylphenol2-Nitrophenol4-NitrophenolPhenanthrenePhenol1 ,2,4,5-Tetrachlorobenzene2,3,4,6-Tetrachlorophenol

Run5EmissionRate3(g/sec)

1.6E-07X11.6E-07X11.6E-07X11.6E-07X11.6E-07X16.6E-06 B1.6E-07X11.8E-058.2E-06 B1.6E-07X11.9E-06 JB1.6E-07X11.6E-07X11.6E-07X11.6E-07X11.6E-07X16.5E-06 B1.0E-05 B1.8E-051.6E-07X18.2E-07 J1.2E-045.1E-07 J1.6E-07X1


1.6E-07X11.6E-07X11.6E-07X11.6E-07X11.6E-07X16.6E-06 B1.6E-07 X11.9E-051.7E-05 B1.6E-07X11.3E-06 JB1.6E-07X11.6E-07X11.6E-07X11.6E-07X11.6E-07X12.1E-06 B3.5E-06 B1.5E-051.6E-07X19.3E-07 J1.0E-045.8E-07 J1.6E-07X1


1.6E-07X11.6E-07X11.6E-07X11.6E-07X11.6E-07X16.2E-06 B1.6E-07X11.9E-059.5E-06 B1.6E-07X11.7E-06 JB1.6E-07X11.6E-07X11.6E-07X11.6E-07X11.6E-07 X12.2E-06 B3.2E-06 B1.5E-051.6E-07X18.5E-07 J1.0E-043.7E-07 J1.6E-07 X1

AverageEmissionRate(g/sec)1.6E-071.6E-071.6E-071.6E-071.6E-076.4E-061.6E-071.9E-051.1E-051.6E-071.6E-061.6E-071.6E-071.6E-071.6E-071.6E-073.6E-065.6E-061.6E-051.6E-078.7E-07HE-044.9E-071.6E-07

a From Table 3.4-2.


3-36

AR3U682

Table 3.4-3B. MM5-SemivoIatile Average Emission Rates in Ib/hr

Benzo(a)anthraceneBenzo(a)pyreneBenzo(b)fluorantheneBenzo(k)fluorantlieneChryseneDibenz(a, h)anthracene1 ,2-Dichlorobenzene1 ,4-DichlorobenzeneFluorantheneHexachlorobenzenelndeno(1 ,2,3-cd)pyreneNaphthalene

p-Naphthylamine

2-Nitroaniline4-NitroanilineNitrobenzenePentachlorobenzenePentachlorophenolPyrene1 ,2,4-Trichlorobenzene2,4,5-Trichlorophenol2,4,6-TrichlorophenolAcenaphtheneAcenaphthyleneAnthraceneBenzo(e)pyreneBenzo(g,h,i)peryleneBenzole acidbis(2-Chloroethoxy)methanebis(2-Ethylhexyl)phthaiateButylbenzylphthalateCarbazole4-Chloroaniline4-ChIoro-3-methylphenoI2-Chloronaphthalene


1.3E-06X11.3E-06 X11.3E-06X11.3E-06X11.3E-06X11.3E-06 X19.6E-06 J4.0E-06 J1.3E-06X11.3E-06X11.3E-06 X15.5E-05'B

1.3E-06X1

1.3E-06X11.3E-06X11.3E-041.3E-06 X14.8E-06 JB1.3E-06X11.3E-06X11.3E-06X11.3E-06X11.3E-06 X11.3E-06 X14.6E-06 JB1.3E-06X11.3E-06X11.5E-02 B1.3E-06X12.2E-04 B2.0E-05 B1.3E-06X11.3E-06 X11.4E-05 J1.3E-06X1


1.3E-06X11.3E-06X11.3E-06X11.3E-06 X11.3E-06 X11.3E-06X13.6E-06 J4.1E-06 J1.3E-06 X11.3E-06 X11.3E-06X14.5E-05 B

1.3E-06 X1

1.3E-06X11.3E-06X11.1E-041.3E-06 X11.3E-06X11.0E-05 J1.3E-06X11.3E-06 X11.3E-06 X11.3E-06X11.3E-06X14.4E-06 JB1.3E-06X11.3E-06X11.1E-02 B1.3E-06 X18.9E-04 B1.9E-05 B1.3E-06 X11.3E-06X11.3E-06X11.3E-06X1


1.2E-06 X11.2E-06 X11.2E-06X11.2E-06X11.2E-06 X11.2E-06 X15.3E-06 J3.8E-06 J1.2E-06 X11.2E-06X11.2E-06X14.9E-05 B

1.2E-06X1

1.2E-06X11.2E-06X11.3E-041.2E-06X11.2E-06X11.2E-06X11.2E-06X11.2E-06X11.2E-06 X11.2E-06X11.2E-06 X15.2E-06 JB1.2E-06 X11.2E-06X11.2E-02 B1.2E-06X13.2E-04 B1.9E-05 B1.2E-06X11.2E-06X11.2E-06 X11.2E-06X1

AverageEmissionRate(Ib/hr)1.3E-061.3E-061.3E-061.3E-061.3E-061.3E-066.2E-064.0E-061.3E-061.3E-061.3E-065.0E-05

1.36-06

1.3E-061.3E-061.2E-041.3E-062.4E-064.3E-061.3E-061.3E-061.3E-061.3E-061.3E-064.7E-061.3E-061.3E-061.3E-021.3E-064.7E-041.9E-051.3E-061.3E-065.4E-061.3E-06

3-37

AR3U683-

Table 3.4-3B. (Continued)MM5-SemivoIatile Average Emission Rates, in Ib/hr

2-ChlorophenolDibenzofuran1 ,3-Dichlorobenzene3,3-DichIorobenzidine2,4-DichlorophenolDiethylphthalate2,4-DimethylphenolDimethylphthalateDi-n-butylphthalate2,4-DinitrophenoIDi-n-octylphthalateFluoreneHexachlorobutadieneHexachlorocyclopentadieneHexachoroethane2-Methylnaphthalene2-Methylphenol4-MethyIphenoI2-Nitrophenol4-NitrophenolPhenanthrenePhenol1 ,2,4,5-Tetrachlorobenzene2,3,4,6-Tetrachlorophenol


1.3E-06X11.3E-06X11.3E-06X11.3E-06 X11.3E-06X15.3E-05 B1.3E-06X11.4E-046.5E-05 B1.3E-06 X11.5E-05 JB1.3E-06X11.3E-06X11.3E-06X11.3E-06X11.3E-06X15.2E-05 B8.1E-05 B1.4E-041.3E-06X16.5E-06 J9.4E-044.0E-06 J1.3E-06X1


1.3E-06X11.3E-06X11.3E-06X11.3E-06X11.3E-06X15.2E-05 B1.3E-06X11.5E-041.3E-04 B1.3E-06 X11.0E-05 JB1.3E-06X11.3E-06X11.3E-06 X11.3E-06X11.3E-06 X11.7E-05 B2.8E-05 B1.2E-041.3E-06X17.4E-06 J8.2E-044.6E-06 J1.3E-06X1

Run?EmissionRate*(Ib/hr)

1.2E-06X11.2E-06 X11.2E-06X11.2E-06X11.2E-06X14.9E-05 B1.2E-06X11.5E-047.6E-05 B1.2E-06 X11.3E-05 JB1.2E-06 X11.2E-06X11.2E-06X11.2E-06 X11.2E-06 X11.8E-05 B2.5E-05 B1.2E-041.2E-06X16.7E-06 J8.2E-042.9E-06 J1.2E-06X1

AverageEmissionRate(Ib/hr)1.3E-061.3E-061.3E-061.3E-061.3E-065.1E-051.3E-061.5E-049.1E-051.3E-061.3E-051.3E-061.3E-061.3E-061.3E-061.3E-062.9E-054.5E-051.3E-041.3E-066.9E-068.6E-043.8E-061.3E-06

a From Table 3.4-2.

U Indicates compound was analyzed for but not detected.B Indicates that measured value is not greater than 5 times the blank value.J Indicates an estimated value; above the MDL but below the PQL.X1 Indicates that the value consists only of ND values (using one half the DL for ND values).X2 Indicates that the value includes NO values that represent >20% of the total.X3 Indicates that the value includes ND values that represent <20% of the total.X4 Indicates that the value includes ND and J values that represent <20% of the total.

3-38

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3-40

AR3U686

Table 3.4-6A. MM5-Pesticide Average Emission Rates in g/sec

Aidrina -Chlordaney -Chlordane4,4 -ODD2,4 -DDE4,4 -DDE4,4 -DOTEndosulfan 1Endosulfan sulfateEndrinEndrin aldehydeHeptachlorP -Hexachlorocyclohexane

Run5EmissionRate3(g/sec)8.1E-07 X18.1E-07 X18.1E-07 X18.1E-07 X18.1E-07 X18.1E-07 X18.1E-07 X18.1E-07 X18.1E-07 X18.1E-07 X18.1E-07 X18.1E-07 X18.1E-07 X1

Run 6EmissionRate3(a/sec)7.9E-07 X17.9E-07 X17.9E-07 X17.9E-07 X17.9E-07 X17.9E-07 X17.9E-07 X17.9E-07 X17.9E-07 X17.9E-07 X17.9E-07 X17.9E-07 X17.9E-07 X1

Run 7EmissionRate3(g/sec)7.8E-07 X17.8E-07 X17.8E-07 X17.8E-07 X17.8E-07 X17.8E-07 X17.8E-07 X17.8E-07 X17.8E-07 X17.8E-07 X17.8E-07 X17.8E-07 X17.8E-07 X1

AverageEmissionRate(g/sec)7.9E-077.9E-077.9E-077.9E-077.9E-077.9E-077.9E-077.9E-077.9E-077.9E-077.9E-077.9E-077.9E-07

a From Table 3.4-5.

X1 Indicates that the value consists only of ND values (using one half the DL for ND values).

MRI-AppIi«NU620-28.S3A 3-41

AR3IU687

ITable 3.4-6B. MM5-Pesticide Average Emission Rates in Ib/hr

Aldrina -Chlordaney -Chlordane4,4 -ODD2,4 -DDE4,4 -DDE4,4 -DOTEndosulfan 1Endosulfan sulfateEndrinEndrin aldehydeHeptachlorP -Hexachlorocyclohexane

Run5EmissionRate3

Jlb/hr)6.5E-06 X16.5E-06 X16.5E-06 X16.5E-06 X16.5E-06 X16.5E-06 X16.5E-06 X16.5E-06 X16.5E-06 X16.5E-06 X16.5E-06 X16.5E-06 X16.5E-06 X1


6.3E-06 X16.3E-06 X16.3E-06 X16.3E-06 X16.3E-06 X16.3E-06 X16.3E-06 X16.3E-06 X16.3E-06 X16.3E-06 X16.3E-06 X16.3E-06 X16.3E-06 X1


6.2E-06 X16.2E-06 X16.2E-06 X16.2E-06 X16.2E-06 X16.2E-06 X16.2E-06 X16.2E-06 X16.2E-06 X16.2E-06 X16.2E-06 X16.2E-06 X16.2E-06 X1

AverageEmissionRate(Ib/hr)6.3E-066.3E-066.3E-066.3E-066.3E-066.3E-066.3E-066?3E-066.3E-066.3E-066.3E-066.3E-066.3E-06

a From Table 3.4-5.

X1 Indicates that the value consists only of ND values (using one half the DL for ND values).

MRI-Applie*R3«20-Z8.S3A 3-42

AR3U688

Table 3.4-7. Matrix Spike Recoveries (XAD) for SVOCs

NAME

Benzo(a)anthraceneBenzo(a)pyreneBenzo(b)fluorantheneBenzo(k)fluorantheneChryseneDibenz(a,h)anthracene1 ,2-Dichlorobenzene1,4-DichlorobenzeneFluorantheneHexachlorobenzenelndeno(1 ,2,3-cd)pyreneNaphthalene

p-Naphthylamine

2-Nitroaniline4-NitroanilineNitrobenzenePentach lorobenzenePentachlorophenolPyrene1 ,2,4-Trichlorobenzene2,4,5-Trichlorophenol2,4,6-TrichlorophenolAcenaphtheneAcenaphthyleneAnthraceneBenzo(e)pyreneBenzo(g,h,i)peryleneBenzole acid

% Recovery(for 25 ug spike level)QA Objective 50-1 50%

929294899292767397899483

3ga,b

8756809341 a997990839188861079269

a Recovery outside QA objective range of 50-150%.b Recovery result of 36% is for a separate matrix spike of p-Naphthylamine only.

MRI-AppIicd\R3620-28.S3A

Table 3.4-7 (Continued)Matrix Spike Recoveries (XAD) for SVOCs

NAME

bis(2-Chloroethoxy)methanebis(2-Ethylhexyl)phthalateButylbenzylphthalateCarbazole4-Chloroaniline4-Chloro-3-methylphenol2-Chloronaphthalene2-ChlorophenolDibenzofuran1 ,3-Dichlorobenzene3,3'-Dichlorobenzidine2,4-DichlorophenolDiethylphthalate2,4-DimethylphenolDimethylphthalateDi-n-butylphthalate2,4-DinitrophenolDi-n-octylphthalateFluoreneHexachlorobutadieneHexachlorocyclopentadieneHexachoroethane2-Methylnaphthalene2-Methylphenol4-Methylphenol2-Nitrophenol4-NitrophenolPhenanthrenePhenol1 ,2,4,5-Tetrachlorobenzene2,3,4,6-Tetrachlorophenol

% Recovery(for 25 ug spike level)QA Objective 50-1 50%

8497937571848676957433 a819561929114 a95897729 a74907675797287788278

a Recovery outside QA objective range of 50-150%.b Recovery result of 36% is for a separate matrix spike of p-Naphthylamine only.

MRI-Appfe*R3«20-28.S3A 3-44

AR3U690

Table 3.4-8. Matrix Spike (XAD) Recoveries for Pesticides and Surrogates% Recovery

(for 5 jig spike level)Q A Objective 50 -150%

Aldrina -Chlordaney -Chlordane4,4 -ODD2,4 -DDE4,4 -DDE4,4 -DOTEndosulfan IEndosulfan sulfateEndrinEndrin aldehydeHeptachlorp -Hexachlorocyclohexane

Surrogate Recoveries (%)2-FluorophenolPhenol-d52-Chloropheno!-d41 ,2-Dichlorobenzene-d4Nitrobenzene-d52-Fluorobiphenyl2,4,6-TribromophenolTerphenyl-d14

951111111011081129699961229796101

6876747584838787


AR3U69I

Table 3.4-9. MM5-SemivolatiIe Blank Train AnalytesAssociated with Twenty Largest Peaks Identified in

Sample Trains

ButoxyethoxyethanolBenzoic acidXylenes aEthyl benzaldehydeMethyl benzoateAlkane aBenzaldehydeUnknown aEthyl benzoic acid aEthyl acetophenone aDecane + C3 benzeneAlkyl acetophenone abis(2-Ethylhexyl)phthalateEthyl methyl benzoateAcetophenoneDichlorocyclohexaneDimethyl cyclohexanePhenol

Total

TIC660

215684039272323221512

105.84.93.3

amount (ng)

Z

zZzzzzzzzz

zzzz

Targetanalyte"

526

10.2

1.59

a This compound represents the sum of several similar compounds withunique mass spectra that cannot be otherwise identified using the massspectral library.

b From Table 3.4-1.

Z Indicates a compound that is only tentatively identified and semiquantitated.

3-46

AR3U692

Table 3.4-10. Twenty Largest Peaks Identified in Run 5 MM5-SemivoIatiIe Train

Benzole acidButoxyethoxyethanolXylenes aBenzaldehydeEthyl berizaldehydeUnknown Alkane aUnknown aMethyl benzoatePhenolEthyl benzoic acidDichlorocyclohexaneEthyl acetophenoneDecane + C3 benzeneBromobenzenelodobenzeneMethyl hexenoneHydroxymethyl pentanoneDimethyl cyclohexanebis(2-Ethylhexyl)phthaIateNitrobenzene

Total amount (ng)Target

TIC analyted599 B

250 BZ243 BZ120 BZ120 BZ57 Z54 BZ43 BZ

36.436 BZ25 BZ16 BZ15 BZ14 Z12 Z11 Z10 Z9.1 BZ

8.38 B5.18

Stack gasconcb

([ig/dscm)1968280393919181412128.25.24.94.63.93.63.33.02.71.7

Emission Rate0(g/sec) (Ib/hr)

2.0E-03 B 1.5E-02 B8.1E-04 BZ 6.5E-03 BZ7.9E-04 BZ 6.3E-03 BZ3.9E-04 BZ 3.1E-03 BZ3.9E-04 BZ 3.1E-03 BZ1.9E-04 Z 1.5E-03 Z1.7E-04 BZ 1.4E-03 BZ1.4E-04 BZ 1.1E-03 BZ1.2E-04 9.4E-041.2E-04 BZ 9.3E-04 BZ8.1E-05 BZ 6.5E-04 BZ5.1E-05 I3Z 4.1E-04 BZ4.9E-05 BZ 3.9E-04 BZ4.6E-05 Z 3.6E-04 Z3.9E-05 Z 3.1E-04 Z3.6E-05 Z 2.8E-04 Z3.3E-05 Z 2.6E-04 Z3.0E-05 BZ 2.4E-04 BZ2.7E-05 B 2.2E-04 B1.7E-05 1.3E-04

a This compound represents the sum of several similar unknown compounds with unique mass spectra thatcannot otherwise be identified using the mass spectral library.

b Concentration calculated from volume of gas sampled, 3.056 dscm (from Table 3.1-1).c Emission rates calculated from average stack flow rate, 597 dscm/min (from Table 3.1-1).d From Table 3.4-1.

B Indicates that measured value is not greater than 5 times the blank value.Z Indicates a compound that is only tentatively identified and semiquantitated.

3-47

Table 3.4-11 Twenty Largest Peaks Identified in Run 6 MMS-SemivoIatile Train

Benzoic acidUnknown aAlkane aXylenes aBenzaldehydebis(2-Ethylhexyl)phthalateEthyl benzaldehydePhenolMethyl benzoateDichlorocyclohexaneEthyl benzoic acid aHydroxymethyl pentanoneMethyl hexenonelodobenzeneBromobenzeneAlkyl acetophenone aDecane + C3 benzeneAcetophenoneBiphenylEthyl methyl benzoate

Total amount (|ig)Target

TIC analyte"438 B

151 Z99 BZ77 BZ54 BZ

35.3 B34 BZ

32.931 BZ26 BZ23 BZ11 Z11 Z10 Z9.3 Z9 BZ

8.3 BZ6.3 BZ6.2 Z6.2 BZ

Stack gasconcb

(ng/dscm)14148322517111111108.37.33.53.53.23.02.92.72.02.02.0


1.4E-03 B 1.1E-02 B4.8E-04 Z 3.8E-03 Z3.1E-04 BZ 2.5E-03 BZ2.4E-04 BZ 1.9E-03 BZ1.7E-04 BZ 1.4E-03 BZ1.1E-04 B 8.8E-04 B1.1E-04 BZ 8.5E-04 BZ1.0E-04 8.2E-049.8E-05 BZ 7.8E-04 BZ8.2E-05 BZ 6.5E-04 BZ7.1E-05 BZ 5.7E-04 BZ3.5E-05 Z 2.8E-04. Z3.5E-05 Z 2.8E-04 Z3.2E-05 Z 2.5E-04 Z2.9E-05 Z 2.3E-04 Z2.8E-05 BZ 2.3E-04 BZ2.6E-05 BZ 2.1E-04 BZ2.0E-05 BZ 1.6E-04 BZ2.0E-05 Z 1.6E-04 Z2.0E-05 BZ 1.6E-04 BZ




3-48

Table 3.4-12 Twenty Largest Peaks Identified in Run 7 MM5-Semivolatile Train

Benzole acidEthyl benzaldehyde aXylenes aBenzaldehydeChlorinated unknownDichlorinated unknownAlkane aMethyl benzoateUnknown aPhenolEthyl benzole acid aEthyl acetophenone abis(2-Ethylhexyl)phthalateAlkyl acetophenone aBromobenzeneC14H2002 Alkyl cyclohexadienedioneEthyl methyl benzoateDecane + C3 benzeneHydroxymethyl pentanonelodobenzene

Total amount (ng)Target

TIC analyted472 B

340 BZ111 BZ55 BZ42 Z42 Z38 BZ37 BZ37 BZ

33.327 BZ18 BZ

13.0 B12 BZ11 Z11 Z11 BZ10 BZ10 Z10 Z

Stack gasconcb

(|ig/dscm)14610534171313121111108.45.74.03.63.43.43.43.13.13.1


1.5E-03 B 1.2E-02 B1.1E-03 BZ 8.4E-03 BZ3.4E-04 BZ - 2.7E-03 BZ1.7E-04 BZ 1.4E-03 BZ1.3E-04 Z 1.0E-03 Z1.3E-04 Z 1.0E-03 Z1.2E-04 BZ 9.4E-04 BZ1.1E-04 BZ 9.1E-04 BZ1.1E-04 BZ 9.1E-04 BZ1.0E-04 8.2E-048.5E-05 BZ 6.7E-04 BZ5.7E-05 BZ 4.5E-04 BZ4.0E-05 B 3.2E-04 B3.6E-05 BZ 2.8E-04 BZ3.4E-05 Z 2.7E-04 Z3.4E-05 Z 2.7E-04 Z3.4E-05 BZ 2.7E-04 BZ3.1E-05 BZ 2.5E-04 BZ3.1E-05 Z 2.5E-04 Z3.1E-05 Z 2.5E-04 Z




695

3-49

3.5 PCDD/PCDF Emissions Results

PCDDs/PCDFs present in the stack emissions were collected using EPA Method 23, todetermine total PCDD/PCDF concentrations and the concentration of 2,3,7,8-substituteddioxins and furans. The extraction, cleanup, and analysis for PCDD/PCDF were done inaccordance with EPA Method 23 with a few minor modifications as specified in the TrialBurn Plan. Analysis was performed by high resolution gas chromatography/high resolutionmass spectroscopy. Dioxin and furan levels were calculated by comparison to calibrationstandards and results are summarized in Table 3.5-1. The 2,3,7,8-substituted TCDD/TCDFresults are summarized in Table 3.5-2. In Table 3.5-3, each 2,3,7,8-TCDD/TCDF congenerwas converted to its 2,3,7,8-equivalent using EPA's 1989 2,3,7,8-TCDD toxic equivalencyfactors. The total 2,3,7,8-TCDD equivalent concentrations and mass emission rates areincluded in Table 3.5-3. The average 2,3,7,8-TCDD equivalent emission rate for all runs isshown in Table 3.5-4.

It was noted that the toluene QA rinses for the sample trains did contain some OCDD.This might have been interpreted to mean that the amounts of OCDD in the sample trainswas biased low. However, this is refuted by the fact that the toluene rinse for the blanktrain contained a greater amount than that found in the sampling train QA rinses, indicatingthat there is no such bias.

Surrogate recovery data for all the samples, including QC samples, are given inTable 3.5-5. All recoveries meet the QA objectives for PCDD/PCDF analysis. Other QCresults are shown in Table 3.5-6, including a laboratory control sample (blank XAD) whichwas spiked with all the 2,3,7,8 substituted dioxins and furans. Recoveries for these targetanalytes in the laboratory control spike were all within 85-126%, which met the QAobjective of 30-150%.

Two EPA audit samples were also analyzed along with the actual samples from theRisk Burn. MRI's analytical results for those two audit samples are shown in the tables andare being reported separately to EPA as required.

MRI-Appli«WUS20-28.S3B 3-50

AR3U696

Table 3.5-1. Dioxin/Furan Results for MM5-M23 Samples

AnalyteField

blank trainSample volume (dscm)a —Stack flow rate (dscm/m)aCarbon Dio.xide cone. (% dry basis)"

Dioxins (ng)TCDDPeCDDHxCDDHpCDDOCDD

Furans (ng)TCDFPeCDFHxCDFHpCDFOCDF

Total dioxins and furans (ng)

Total Concentration

Total Concentration(corrected to 7%

(ng/dscm)

(ng/dscm)O2 equiv)b

O.00130 U<0.00071 U

0.0110.0450.094

0.0140.012<0.046 U0.0550.051

0.28

,--

—

Run 53.16259710.4

0.6310.9690.7930.188 B0.135 B

0.3330.2620.2750.251 B0.101 B

3.94

1.25

1.02

Run 63.310590

10.5

0.5430.8000.6170.174 B0.144 B

0.2290.2770.2340.198 B0.069 B

3.29

0.992

0.803

Run?3.451603

10.4

0.4260.7320.6830.171 B0.174 B

0.2910.2170.1960.168 B0.074 B

3.13

0.908

0.742

a From Table 3.1-1.b Corrected to 7% O2 equivalent per Appendix B of the Trial Bum Plan.

U Indicates compound was analyzed for but not detected.B Indicates that the measured value is not greater than 5X the blank value.- Not applicable.

MRI-Applied\R3620-28.S3B

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3-53

AR3U699

Table 3.5-4. 2,3,7,8-TCDD Equivalent Average Emission RatesRun 5* Run 61 Run 71 Average

Emission rates for each run from Table 3.5-3.

Total 2,3,7,8-TCDDEquivalent EmissionRate (g/sec) 2.0E-10 1.6E-10 1.6E-10 1.7E-10

Total 2,3,7,8-TCDDEquivalent EmissionRate (Ib/hr) 1.6E-09 1.3E-09____1.3E-09 1.4E-09

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AR3U702

3.6 PCB Emissions Results

PCB emissions were sampled using the procedures in EPA Method 23 (PCDD/PCDF).Extraction and cleanup of samples was based on EPA Method 23, modified as appropriatefor PCB analysis instead of PCDD/PCDF. Samples were analyzed for PCBs by GC/MS perEPA draft Method 1668. PCB analysis results for the blank train and the method blanks areshown in Table 3.6-1, and results for stack samples are shown in Table 3.6-2. The blanktrain did contain some PCBs (37 ng) but the amount was less than in any of the sampletrains (181 to 260 ng).

Surrogate recovery data for the PCB analysis are included in Tables 3.6-1 and 3.6-2,which all were within the QA objective of 50-150%. However, there were no analysisresults for the toluene QA rinse for Run 7 since no laboratory surrogates were found;presumably because they were mistakenly not spiked. No portion of the original samplewas available that could be respiked and reanalyzed. This was not considered a seriousproblem since the results for the toluene QA rinses are not used in any calculation of results.

Recovery of PCBs spiked onto a blank XAD (i.e., laboratory control spike) shown inTable 3.6-3, met the QA objective of 50-170%. Recoveries determined in the initialprecision and recovery (DPR) samples shown in Table 3.6-4 met the QA objective of50-150% except for high recoveries of Di (BZ-5). Conversely, recovery of Di (BZ-5) was102% for the LCS (Table 3.6-3).

The results given in Table 3.6-2 were used to calculate the PCB emission rates shownin Tables 3.6-5, 3.6-6, and 3.6-7 and to calculate the average emission rate shown inTable 3.6-8.

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Table 3.6-3 Results for Laboratory Control Spike of XAD

Amount FoundAnalyte Spiked (ng)

Mono (BZ-2)Di(BZ-5)Tri (BZ-29)Tetra (BZ 50)Tetra (BZ 77)Penta (BZ 87)Penta (BZ 123)Penta (BZ 11 8)Penta (BZ 11 4)Penta (BZ 105)Penta (BZ 126)Hexa(BZ154)Hexa(BZ167)Hexa(BZ156)Hexa(BZ157)Hexa(BZ169)Hepta(BZ188)Hepta(BZ180)Hepta(BZ170)Hepta(BZ189)Octa (BZ 200)Deca (BZ 209)

Field Surrogates Spiked - QA Objective13C3-Mono13C15-DJ13C52-Tetra13C153-Hexa13C202-Octa13C209-Deca

1.172.041.53 ,2.451.773.648.759.099.19.138.383.66

14.514.914.218.15.2817.118.318.96.198.54

50-150%

Amount Spiked(nq)22242410101010104202020206202020610

Recovery(%)

QA Objective50-170%5910277618991889191918492737571918886929510385

6583898490110

Laboratory Surrogates Spiked - QA Objective 21-178%13077-Tetra13C118-Penta13C105-Penta130126-Penta13C156-Hexa13C169-Hexa13C180-Hepta

91998893127111112

MRl-ApplKd\R3«20-28.S3B 3-60

AR3U706

Table 3.6-4. Initial Precision and Recovery (IPR) Results (% Recovery)

Natives Spiked -Mono (BZ-2)Di (BZ-5)Tri (BZ-29)Tetra (BZ SO)Tetra (BZ 77)Penta (BZ 87)Penta (BZ 123)Penta (BZ 11 8)Penta (BZ 11 4)Penta (BZ 105)Penta (BZ 126)Hexa(BZ154)Hexa(BZ167)Hexa(BZ156)Hexa(BZ157)Hexa (BZ 169)Hepta(BZ188)Hepta(BZ180)Hepta(BZ170)Hepta(BZ189)Octa (BZ 200)Deca (BZ 2:09)

Field Surrogates13C3-Mono13015-Di13052-Tetra13C153-Hexa13C202-Octa13C209-Deca

IPR1QA Recovery Objective

88397a706512398921118896847488929093788570738980

IPR 250-150%

92435s676512491971089298837789959193788672779078

IPR 3

91402a64621218798 -1148798847192919092708575788176

IPR 4

89406a7069119100951089098857697929491738976837870

Average

90410'68651229496110899884759293'9192758673788576

Spiked - QA Recovery Objective 50-150%668296965983

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7182889492101131

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' Outside QA objective for IPRs of 50-1 50%, as discussed in narrative for Section 3.6.

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Table 3.6-8. Average PCB Emission Rate

PCB Emission rate (g/sec)1(lb/hr)a

Run5

8.19E-07

6.52E-06

Run 6

7.03E-07

5.58E-06

Run?

5.50E-07

4.36E-06

Average

6.91 E-075.49E-06

' From Tables 3.6-5 through 3.6-7

MRI-AppIietWU620-28.S3B 3-65

! !

3.7 Metals Analysis Results for MM 5 -MM Samples

Stack emissions were sampled for 22 metals using EPA Method 29. Analysis resultsfor the samples and for the simulated blank train comprised of field reagent blanks, aregiven in Tables 3.7-1 and 3.7-2. For calculating the concentration and emission rates shownin these tables, one half the detection limit was used for the non-detect amounts.

As expected, some metals were found in the samples and in the blank train (e.g., Ba,Al, Ca, Mg, K and Na). Smaller quantities of some other metals were found inapproximately equal amounts in the samples and blank train (e.g., Be, Cr, Cd, Ni, Se, Ag,Sb, Co, and V). Several, if not all, of these metals likely represent background levels of themetals in the filter media used in the sampling train.

EPA Method 29 includes procedures for blank correction of results. These blankcorrected values are given in Tables 3.7-1 and 3.7-2. Blank correction was performed usingthe notes to Method 29, sections 8.4.3 and 8.5.3. The blank correction methods specifiedin Method 29 do not adequately address the situations which arise when analyzing for Ba,Al, Ca, Mg, K, and Na. Even though closely matching values were found for theseelements in both the samples and the blanks, the method only allows a small blankcorrection. Thus, the calculated emission values shown in the tables are almost certainlyhigher than actual emissions.

Whenever the EPA Method 29 blank correction amount was greater than the amountmeasured in the sample, a value of zero was used for the blank corrected amount. Also, avalue of l/2 the detection limit was used whenever the blank corrected amount was a "lessthan" value.

Metal emission rates for each run (from Tables 3.7-1 and 3.7-2), and the averageemission rates over all runs, are shown in Table 3.7-3. Emission rates for some of thesemetals are biased high as noted above.

QA results for matrix spike sample and standard reference materials are given inTable 3.7-4. Recovery for the matrix spike samples met the QA objective of 65-135% forall the metals except Ag. As noted in Table G4-7a of the Trial Burn Plan, low recovery forAg was expected since any Cl present forms AgCl which is not recoverable in the EPAMethod 29 digestion process.

MRI-ApplKd\R3620-28.S3B 3-66

Analysis results for the standard reference materials (SRMs) met the accuracy objectiveof 75-125% for all the metals that were present in the SRM. As discussed in Appendix J, aQC check standard and an interference check sample were also analyzed and met the QAobjectives.

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AR3U720

Table 3.7-2. Analysis Results for MM5-MM (Metals) Train, Mercury Results—Blank Corrected

Mercury8

Run 5Rinse and filter, ugHNO3 implnger. ugFourth impinger.ugKMnO< implnger, ugHCI rinse, ug

Total, ug

Concentration, ug/dscmEmissions, g/sEmissions, Ib/h

Run 6Rinse and filter, ugHNO3 impinger, ugFourth impinger.ugKMnOj impinger, ugHCI rinse, ug

Total, ug


Run 7Rinse and filter, ugHN03 impinger, ugFourth impinger.ugKMnO4 impinger, ugHCI rinse, ug

Total, ug


Field Reagent BlankRinse and filter, ugHNO3 implnger, ugFourth impinger, ugKMnO4 impinger, ugHCI rinse, ug

Total . ug

Method Detection LimitRinse and filter, ugHNOj impinger, ugFourth impinger.ugKMnO« Impinger, ugHCI rinse, ug

Total . ug

Measured Measured values Blank correction Blank correctedValues usina 1/2 DL* amount total^

< 0.40 U 0.20 U< 6.51 U 3.26 U

0.38 J 0.38 J9.94 9.94277 277

291 X4 0 c 291 X4

96.2 X49.57E-04 X47.60E-03 X4

< 0.40 U 0.20 U6.42 J 6.42 J1.30 J 1.30 J327 3276.23 6.23

341 X4 0 c 341 X4

107 X41.06E-03 X48.37E-03 X4

0.69 J 0.69 J8.39 J 8.39 J

•= 0.21 U 0.11 U169 169

155 155

333 X4 0 c 333 X4

106 X41.07E-03 X48.46E-03 X4

< 0.40 U< 6.00 U< 0.20 U< 0.80 U< 1.00 U< 8.40 U

0.46111

9.4

MRI-Applied\R3(>20-:>8.S3B

" Mercury analysis performed by CVAA.b Blank corrected total Hg, = (Hg,,, - Hg,,,,) - (HgbK - Hgbh,,); per M29, Section 8.5.3.,eq. 29-8.

c Blank value less than MDL so the blank correction was conservatively set to zero." Using 1/2 detection limit for non-detect value from Table 3.7-2.Run 5 gas sample volume = 3.025 dscm. Stack gas flow rate = 597 dscm/min.Run 6 gas sample volume = 3.178 dscm. Stack gas flow rate = 590 dscm/min.Run 7 gas sample volume = 3.139 dscm. Stack gas flow rate = 603 dscm/min.

J indicates an estimated value; above the MDL but below the POL.U Indicates compound was analyzed but not detected (ND).X4 Sum includes ND and J values that represent less than 20% of the total.

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3"76

Table 3.7-4. Metals Analysis QA Results

Spiked laboratory reagent blanks— %QA objective: 65-135%

Metal

AsBaBeCdCr

PbHgNiSeAg

AlSbCaCoCu

FeMgMnKNa

VZn

Front Half

106989192 .97

9310198954a

951011069595

9496978894

9892

Front HalfDup

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9892

Back Half

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9396948998

9495

Recovery

Back HalfDup

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10091909492

9396949197

9397

Standard ReferenceMaterial (% Accuracy)QA objective: 75-125%

SRM#1

1249794102105

90NA10610090

NANANA10399

93NA101NANA

106100

SRM#1Dup

12111095104103

91NA1159398

NANANA10199

94NA101NANA

104102

Matrix Spike Recoveries for Hg (%)FrontHalf98

Dup

96

H2O2/HNO3Impingers

98Dup

96

KMnO4/H2SO4Impingers

99

Dup

99

HCI Rinse

102

Dup

106

' Recovery outside QA objective of 65-135%, as discussed in text of report:.

NA = Not applicable.

MRI-ApplioWUS20-28.S3B

AR3U7233-77

3.8 Hexavalent Chromium Emissions Results

The hexavalent chromium content of the MM5-CR train samples was measured by ionchromatography (1C) employing a postcolumn reactor (IC/PCR), according to the EPA BIFmethod titled "Determination of Hexavalent Chromium Emissions from StationarySources," as specified in 40 CFR 266, Appendix IX, Section 3.2.

Analysis results for the train samples and calculated emission rates, where one-half thedetection limit was used for non-detect values, are given in Table 3.8-1, including theaverage emission rate for all three runs. If the blank values had been used to correct thedata, as allowed in the method, the blank corrected emission rates would be zero.

The MS and MSD samples showed recoveries of 79% and 78%, as noted inTable 3.8-1. Also, an independently prepared audit sample, at a concentration of11.3 ug/L, showed recovery of 101%, which met the QA objective of 90-110%.

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AR3U725

3.9 Volatile Organic Analysis Results for Feed, Bottom Ash,and Fly Ash

Feed samples were taken during each run in accordance with the Trial Burn Plan andanalyzed for specific volatile organic compounds, with the results as shown in Table 3.9-1.Samples of the bottom ash and fly ash were also collected during each of the test runs. Thesamples were analyzed for specific VOCs, with the results given in Table 3.9-2.

Surrogate recoveries are also shown in Tables 3.9-1 and 3.9-2. Several weresomewhat outside the QA objective range of 70-120%. However, the lowest recovery was60% and the highest was 185%. As noted in Table G7-2A of the Trial Burn Plan, surrogaterecoveries for Method 8260 analytes are generally in the range of 70-120%, so the range ofthe recoveries for the samples is not considered significant.


AR3U726

Table 3.9-1. VOCs in Feed Samples

Analyte

Benzene

Toluenec/s-1 ,2-Dichloroethene

£-1 ,2-DichloroetheneTetrachloroethene

EthylbenzeneTrichloroethene

m-/p-Xy\eneo-Xylene

Chlorobenzene

Surrogate Recovery (%)1 ,2-Dichloroethane-o1,,

4-BromofIuorobenzeneToluene-ck

Methoddetection Method

limit blank(ug/kg) (ug/kg)0.5

0.5 1.5 J0.3

0.5

0.5

0.4

0.2

0.4 0.5 J

0.3

0.4

-QA Objective 70-1 20%

Concentration (Mg/kg)

Run 5 Run 6 Run 7

Rep 1

-

19-

--

172.6 J

111

55

330

116

134"

60*

Rep 2

_

45 42 44- - -_

- - •

18 21 16

2.5 J 3.3 J 2.8 J

124 140 100

60 63 47

390 450 370

113 122' 113

131' 129' 128'

76 72 132'

' Surrogate recovery outside QA objective range of 70-120% (for ash samples).- Indicates that analyte was not detected (i.e., < MDL).J Indicates an estimated value; above the MDL but below the PQL.


AR3U727

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3-82

AR3U728

3.10 Semivolatile Organic Analysis Results for Feed, BottomAsh, and Fly ash

Samples of the feed, bottom ash and the fly ash were collected during each of the testruns. The samples were analyzed for specific SVOCs, with the results given in Table 3.10-1and 3.10-2.

Surrogates spiked into the samples are also listed in Tables 3.10-1 and 3.10-2.Recoveries for these surrogates met the QA objective of 30-130%. Matrix spike sampleswere prepared in duplicate, for the feed, bottom ash, and fly ash, and the recovery for all theSVOCs are shown in Table 3.10-3. No QA criteria had been set up for these MS/MSDexcept for p-naphthylamine (30-130%). Most of the recoveries were good except for avery few of the compounds. Because of analytical problems with p-naphthylamine analysis,samples of the feed, bottom ash, and fly ash were sent to ECC for analysis even though the14-day holding time for bottom ash and fly ash would be exceeded by 2-4 days.

The ECC results for 3-naphthylamine are included in Tables 3.10-1 and 3.10-2. ECCresults given in Table 3.10-2 show that the concentration was below 55 ug/kg in both thebottom ash and in the fly ash. ECC surrogate recoveries were all in the acceptable range of30-130%. ECC also determined recoveries for a MS/MSD on the feed, bottom ash, and flyash. Those results are included in Table 3.10-3 and show that the ECC recoveries for thebottom ash were 83% and 79%; well within the acceptable range. MS/MSD recoveries forthe fly ash were lower (20% and 19%); both being outside the ECC limits of 25-100%.

MRI-App!iedR36:!0-28.S3C 3-83

AR3U729

Table 3.10-1. Semivolatile Organic Compounds in Feed Samples

1 ,2-Dichlorobenzene1 ,4-DichIorobenzene1 ,2,4-TrichlorobenzeneBenzo(k)fluoranthene.Benzo(a)pyreneBenzoic acidNaphthalenePhenanthreneBenzo(a)anthraceneChrysenePhenolPentachlorophenolFluoranthenePyreneBenzo(b)fluoranthene

p-Naphthylamine (by ECC)b

Surrogate Recoveries (%) -2-FluorophenolPhenol-d52-ChlorophenoI-d41 ,2-Dichlorobenzene-d4Nitrobenzene-d5°2-Fluorobiphenyl°2,4,6-TribromophenolTerphenyl-d14c

Detection limitbased on 1/5 lowest

standard3

(ng/kg)1,0001,0001,0001,0001,0001,0001,0001,0001,0001,0001,0001,0001,0001,0001,000

(550) d

Feed ( g/kg)

Rep 1UUUUUUUU

2,410UUU

1,8301,430U

(2,450)

Run 5Rep 21,360UUUU

1,090U

1,080J 3,240

UUU

J 1,750J 1,450

U

NA

Run 6

J 1,200 JUUUU

J UU

J 1,280 JJ 2,700 J

UUU

J 1,550 JJ 1,250 J

U

(3,430)

Run 7

1,570 JU

1,280 J1,160 J1,350 JUU

5,1303,810 J1,710 JUU

4,550 J3,800 J1,150 J

(4,040)

QA objective (30-1 30%)51555759

61(35)65(52)70

73(126)

6871747677798390

65697174

73(42)77(46)82

89(123)'

65707273

75(44)77(60)83

89(118)

" Detection limit equal to 1/5th the lowest standard. This is based on the area counts for the lowest standard, which weresufficiently high to enable detection and estimated quantitation of compounds whose area counts are 1/5 as high asthose for the lowest standard.

b Samples of feed were sent to ECC by MRI, and were analyzed within the holding time of 14 days.c Surrogate recoveries shown in parenthesis are for ECC analysis of samples.d ECC detection limit for p-Napthylamine in feed samples.

U Indicates compound was analyzed for but not detected.J Indicates an estimated value; above the MDL but below the PQLNA - Not analyzed

Note: A method blank was analyzed, but all analytes were non-detect.

MRI-AppliedR3«20-28.S3C 3-84

AR3U730

Table 3.10-2. Semivolatile Organic Compounds in Ash Samples

PhenolBis(2-chloroethyl) ether2-Chlorophenol1 ,3-Oichlorobenzene1 ,4-DichlorobenzeneBenzyl alcohol1 ,2-Dichlorobenzene2-MethylphenolBis(2-chloroisopropyl) ether4-MethylphenolW-Nitroso-di-n-propylamineHexachloroethaneNitrobenzeneIsophorone2-Nttrophenol2,4-DimethylphenolBenzole acidBis(2-chloroethoxy) methane2,4-Dichlorophenol1 ,2,4-TrichlorobenzeneNaphthalene4-ChloroanilineHexachlorobutadiene4-Chloro-3-methy!phenol2-MethylnaphthaleneHexachlorocyclopentadiene2,4,6-Trichlorophenol2,4,5-Trichlorophenol2-Chloronaphthalene2-NltroanilineDimethyl phthalateAcenaphthylene3-NitroanilineAcenaphthene

DetectionLimit:

Based on1/5 loweststandard •(pg/kg)BottomAsh/

Fly Ash140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70

Bottom ash (ug/kg)

Run5

Rep. 1UUUUUUUUUUUUUUUU

2,060 JUUUUUUUUUUUUUUUUU

Rep. 2UUUUUUUUUUUUUUUU


Run6

UUUUUUUUUUUUUUUU


Run 7 .

UUUUUUUUUUUUUUUU

250 JUUUU

. UUUUUUUUUUUUU

Flyash(ug/kg)

Run5

Rep. 1UUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUU

Rep. 2UUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUU

Run 6

UUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUU

Run 7

UUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUU


MRI-AppliedR3S20.28.S3C 3-85

AR'3ll*73

Table 3.10-2 Continued(Semivolatile Organic Compounds in Ash Samples)

DetectionLimit •(ug/kg)Bottom

Bottom ash (ug/kg)

Run 5Ash/Fly Ash Rep. 1

2,4-Dinitrophenol4-NrtrophenolDibenzofuran2,4-Dinitrotoluene2,6-DinitrotolueneDiethyf phthalate4-Chlorophenyl phenyl etherFluorene4-Nitroaniline4,6-Dinitro-2-methylphenol/V-Nftrosodiphenylamine4-Bromophenyl phenyl etherHexachlorobenzenePentachlorophenolPhenanthreneAnthraceneDi-n-butyl phthalateFluoranthenePyreneButyl benzyl phthalate3,3'-DichlorobenzidineBenz[a]anthraceneBis(2-ethylhexyl) phthalateChryseneDi-n-octyl phthalateBenzo[jb]fluorantheneBenzo[k]fluorantheneBenzo[a]pyrenelndeno[1 ,2,3-cd]pyreneBenzo[g,/J,/]perylene

p-Naphthylamine (by ECC)b

140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70

(16/9)

UUUUUUUUUUUUUUUUUUUUUUUUUUUUUU

(U)

Rep. 2UUUUUUUUUUUUUUUUUUUUUUUUUUUUUU

(NA)

Run 6 Run 7 .

Fly ash (ug/kg)

RunS Run 6 Run 7

Rep. 1 Rep. 2UUUUUUUUUUUUUUUUUUUUUUUUUUUUUU

(U)


(U)


(U)

UUUUUUUUUUUUUUUUUUUUUu •Uuuuuuuu

(NA)

UUUUUUUUUUuuuuuuuuuuuuuuuuuuuu

(U)

UUUUUUUUUUUUUUUUUUUUUuuuuuuuuu(U)

Surrogate Recoveries (%)-QA Objective 30-130%.2-FluorophenoIPhenol-d52-chlorophenol-d41 ,2-Dichlorobenzene-d4Nitrobenzena-d5e2-Fluorobiphenyt°2,4,6-TribromophenolTerphenyl-d14c

76838186

86(62)86(68)86

82(94)

6771697377727273

64696871

77 (83)72(90)76

69(90)

6470687278(110)72(71)7372(97)

64706970

77 (82)72(88)72

76(120)

6066646775707175

66727073

78 (53)72(71)71

77(112)

68747374

80(66)75 (81)73

79(116)

a Detection limit equal to 1/5th the lowest standard. This is based on the area counts for the lowest standard, which weresufficiently high to enable detection and estimated quantitation of compounds whose area counts are 1/5th as high as those forthe lowest standard.

b Samples were sent to ECC after receipt at MRI. Thus, the 14 day holding time was exceeded by 2-4 days.c Surrogate recoveries shown in parenthesis are for ECC analysis of samples.

U Indicates compound was analyzed for but not detected.J Indicates an estimated value, above the detection limit, but below the PQL.NA Not analyzedNote: A method blank was analyzed, but all analytes were non-detect.

MRJ-AppliedR3620-28.S3C 3-86

AR3U732

Table 3.10-3. Matrix Spike Recoveries for Feed, Bottom Ash and Fly Ash

Feed Bottom ash% Recovery % Recovery

(QA Objective 30-1 30%) (QA Objective 30-1 30%) .MS MSD MS MSD

PhenolBis(2-chloroethyl) ether2-Chlorophenol1 ,3-Dichlorobenzene1 ,4-DichlorobenzeneBenzyl alcohol1 ,2-Dichlorobenzene2-MethylphenolBis(2-chloroisopropyl) ether4-Methylphenol/V-Nitroso-di-W-propylamineHexachloroethaneNitrobenzeneIsophorone2-Nrtrophenol2,4-DimethylphenolBenzole acidBis(2-chloroelhoxy) methane2,4-Dichlorophenol1 ,2,4-TrichlorobenzeneNaphthalene4-ChloroanilineHexachlorobutadiene4-Chloro-3-methylphenol2-MethylnaphlhaleneHexachlorocyclopentadiene2,4,6-Trichlorophenol2,4,5-Trichlorophenol2-Chloronaphthalene2-NitroanilineDimethyl phthalateAcenaphthylene3-NitroanilineAcenaphthene

79 63 85- - 77- 75- 7781 65 78_ _ gt

88 71 7965 .

- - 80- 63— — 71- - 76- 83- - 89

75- - 29"35 27* 5*- 79

7691 74 8193 75 89- - 48- - 79- - 83- 90

16"- - 65- - 93- - 83- - 77

90- - 85

76- - 91


92888384855'877085857582899985401068986899756889310018"7311195891029585101

Fly ash% Recovery

(QA Objective 30-1 30%)MS MSD82818179805'8275846773778892824917*8177838659828491377489868089868292

84848483846"8577908574828595804116'8482848965848795357986918495919097

MRI-AppHcdR3620-28.S3C

AR3U7333-87

Table 3.10-3 Continued(Matrix Spike Recoveries for Feed, Bottom Ash and Fly Ash)

Feed% Recovery

(QA Objective 30-1 30%)MS MSD

2,4-Dinrtrophenol4-NftrophenolDibenzofuran2,4-Dinitrotoluene2,6-DinitrotolueneDiethyl phthalate4-Chlorophenyl phenyl etherFluorene4-Nitroaniline4,6-Dinitro-2-methylphenolA/-Nitrosodiphenylamine4-Bromophenyl phenyl etherHexachlorobenzenePentachlorophenolPhenanthreneAnthraceneDi-n-butyl phthalateFluoranthenePyreneButyl benzyl phthalate3,3'-DichlorobenzidineBenzfajanthraceneBis(2-ethylhexyl) phthalateChryseneDi-n-octyl phthalateBenzo[b]fluorantheneBenzo[k]fluorantheneBenzo[a]pyrenelndeno[1 ,2,3-cd]pyreneBenzo[g,/y]perylene

P-Naphthylamine (by ECC)

------------—86115--123127--129-105-959392——

(30)

--—----------7383--95103--99-86—797676--

(38)

Bottom ash% Recovery

(QA Objective 30-1 30%) .MS MSD367510986849790929979918891749084981099690699210891898484829189

(83)

4987125979210810210310891100961008499921091241089980102117102101851029410198

(79)

Fly ash% Recovery

(QA Objective 30-1 30%)MS MSD5467108858294899310283908890708586951061009067859990918184838783

(20)b

58771159287102949710888949395759093103113106"95749311398988597919592

(19)"

Surrogate Recoveries (Ve)-QA Objective 30-130%2-FluorophenolPhenol-d52-chlorophenol-d41 ,2-Dichlorobenzene-d4Nttrobenzene-d5 c2-Fluorobiphenyl2,4,6-Tribromophenol cTerphenyl-d14c

60707070

77(76)78

83(89)89(116) •

52575859

66(70)67

73(88)80(105)

65706870

75(73)73

74(103) «72(111)

69757375

82(82)80

83(101)79(107)

67727170

77(89)70

71(99)72(125)

68767474

81(84)77

78(91)78(109)

a Recovery outside QA objective range of 30-130%.b Recovery outside ECC limits of 25-100%.c % Recovery shown in parentheses is for surrogates spiked into samples by ECC for p-Naphthylamine analysis.- Not spiked because not a target analyte in the feed.Note: Spike level was 50 ug equal to 10,000 ug/kg for feed.

Spike level was 15 ug equal to 1,000 pg/kg for bottom ash and 500 ug/kg for fly ash.ECC spike level was 6,670 ug/kg for p-Naphthylarnine in feed.ECC spike level was 833 ug/kg for p-Naphthylamine in bottom ash and fly ash.

MRI-Appli«iR3620-28.S3C _,_ 3-66

AR3U731*

3.11 PCDD/PCDF Analysis Results for Bottom Ash and FlyAsh

Samples of the bottom ash and of the fly ash were collected during each of the test runsfor 2,3,7,8-substituted dioxins/furans. The extraction, cleanup, and analysis for thesedioxins/furans were done in accordance with EPA Method 8290. Analysis was performedby high resolution gas chromatography/high resolution mass spectroscopy with selected ionmonitoring. The 2,3,7,8-substituted PCDD/PCDF results for the bottom ash and the fly ashsamples are given in Tables 3.11-1 and 3.11-2. Duplicate analysis of samples from one runis included in the tables.

Recoveries for the laboratory surrogates spiked into the samples are included inTables 3.11-1 and 3.11-2. The recoveries were all within the QA objective of 40-120%.Table 3.11-3 provides QC results pertaining to the D/F analysis of bottom ash/fly ashsamples, consisting of MS/MSD and a laboratory control spike. Recoveries for thelaboratory control spike were good; all within a range of 72-112%. Recoveries for the MSand MSD were also good, in the range of 70-113%.

The 2,3,7,8-substituted dioxin/furan results given in Tables 3.11-1 and 3.11-2 wereused to calculate the 2,3,7,8-TCDD equivalent concentration using the 1989 EPA factors.These results are presented in Tables 3.11-4 and 3.11-5.

MRI-ApplredR3620-28.S3C 3-89

Table 3.11-1. 2,3,7,8-Substituted Dioxin/Furan Results for Bottom Ash SamplesConcentration (ng/kg)

AnalvteDioxins2,3,7,8-TCDD1,2,3,7,8-PeCDD1,2,3,4,7,8-HxCDD1,2,3,6,7,8-HxCDD1,2,3,7,8,9-HxCDD1 ,2,3,4,6,7,8-HpCDD1,2,3,4,6,7,8,9-OCDD

Furans2,3,7,8-TCDF1,2,3,7,8-PeCDF2,3,4,7,8-PeCDF1, 2,3,4 ,7,8-HxCDF1,2,3,6,7,8-HxCDF2,3,4,6,7,8-HxCDF1,2,3,7,8,9-HxCDF1, 2,3,4 ,6,7,8-HpCDF1,2,3,4,7,8,9-HpCDF1 ,2,3,4,6,7,8,9-OCDF

Labeled Analogs (\QB)13C-2,3,7,8-TCDD13C-1,2,3,7,8-PeCDD13C-1,2,3,6,7,8-HxCDD1 3C-1 ,2,3,4,6,7,8-HpCDD13C-OCDD

13C-2,3,7,8-TCDF13C-1,2,3,7,8-PeCDF13C-1,2,3,4,7,8-HxCDF13C-1.2.3.4.6.7.8-HDCDF

MethodBlank

<0.0368 U<0.138U<0.798 U<0.0711U<0.0874 U0.786 J1.62J

<0.0578 U<0.105U<0.102U<0.0557 U<0.0455 U<0.0584 U<0.0623 U<0.0691 U0.752 J0.481 J

IQS

7064658172

665865"67

Run 5

<0.0710U<0.149U<0.140U<0.125U<0.153U

6.14J36.8 J

<0.0872U<0.136U<0.133U<0.0601U .<0.0491 U<0.0630 U<0.0672U<0.0506U<0.582U<0.0996U

Run 5Duplicate

<0.0431 U<0.133U0.209 J0.887 J1.12J6.85 J44.8 J

0.302 J<0.0687 U<0.0670 U<0.0470 U<0.0384 U

0.316 J<0.0525 U<0.0615U<0.0708 U<0.0758 U

Run 6

O.149U<0.159U<0.133U0.820 J0.860 J10.3J68.3

<0.0864 U<0.132UO.129U<0.0850 U<0.0694 UO.0890 U<0.0950 U0.765 J0.444 JB1.25JB

Run 7

<0.113U<0.160U<0.130U<0.116U

1.35J7.20 J43.0 J

<0.0913U<0.110U<0.107U<0.0604U<0.0493U<0.0633U<0.0675 U

0.61 3 J<0.0870U

0.621 JB

Surrogate Recoveries (%) — QA objective 40-120%

5960717370

54538962

5756687063

53528361

5352657261

49508861

5656677963

54538065

U Indicates compound was analyzed for but not detected.J Indicates an estimated value; above the MDL but below the PQL.B Indicates that measured value is not greater than 5 times the blank value.

MRI-Appli«dR3«20-28.S3C 3-90

AR3U736

Table 3.11-2. 2,3,7,8-Substituted Dioxin/Furan Results for Fly Ash SamplesConcentration (ng/kg)

AnalvteDioxins2,3,7,8-TCDD1,2,3,7,8-PeCDD1,2,3,4,7,8-HxCDD1,2,3,6,7,8-HxCDD1,2,3,7,8,9-HxCDD1,2,3,4,6,7,8-HpCDD1,2,3,4,6,7,8,9-OCDD

:urans2,3,7,8-TCDF1 ,2,3,7,8-PeCDF2,3,4,7,8-PeCDF1,2,3,4,7,8-HxCDF1,2,3,6,7,8-HxCDF2,3,4,6,7,8-HxCDF1,2,3,7,8,9-HxCDF1,2,3,4,6,7,8-HpCDF1,2,3,4,7,8,9-HpCDF1,2,3,4,6,7,8,9-OCDF

.abeled Analoas (\QS)13C-2,3,7,8-TCDD130-1,2,3,7,8-PeCDD130-1,2,3,6,7,8-HxCDD130-1,2,3,4,6,7,8-HpCDD13C-OCDD

130-2,3,7,8-TCDF130-1,2,3,7,8-PeCDF130-1,2,3,4,7,8-HxCDF130-1,2,3,4,6,7,8-HpCDF

MethodBlank

<0.0368U<0.138U<0.798 U<0.0711U<0.0874 U0.786 J1.62J

<0.0578 U<0.105U<0.102U<0.0557 U<0.0455U<0.0584U<0.0623 U<0.0691 U0.752 J0.481 J

7064658172

66586567

Run5Run 5

Duplicate

<0.0671U <0.0887U<0.141 U<0.110U<0.0980 U<0.120U

3.73 JB6.01 JB

0.0763 UO.0884U0.648 J1.19J0.837 J0.630 J

<0.0669 U2.95 J

. 0.456 JB<0.161 U

IQS Surrogate

5349565754

51485552

<0.149U0.202 J0.478 J<0.189U

4.24 J5.71 JB

0.925 J<0.159U<0.155U

1.15J0.269 J0.998 J<0.114U

3.15J<0.137U

2.78 J

Recoveries

5250666966

49486561

Run 6

<0.104UO.185U<0.0994 U

2.35 J<0.109U

9.59 J9.61 J

0.731 J<0.0916U

1.08J1.53J1.29J1.33J

<0.0818U4.62 J1.32JB5.19J

Run 7

<0.0801 U0.621 J1.12J3.33 J4.35 J12.6J9.53 J

<0.0541 U0.505 J

<0.0838 U1.62J1.20J

<0.0834 U<0.0890 U

3.06 J1.09JB3.55 J

(%)— QA objective 40-120%

5253636460

49506557

6859596054

66566253

U Indicates compound was analyzed for but not detected.J Indicates an estimated value; above the MDL but below the PQLB Indicates that measured value is not greater than 5 times the blank value.

MRl-AppIicdR3620.28.S3C 3-91

AR3U737

Table 3.11-3. QC Results for 2,3,7,8-Substituted Dioxin/Furan Samples


Furans2,3,7,8-TCDF1,2,3,7,8-PeCDF2,3,4,7,8-PeCDF1 ,2,3,4 ,7,8-HxCDF1,2,3,6,7,8-HxCDF2,3,4,6,7,8-HxCDF1,2,3,7,8,9-HxCDF1 ,2,3,4,6,7,8-HpCDF1,2,3,4,7,8,9-HpCDF1,2,3,4.6,7,8,9-OCDF

.abeled Analoas (IQS)13C-2,3,7,8-TCDD13C-1,2,3,7,8-PeCDD13C-1,2,3,6,7,8-HxCDD13C-1,2,3,4,6,7,8-HpCDD13C-OCDD

13C-2,3,7,8-TCDFISC-I .SJ.S-PeCDF130-1,2,3,4,7,8-HxCDF13C-1,2,3,4,6,7,8-HpCDF

MatrixSpike*

(% Recover^

7082868295102113

108929172637263108102111

IQS Surroqate

7064737961

636410270

MatrixSpike Dup.*(% Recover^

7586928611296113

1009110172Q27570106

Laboratory control spike% Recovery

QA objective 50-1 50%

72828881112101107

9497101999310397110

101 106104 108

Recoveries (%) — QA objective 40-120%

6763596358

54578556

5959616562

56556157

Matrix spike of bottom ash.

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3.12 Herbicides Analysis Results for Feed, Bottom Ash andFly ash

Samples of the feed, bottom ash and fly ash collected during each of the test runs wereanalyzed for herbicides. The samples were extracted with alkaline acetone/ether,derivatized with diazomethane to form the methyl esters and analyzed using GC/ECD.

The analysis results are summarized in Tables 3.12-1 and 3.12-2, which include thesurrogate recoveries. One of the surrogate recoveries was somewhat low (40%) for thefeed in Run 6, and for the bottom ash in Run 7 (45%). Both surrogates were somewhatlow for the fly ash in Run 7 (37% and 47%) and one was low in Run 6 (39%). Also, alaboratory control spike (LCS) was prepared and analyzed for herbicides. The recoveries,shown in Table 3.12-3, were generally good, except for 2,4-DB at 22% recovery andDalapon at 33% recovery. Analysis for herbicides has historically shown considerablevariability in such recovery data.

Samples of the feed, bottom ash, and fly ash were sent to ECC for Fenac analysis, eventhough the 14-day holding time would be exceeded, after analytical problems wereencountered in the MRI analysis for Fenac, as noted in the Risk Burn No. 1 report. ThoseECC results are included in Tables 3.12-1, 3.12-2 and 3.12-3. The ECC results met all therequired QC criteria.

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Table 3.12-3. Summary Table for Herbicide Laboratory Control Spike b

LCS

Analvtes2,4-D2,4-DB2,4,5-T2,4,5-TPDalaponDicambaDichloropropDinosebMCPAMCPP

Fenac (by ECC)

Surrogates (% Recovery) — QA2,4-Dichlorophenylacetic acidTriclopyrTriclopyr (by ECC)

Spike Level(ua/ka)1,0001,0001001002,5001001,000500

100,000100,000

(1,200)

Objective 50-1 60%

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(1070)

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(89)

104102(106)

a Indicates recovery below 35%, although no specific objective has been established.b Laboratory control spike was done on a previously analyzed fly ash sample; not one of the fly ash

samples from Risk Burn No. 2.

D Indicates compound identified in an analysis at a secondary dilution factor.

Note: MRI sent the samples of feed, fly ash and bottom ash to ECC, who analyzed them for Fenacand performed analysis of a matrix spike and matrix spike duplicate, with results as follows:

% RecoveryECC Limits: 35-150%

MS MSPBottom Ash 86 127Fly Ash 60 80Feed 99 101

MRI-Appli«UU620-28.S3C 3-98

3.13 Metals Analysis Results for Feed Samples and TCLPMetals in Bottom Ash, Fly Ash, and Scrubber WaterSamples

Samples of feed taken in each run were analyzed for six metals (As, Be, Cd, Cr, Pb andHg) by acid digestion and analysis by ICP (or CVAA for Hg). Those analysis results arepresented in Table 13.1-1. This table includes recoveries for the LCS and for the MS/MSD,all of which met the QA objective of 70-130%.

Samples of the bottom ash, fly ash, and scrubber water were collected during each ofthe test runs. The samples were extracted using EPA SW846 Method 1311 and thenanalyzed for the TCLP metals (Ag, As, Ba, Cd, Cr, Hg, Pb, and Se), with the results givenin Table 3.13-2.

Table 3.13-2 includes results for the extraction fluid blank and recovery data for alaboratory control spike and for a matrix spike/matrix spike duplicate (MS/MSD). Theserecoveries were all within the QA objective of 70-130%.

It may be noted in Table 3.13-1 that non-detect values for scrubber water samples areconsiderably higher than for the ash samples. In fact, the non-detect values for Cr, Pb, andAg exceeded the PQLs given in the Trial Burn Plan. The reason for this is that the scrubberwater samples had a level of total dissolved solids that necessitated dilution down to a levelthat could be tolerated by the analytical instruments.

MRI-AppliedR3«20-28.S3C 3-99

Table 3.13-1. Metal Concentration in FeedConcentration (ug/g or mg/kg)

Analysis by

FeedRun 5Run 5 dup

Run 6Run 7'

Method Blank

Spike Recovery (%) -LCSMatrix spikeMatrix spike dup.

ICPAs

7.04 J7.66 J

6.02 J3.49 J

< 2.88 U

ICPBe

0.690.70

0.540.76

< 0.03 U

ICPCd

<0.21 U< 0.22 U

0.35 J< 0.24 U

<0.23 U

ICPCr

26.626.6

21.126.7

< 0.32 U

ICPPb

37.736.0

33.638.1

<1.89U

CVAAHa

0.52 J0.25 J

< 0.20 U0.26 J

< 0.20 U

QA Objective 70-1 30%9299101

100100100

105102101

105101101

102103101

948786

U Indicates compound was analyzed but not detected.J Indicates an estimated value, above the MDL but below the PQL.B Indicates that the value is not greater than 5X the blank value.

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3.14 Feed Characteristics

Feed samples were taken in each run and sent to Galbraith Laboratories for ASTMmethod analysis for total solids, moisture, ash, heating value, and chlorine content. Resultsof those analyses are presented in Table 3.14-1.

As part of the above analysis, MRI submitted performance evaluation samples (PES)for analysis. Those results are given below.

Results for Performance Evaluation Samples

Heating value (Btu/lb)Chlorine (%)

Ash (%)

Measured value

14,330

33.72

4.77

True value13,463

33.3

4.74

Accuracy

106%

101%

101%

MRI-AppKedR3«20-28.S3C 3-102

Table 3.14-1. Feed CharacteristicsRun 5"

CharacteristicTotal solids (%)

Moisture, as % loss ondrying (%)Ash (%)Heating value (Btu/lb)

Chlorine (ppm)

Rep1

84.19

15.81

78.40

293

300

Rep 2

83.82

16.18

78.04

282

280

Run 6

83.87

16.13

77.87

380

250

Run 7

84.21

15.79

78.11

161

250

a Samples analyzed in duplicate

MRI-ApplicdR3620-28.S3C 3-103

3.15 Continuous Emission Monitoring Results for SO2

In addition to the facility CEMs, MRI performed continuous monitoring for SO2 (perEPA Method 6C) during each run. The one-minute readings from these two monitors arecontained in Appendix N. A summary of those results is shown in Table 3.15-1.

MRI-AppUedR3620-28.S3C 3-104

AR3U750

Table 3.15-1. Summary of SO2 Monitoring Data

Run 5Run6Run 7

min000

S02 (ppm dry basis)max avg0.4 <0.10.4 <0.10.3 <0.1

MRI-ApplicdR3620.28.S3C 3-105

Section 4Quality Assurance Report

Based on the Quality Assurance (QA) reviews and audits described below, and with therelatively few minor exceptions noted in this summary, the reported test results for RiskBurn No. 2 were found to be complete relative to the Trial Burn Plan, traceable tosupporting documentation, and accurately reported as determined by results of performanceaudit samples, internal quality control (QC) data, and calculation checks of representativetest results. (A summary of QA/QC issues and concerns is given in Table 4-0, as noted inSection 4.1.)

The validity of the data is demonstrated by comparing the QA/QC results with the dataquality objectives specified in the Project Quality Assurance Plan (Trial Burn Plan for theDrake Chemical Superfund Site's Mobile Hazardous Waste Incinerator, datedSeptember 20, 1996). This comparison (see Tables 4-1 through 4-4) shows that over 90%of the accuracy, precision, and method performance objectives were met. This is based onthe number of QA objectives that were met, or met with minor exceptions, compared withthe total number of QA objectives. The minor exceptions are noted in Tables 4-1, through4-4.

The following quality assurance (QA) activities were performed in conjunction with theRisk Burn No. 2 test:

• Performance Evaluation (PE) samples were incorporated into the analyses tomeasure accuracy. Results for these PE samples are presented in Table 4-1.

• Surrogate recoveries, spike recoveries, precision and method blank data wereevaluated relative to the data quality objectives of the project QA plan (seeTable 4-2). Method blank and recovery QC results are presented in the previous textwith the sample results; precision results are presented in this section.

• The final report (in draft form) was independently reviewed and representative datafrom Run 5 were audited for correct calculation of sample results and derivedemission rates. These were found to be accurately reported and traceable tosupporting records.

MRI-Appli«I\R3620-28.s4 ' 4-1

AR3U752

4.1 Discussion

On the basis of this extensive QA review, only two issues were identified which meritfurther discussion. The actions taken to resolve these issues are also discussed as well asthe potential impact these difficulties have on the subsequent use of the test results.

• Initial analysis results for recovery of Fenac and p-naphthylamine were very low orerratic for spiked feed and bottom ash samples. Because of these problems, sampleswere sent to ECC for analysis. This corrective action, and the associated ECC QCresults, indicated that the initial analytical problem did not have any impact on thedata in the report. Although the ECC analysis necessarily exceeded the holding timeby 2-5 days, it is not expected that this would significantly affect the results.

• Silver recoveries are low in the front half/back half train sample components due tomethod characteristics relative to this metal alone. This was expected, as noted inAppendix G of the Trial Burn Plan. Overall silver emission data should beconsidered as estimated values and possibly higher than reported.

A summary of QA/QC issues, along with corrective actions and assessment of theirimpact on the data and test results, is given in Table 4-0. Minor exceptions are also notedin subsequent tables of this section.

MRI-Applied\R3«20.28.s4 4-2

AR3U753

Table 4-0. Summary of Issues/ConcernsRisk Burn No. 2

Description ofQC Issue or Concern

Table 2-2 — Stopped samplingfor 3 min during Run 5 due tostoppage of ash dischargeconveyor.

Table 2-2 and 3.1-1— Failedfinal pitot leak check on SV trainin Run 7.

Table 3.2-1 — Matrix spikerecovery for caustic wassomewhat high at 128%.Tables 3.3-1 through 3.3-3—Benzene quantity saturated theGC/MS detector for the primaryion.Tables 3.3-1 through 3.3-3 —High recovery for one of thethree surrogates (1 ,2-DCE-d4)due to interference frombenzene.

Table 3.3-1 through 3.3-3—Interference from benzenenecessitated quantitation of 1 ,2-DCE using a secondary ion.

Tables 3.3-4 through 3.3-6— Afew VOCs present in methodblank at levels higher than incondensate samples.

Table 3.3-4 — VOST condensatesample from Train B in Run 5broken during shipment.

Table 3.4-7 — Matrix spike ofXAD showed somewhat lowrecovery of 36% forp-Naphthylamine

Corrective Action orResolution

None since feed stoppage wasless than 5 min.

Used pitot readings from PCBtrain (done at the same time andat the same level) to calculateisokinetic on SV train.

No corrective action since allsamples were non-detect.

Benzene was quantitated using asecondary ion.

Quantitated off a secondary ionbut recoveries did not improve.

Quantitation done using asecondary ion.

None since some compoundsare normally found in methodblank.

Calculations based onconcentrations found in Train Acondensate analyzed by SIM.

None. While recovery is belowplan guidelines of 50-1 50%, it isconsistent with EPA Method8270 recovery information.

Assessment of Impacton Test Results

None

None. Calculations showed thatSV train met isokinetic.

None. All samples were non-detect.

None

Impact on data was minimal andat worst might indicate thatreported values for someanalytes are higher than actual.

No impact on results.

Reported emission rates for thefew VOCs may be higher thanactual emission rates.

None because the concentrationof analytes in Train Acondensate should be the sameas Train B condensate.None.

MRI-AppIied\R3620-28.«4 4-3

AR3U75U


Table 3.4-7— XAD matrix spikerecoveries out of limits for 4 outof 56 compounds spiked (~7%)as follows:•Pentachlorophenol (41%)•3,3-Dichlorobenzidine (33%)•2,4-Dinitrophenol (14%)•Hexachlorocyclopentadiene(29%)

Tables 3.4-9 through 3.4-12—TIC levels were comparablebetween blank and samples.

Table 3.6-2— No PCB analysisresults for toluene QA rinse inRun 7, because laboratorysurrogates were mistakenly notspiked into samples.

Table 3.7-1 — Several metalspresent in simulated blank trainand sample trains in approx.equal amounts.

Table 3.7-4 — Low recovery ofAg in matrix spikes.

Table 3.9-1 and 3.9-2 — Severalof the surrogate recoveries weresomewhat outside QA objectiveof 70-1 20% for VOCs in feedand ash samples.

Table 3.10-2 — Requiredreanalysis of ash samples forp-Naphthylamine by ECCcaused extraction holding time tobe exceeded by 1 to 5 days.

Table 3.1 0-3— MS/MSDrecoveries were low, butconsistent, for 1 out of 64 (~2%)semivolatile compounds spikedin feed, 4 out of 64 (-6%) spikedin bottom ash, and 2 out of 64(~3%) spiked into flyash.


None. Majority of matrix spikerecoveries were within planguidelines.

No corrective action warranted.

Problem investigated but nocorrective action possible.

None. No corrective actiontaken since these metals areubiquitous and are likelyconstituents of the filters used insample trains.

Problem was expected aspointed out in the Trial BurnPlan. Analysis, per EPA Method29, is not efficient for recovery ofAg.No corrective action takenbecause recoveries were mostlyhigh (above 120%) and problemwas considered to be minorsince lowest recovery was 60%and highest was 185%.None possible due to "one of akind" nature of samples.

None. Majority of matrix spikerecoveries were within planguidelines.


None

TIC emission rates may bereported high since they werealso present in blank.

None. Toluene QA rinse data isnot used in any calculation ofresults.

Reported results will be highsince Method 29 limits theamount of blank correctionallowed.

Indicates that emission resultsfor Ag are uncertain, and may behigher than reported. However,results from analysis of SRMshowed good recovery.None.

None. Degradation notexpected in this time frame dueto sterile nature of matrix and thefact that samples were sealed,stored at 4°C, and protectedfrom light.None.

MRJ-Applkd\R3620-28.«4 4-4

AR3U755


Table 3.10-3— MS/MSD resultsshowed somewhat low recoveryfor p-Naphthylamine in flyash(20%/19%)

Table 3.12-1 and 3.12-2— Lowsurrogate recoveries for onesurrogate in one feed sample,and one bottom ash sample, andtwo surrogates in two flyashsamples.

Table 3.12-2 — Requiredreanalysis of ash samples forFenac by ECC caused extractionholding time to be exceeded by 2to 5 days.

Table 3.12-3 — LaboratoryControl Spike (LCS) ofherbicides onto flyash yieldedrecoveries which were slightlybelow plan guideline of 35% for2,4-DB (22%) and for Dalapon(33%).

Table 4-1 — One performanceaudit sample, for CI" in 0.1 NH2SO4, showed slightly highrecovery of 115% (QA objective90-110%)

Tables 4-5 through 4-15— Afew of the precision values in thetables were outside QAobjectives.

Appendix B (pages B-193,B-204, and B-205)— On these 3traceability sheets the firsttransfer of the samples wasinadvertently not recorded.


None since recovery was onlyslightly below ECC limits of25-100%.

No corrective action taken sincerecoveries were only slightlybelow QA objective of 50-160%,with the lowest being 37%.

None possible due to "one of akind" nature of samples.

None. Most samples and allLCS surrogate recoveries werein acceptable range and majorityof LCS spike recoveries (9 out of1 1 , or 82%) were within planguidelines.

None, since result was onlyslightly above QA objective.

None since over 98% of theprecision values were within QAobjectives.

This error was noted on thetraceability sheets.


None. Based on the fact thatrecovery of p-Naphthylamine inbottom ash was good(79%/83%) and none wasdetected in bottom ash. It ishighly unlikely that flyash wouldcontain higher levels ofP-Naphthylamine than bottomash.

None. Recoveries were onlyslightly below QA objective.

None. Degradation notexpected in this time frame dueto sterile nature of matrix and thefact that samples were sealed,stored at 4°C, and protectedfrom light.None.

None, based on the fact thatresult was only slightly above QAobjective and audit sample hadbeen spiked at high level(123 mg/L) whereas all sampleswere non-detect at 0.1 0 mg/L.

None.

None — samples were alwaysunder control of MRI personnelin the field.

MRI-AppIiedUU«20-28*4 4-5

AR3U756

4.2 Audit Samples

A summary of the performance audit samples (PAS) is presented in Table 4-1 below.With only one minor exception for a Cl" check standard, the PAS results met accuracyobjectives. Results for the EPA dioxin audit results have been submitted to the USEPA.

AMR!-Al>plie<i\R3620-28.s4 ^

Table 4-1. Performance Audit Sample Results

SampleID

18358

18362

18363

18364

18359

18360

18361

16493,16494"

EPA No.5017

9379

Description

Independentcheck standard in0.1 N NaOH

Independentcheck standard in0.1 N sulfuric acid



Independentcheck standard in0.1 N sodiumhydroxide



Spiked metals onfilter (analyzed induplicate)"

EPA spiked XAD

EPA spiked XAD

Parameteror

compound

Hexavalentchromium

Chloride

Chloride

Chloride

Chloride

Chloride

Chloride

AsBaBeCdCrPbNiSeAgCoCuFeMnVZn

PCDD/PCDF

PCDD/PCDF

Theoretical orprepared value

11.3pg/L

113ug/L

Not spiked

123 pg/mL

94.1 pg/mL

79.3 ug/mL

Not spiked

50 pg10 pg10 pg10 ug10 ug25 ug10 ug25 ug5pg10 ug25 ug25 ug10 ug10 ug50 ug

Provided by EPA

Analysis result

11.46pg/L

117.3ug/L

< 1 ug/mL

141 ug/mL

94.0 pg/mL

78.8 pg/mL

< 1 pg/mL

,

62 ug9.7 pg9.4 ug10.2pg10.5ug22.5 ug10.6pg25.0 ug4.5 ug10.3pg24.9 ug23.3 pg10.1 pg10.6pg50.0 pg

See Section 3.5

Accuracy or comment

101%

104%

Acceptable

115%'

100%

99%

Acceptable

61 pg11.0 pg9.5 pg10.4pg10.3 pg22.8 pg11.5 pg23.3 pg4.9 pg

10.1 pg24.8 pg23.5 pg10.1 pg10.4pgSl.Opg

124979410210590106100901039993101106100

121100951041039111593981019994101104102

Accuracy resultspending from EPA

Provided by EPA See Section 3.5 Accuracy resultspending from EPA

Objective

90%-110%

90-110%

Nocontamination

90%-110%

90%-110%

90%-110%

Nocontamination

75%-125%75%-125%75%-125%75%-125%75%-125%75%-125%75%-125%75%-125%75%-125%75%-125%75%-125%75%-125%75%-125%75%-125%75%-125%

As specified byEPA

As specified byEPA

* Data point outside objective; no significant impact to the data is indicated." Duplicate preparation and analysis of the spiked filter.

MRI-App1ied\R3«20-28.«4 4-7

AR3U758

4.3 Data Quality Objectives (DQO)

The overall quality of the data was very good, with over 90% of the data qualityobjectives for accuracy, precision, and method performance met. Tables 4-2 through 4-4summarize results of the DQO determinations for the various parameters. The results givenin Tables 4-2 through 4-4, as well as Table 4-1, were used to determine the number of QAobjectives met, or met with minor exceptions, compared to the total number of objectives.With few minor exceptions, the QA/QC measurements were within the objectives of theTrial Burn Plan (Appendix G). Method blank and recovery QC results are presented inprevious sections of the report (as indicated). Precision QC results are presented in thissection.

4.4 Data Review

As a final QA function, representative sample results for Run 5 were checked in thefinal (draft) report to help ensure that the derived test results are complete in documentationand format, traceable to supporting records, and accurately reported based on analysis dataand field measurements. Derived emission results for Run 5 were found to be accuratelyreported and traceable to supporting records.

MRi-App1ied\R3620-28.*4

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AR3U766

Table 4-5. Matrix Spike Results for TCLP Metals Extract of Bottom AshSpike Recovery (%)

Matrix spikeMatrix spike dup.

Precision (RPD)

Ag'

79

79

0

Asb

95

108

13

Ba"

87

86

1

Cdb

104

92

12

Cr*

73

74

1

Hg<101

102

1

Pb"113

113

0

Seb

112

127

13

3 Analysis by ICP." Analysis by GFAA.c Analysis by CVAA.

RPD = Relative percent difference

QA Objectives: 70-130% Recovery;20% RPD for precision.

MRI-Applied\R3«20-2834 4-J.O

Table 4-6. Matrix Spike Recoveries and Precision for SVOCs in Bottom Ashand Fly Ash

Feed Bottom ash% Recovery % Recovery

(QA Objective 30-1 30%) (QA Objective 30-1 30%)Precision Precision

MS MSD RPD MS MSD RPDPhenolBis(2-chloroethyl) ether2-Chlorophenol1 ,3-Dichlorobenzene1 ,4-DichlorobenzeneBenzyl alcohol1 ,2-Dichlorobenzene2-MethylphenolBis(2-chloroisopropyl) ether4-MethylphenolA/-Nftroso-di-W-propylamineHexachloroethaneNitrobenzeneIsophorone2-Nitrophenol2,4-DimethylphenolBenzoic acidBis(2-chloroethoxy) methane2,4-Dichlorophenol1 ,2,4-TrichlorobenzeneNaphthalene4-ChloroanilineHexachlorobutadiene4-Chloro-3-methylphenol2-MethylnaphthaIeneHexachlorocyclopentadiene2,4,6-Trichlorophenol2,4,5-Trichlorophenol2-Chloronaphthalene2-NrtroanilineDimethyl phthalateAcenaphthylene3-NitroanilineAcenaphthene2,4-Din'rtrophenol4-NrtrophenolDibenzofuran2,4-Dinitrotoluene2,6-DinitrotolueneDiethyl phthalate

79 63 23 85- - - 77_ 75- - - 7781 65 22 78— — — 5*88 71 21 79- 65_ 80- - - 63- - - 71- - - 76- - - 83- - - 89- - - 75- - - 29'35 27* 26 5s

— 7Qi &

- - - 7691 74 21 8193 75 21 89- 48- 79- - - - - 8 3- - - 90- 16"- 65- 93_ 83- - - 77- 90_ 85_ 76- - - 91_ ^_ _ 36- - - 75- - 109- - - 86- - - 84_ 97


92888384855'8770858575 ,82899985401068986899756889310018'731119589102958510149871259792108

81310990107630587111332184'12121091511111112121813141311111031151412911

Fly ash% Recovery

(QA Objective 30-1 30%)Precision

MS MSD RPD82818179805"8275846773778892824917'81778386598284913774898680898682925467108858294

84848483846*8577908574828595804116"848284896584879535798691849591909758771159287102

244552043724163321864613102446736576957146868

MRI-App!i«W*3«0-28.»4 4-17

AR3U768

Table 4-6 Continued(Matrix Spike Recoveries and Precision for SVOCs in Bottom Ash and Fly Ash)

Feed% Recovery

(Q A Objective 30-1 30%)Precision

MS MSD RPD4-Chlorophenyl phenyl etherFluorene4-Nitroaniline4,6-Dinitro-2-methylphenolA/-Nitrosodiphenylamine4-Bromophenyl phenyl etherHexachlorobenzenePentachlorophenolPhenanthreneAnthraceneDi-n-butyl phthalateFluoranthenePyreneButyl benzyl phthalate3,3 '-DichlorobenzidineBenz[a]anthiaceneBis(2-ethylhexyl) phthalateChryseneDi-n-octyl phthalateBenzo[i>]f]uorantheneBenzo[/c]fluorantheneBenzo[a]pyrenelndeno[1 ,2,3--co]pyreneBenzo[gA']perylene

p-Naphthylarnine (by ECC)

-

—86115_-123127-—129-105-959392-—

(30)

-

-7383—-95103--99~86-797676-—

(38)

—

-1632—~2621-—26-20-182020-—

(24)

Bottom ash% Recovery

(QA Objective 30-1 30%)Precision

MS MSD RPD90929979918891749084981099690699210891898484829189

(83)

10210310891100961008499921091241089980102117102101851029410198

(79)

131110149991310911131210151081113120141010

(4)

Fly ash% Recovery

. (QA Objective 30-1 30%)Precision

MS MSD RPD899310283908890708586951061009067859990918184838783

(20)"

94971088894939575909310311310695749311398988597919592

(19)'

5466465768866510913975149910

(5)

Surrogate Recoveries (%)-QA Objective 30-130%2-FluorophenolPhenol-d52-chlorophenol-d41 ,2-Dichlorobenzene-d4Nitrobenzene-d52-Fluorobiphenyl2,4,6-TribromophenolTerphenyl-d14

Surrogate Recovery (%) by ECCNitrobenzene-d52-FluorobiphenylTerphenyl-d14

6070707077788389

7689116

5257585966677380

7088105

1421191715151311

8110

6570687075737472

73103111

6975737582808379

82101107

677799129

1424

6772717077707172

8999125

6876747481777878

8491109

654651038

6814

1 Data are outside the QA objectives.Objectives: 30-130% Recovery; 35% Relative Percent Difference (RPD)

MRI-Applied\R3620-28.s4 4-18

AR3U769

Table 4-7. 2,3,7,8-Substituted Dioxin/Furan Precision Results forBottom Ash Samples

J Indicates an estimated value.U Indicates compound was analyzed, but not detected.B Indicates that measured value is not greater than 5X the blank value.

NC = Not calculated because one or both determinations were below the practical quantitationlimit.

Objective = s25% RPD for precision.

Concentration Observed (ng/kg)


Furans2,3,7,8-TCDF1,2,3,7,8-PeCDF2,3,4,7,8-PeCDF1,2,3,4,7,8-HxCDF1,2,3,6,7,8-HxCDF2,3,4,6,7,8-HxCDF1,2,3,7,8,9-HxCDF1,2,3,4,6,7,8-HpCDF1,2,3,4,7,8,9-HpCDF1,2,3,4,6,7,8,9-OCDF

Run 5

< 0.0710 U< 0.149 U< 0.140 U< 0.125 U< 0.153 U

6.14 J36.8 J

< 0.0872 U< 0.136 U'< 0.133 U< 0.0601 U< 0.0491 U< 0.0630 U< 0.0672 U< 0.0506 U< 0.582 U< 0.0996 U

Run 5duplicate

< 0.0431 U< 0.133 U0.209 J0.887 J1.12 J6.85 J44.8 J

0.302 J< 0.0687 U< 0.0670 U< 0.0470 U< 0.0384 U

0.316 U< 0.0525 U< 0.0615 U< 0.0708 U< 0.0758 U

Precision(RPD)

NCNCNCNCNCNCNC

NCNCNCNCNCNCNCNCNCNC

MRI-AppUeAR3«20-28.s4 4-19

Table 4-8. 2,3,7,8-Substituted Dioxin/Furan Precision Results for Fly Ash Samples

Concentration (ng/kg)

AnalyteDioxins2,3,7,8-TCDD1,2,3,7,8-PeCDD1,2.3,4,7,8-HxCDD1,2,3,6,7,8-HxCDD1,2,3,7,8,9-HxCDD1,2,3,4,6,7,8-HpCDD1,2,3,4,6,7,8,9-OCDD

Furans2,3,7,8-TCDF1,2,3,7,8-PeCDF2,3,4,7,8-PeCDF1,2,3,4,7,8-HxCDF1,2,3,6,7,8-HxCDF2,3,4,6,7,8-HxCDF1,2,3,7,8,9-HxCDF1,2,3,4,6,7,8-HpCDF1,2,3.4,7,8,9-HpCDF1,2,3,4,6,7,8,9-OCDF

Run5

< 0.0671< 0.141<0.110< 0.0980«: 0.1203.736.01

< 0.0763< 0.08840.6481.190.8370.63

< 0.06692.950.456

< 0.161

UUUUUJ,BJ,B

UUJJJJUJJ,BU

RunSduplicate

< 0.0887< 0.1490.2020.478

< 0.1894.245.71

0.925< 0.159< 0.1550.2690.9980.998

< 0.1143.15

< 0.1 372.78

UUJJUJJ,B

JUUJJJUJUJ

Precision(RPD)

NCNCNCNCNCNCNC

NCNCNCNCNCNCNCNCNCNC

J Indicates an estimated value.U Indicates compound was analyzed, but not detected.B Indicates that measured value is not greater than 5X the blank value.

NC = Not calculated because one or both determinations were below the practical quantitation limit.Objective = s25% RPD for precision.

MRl-Applied\R3620-28.j4 4-20

AR3U77I

Table 4-9. Precision Results for VOCs in Ash Samples

AnalyteChloromethaneBromomethaneVinyl ChlorideChloroethaneMethylene ChlorideAcetoneCarbon Disulfide1,1-Dichloroethene1,1-Dichloroethanet-1 ,2-DichloroetheneChloroform1 ,2-Dichloroethane2-Butanone1 ,1 ,1 -TrichloroethaneCarbon TetrachlorideVinyl AcetateBromodichloromethane1 ,1 ,2,2-Tetrachloroethane1 ,2-DichIoropropanetrans-1 ,3-DichloropropeneTrichloroetheneDibromochloromethane1 ,1 ,2-TrichloroethaneBenzenecis-1 ,3-Dichloropropene2-Chloroethyl-vinyl ether*Bromoform2-Hexanone4-Methyl-2-PentanoneTetrachloroetheneTolueneChlorobenzeneEthyl benzeneStyreneTotal Xylenes

Rep12 J18 J--11 J-5.7 J-----16 J,B----------19

.-----11 J---3.9 J

Bottom AshRun5

1 Rep 211 J17 J--9.8 J-5.1 J---- -------------17------9.2 J---3.0 J

PrecisionRPDNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNC11NCNCNCNCNCNCNCNCNCNCNC

Fly AshRunS

Rep 1 Rep 22.0 J,B 2.1 J,B3.6 J,B 4.1 J,B--2.0 J,B 2.2 J,B-0.5 J,B 0.5 J,B----

3.6 J3.4 J,B---------.-,------

0.8 J,B---0.4 J,B 0.4 J,B

PrecisionRPDNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNCNC

Surrogate Recoveries (%) — QA objective 70-120%1 ,2-Dichloroethane-d44-BromofluorobenzeneToluene-d8

11080157"

10379139"

7112

113 112123" 11763" 134"

1572*

* Not detected in standard solutions. Compound is unstable in the presence of halocarbons.6 Surrogate recovery outside QA objective range of 70-120%." Precision for surrogate does not meet objective of 35% RPD.

J Indicates an estimated value, above the MDL but below the PQL.B Indicates that measured value is not greater than 5X the blank value.

- Indicates that analyte was not detected (i.e., <Method Detection Limit).RPD = Precision, as expressed as Relative Percent DifferenceNC = Not calculated because one or both values were below the PQL.QA objective for precision is 35% RPD.

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Table 4-11. Recovery and Precision Results for Combined MM5 Semivolatile TrainFilter/XAD

Surrogate Recoveries (%)

2-FluorophenolPhenol-dS2-Chlorophenol-d41 ,2-Dichlorobenzene-d4N'rtrobenzene-d52-Fluorobiphenyt2,4,6-TribromophenolTerphenyl-d14

Blank Train

73848187868780113

Runs

7983

80

85

86

85

77

124

Run 6

7681

77

74

80

83

84

113

Run 7

7681

78

78

82

83

80

118

Precision(RSD)

32

2

7

4

2

4

4

QA objectives: 50-150% surrogate recovery and 50% RSD for precision.

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Table 4-14. Initial Precision and Recovery (IPR) Results for PCBs on XAD Resin

Natives SpikedMono (BZ-2)Di (BZ-5)Tri (BZ-29)Tetra (BZ 50)Tetra (BZ 77)Penta (BZ 87)Penta (BZ 123)Penta (BZ 11 8)Penta (BZ 11 4)Penta (BZ 105)Penta (BZ 126)Hexa(BZ154)Hexa(BZ 167)Hexa(BZ156)Hexa(BZ157)Hexa(BZ169)Hepta(BZ188)Hepta(BZ180)Hepta(BZ170)Hepta(BZ189)Octa (BZ 2.00)Deca (BZ 209)

Field Surrogates Spiked13C 3-Mono13C15-DJ13C52-Tetra13C 153-Hexa13C202-Octa13C209-Deca

IPR1

88397"706512398921118896847488929093788570738980

668296965983

IPR 2

92435"676512491971089298837789959193788672779078

688493976384

IPR 3

91402b646212187981148798847192919092708575788176

6789931026492

IPR 4

89406"7069119100951089098857697929491738976837870

6286941066690

AverageRecovery

90410"686512294961108998847592939192758673788576

6685941006387

Precision(RSD)a

2444263321144221524576

442555

Laboratory Surrogates Spiked13C77-Tetra130118-Penta13C105-Penta13C126-Penta13C156-Hexa13C169-Hexa13C180-Heota

7182889492101131

7179891039597124

6778829387102117

7285859988102111

7081869791101121

3445427

Precision expressed as Relative Standard Deviation (RSD) per Section 5 of the Trial Burn Plan.." Outside objective of 50-150% recovery.QA Objectives: 50-150% recovery and 35% RPD for precision.

MRI-Applied\R3620-I8.s4 4-26

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Table 4-15. Metals Train Analysis QA ResultsSpiked laboratory reagent blanks - % RecoveryQA objectives: 65-135% Recovery; 40% RPD

Metal

AsBaBeCdCr

PbHgNiSeAgAlSbCaCoCu

FeMgMnKNa

VZn

FrontHalf

10698919297

9310198954'

951011069595

9496978894

9892

FrontHalf Dup

108100919297

95 '10398967*

961081099495

9596978698

9892

Precision(RPD)

22000

220155'

17310

10024

00

BackHalf

97928997

• 94

101NA969014'

10095919492

9396948998

9495

BackHalf Dup

9491899795

100NA979487

10091909492

9396949197

9397

Standard ReferenceMaterial (% Accuracy)11

Precision(RPD)

31001

1NA14

146"

04100

00021

12

SRM #1 PrecisionSRM #1 Dup (RPD)

1249794102105

90NA10610090

NANANA10399

93NA101NANA

106100

12111095104103

91NA1159398

NANANA10199

94NA101NANA

104102

212122

1NA878

NANANA20

1NA0NANA

22

a Recovery outside QA objective of 65-135%, as discussed in text of report.b Accuracy objective: 75-125%

Precision objective: 50% RPDc Outside precision objective.

RPD = Relative Percent DifferenceNA = Not applicable

Matrix Spike Recoveries for Hg (%)

FrontHalf Dup RPD

98 96 2

H2Oj/HNOjImpingers Dup RPD

98 96 2

KMn04/H2S04Impingers Dup RPD

99 99 0

HCIRinse Dup RPD

102 106 4

MRI-AppIic*R3620-28 4 4-27

A.R3U778

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