BARR ENGINEERING CO MEMO RE: CLP DATA VALIDATION … · Waste Management Division Office of...

BarrEngineering Company8300 Norman Center DriveMinneapolis. MN55437-1026Phone: (612)832-2600Fax: (612) 835-0186

August 20, 1993

Mr. Ted SmithRemedial Project ManagerWaste Management DivisionOffice of Superfund (HSRM-J5)U.S. Environmental protection Agency77 West Jackson BoulevardChicago, IL 60604-3590

RE: Laboratory Data and Data Validation Reports for the ReprocessingTreatability Study conducted on Sludge and Filter Cake Source Materialtaken from the Arrowhead Refinery site, Hermantown, MN

Dear Mr. Smith:

Enclosed is a copy of the raw data supplied by Enseco - Rocky MountainAnalytical Laboratory {Enseco - RMAL) and Huffman Laboratories for samplestaken during the Reprocessing treatability study conducted April 14-15, 1993by 7-7, Inc. I have attached a cover sheet explaining the organization ofthe six constituent laboratory reports.

Please also find enclosed copies of the three CLP Data ValidationReports prepared by Barr Engineering Co. for the three Enseco - RMAL reports,Insufficient information was provided by Huffman Laboratories to perform DataValidation of their analyses. However, the analyses performed by Huffman(for chlorine, sulfur, nitrogen, ash, and heat contents) use establishedmethods which Barr Quality Assurance personnel believe are less subject tolaboratory or sample variability than the analyses performed by Enseco - RMALfor target compounds.

If you have any questions regarding this matter or require furtherinformation, please do not hesitate to call me at 612-832-2620.

Sincerely,

John P. BorovskVice President

JPB/rptcc: Tom Kelley, MPCA

MASC Technical CommitteeEnclosures23\69\065\SMITH.LTR

BARR ENGINEERING COMPANY

MEMORANDUM

TO: Arrowhead Refinery Site Project File 23/69-065DFS52FROM: Grant Paul (GAP)

DATE: August 19, 1993«

RE: CLP Data Validation Report

Laboratory Report No. 28302 May 13, 1993 (Enseco)

I. VOIATtLES - by 8240

Samples: SLUDGE (3.17.93)FILTER CAKE (3.17.93)

A. HOLDING TIMESThe EPA holding time criteria were met.

B. BLANKSThe method blank associated with the samples contained no compoundsabove their reporting limits except acetone at 1200 ug/kg, MEK at 590ug/kg, methylene chloride at 160 ug/kg, and toluene at 110 ug/kg.For the sample SLUDGE, acetone was reported by the laboratory at 9400ug/kg with the B qualifier. The validation procedure required thedata value for acetone be changed to 9400 U ug/kg. For the samereasons, 2-butanone and MIBK were given the U qualifier for theSLUDGE sample. For the FILTER CAKE sample, acetone was reported bythe laboratory at 5200 ug/kg with the B qualifier. The validationprocedure required the data value for acetone be changed to 5200 Uug/kg. For the same reasons, 2-butanone and MIBK were given the Uqualifier for the FILTER CAKE sample.

In addition, toluene was reported in the method blank but notdetected in both of the samples. Therefore the B qualifier reportedby the laboratory for toluene for both samples was dropped accordingto CLP data validation procedures.

C. GCMS TUNINGThe established method performance criteria were met prior to theinitial calibration, the continuing calibration, and to the analysisof the samples.

2369065\INCIN\DV1.MEM\GAP

MEMO: File 2369065DFS52 August 19, 1993 Page 2

D. GCM5 INITIAL CALIBRATIONThe initial calibration met the EPA acceptance criteria.

E. GCMS CONTINUING CALIBRATIONThe continuing calibrations met the EPA acceptance criteria.However, acetone had a 47.3% difference, 1,2 dibromoethane had a25.7% difference1, and MIBK had a 27% difference for the March 24,1993 calibration of instrument B. On March 26, 1993 , vinyl acetatehad a 28.7% difference and meta/para xylene had a 27.2% differencefor the continuing calibration of instrument B. On March 26, 1993, cis-1,2 dichloroethene had a 30% difference, MEK had a 30%difference, and meta/para xylene had a 30% difference for thecontinuing calibration of instrument C. Samples SLUDGE and FILTERCAKE were analyzed on instrument C on March 26, 1993. According tothe CLP data validation procedures, the J qualifier was assigned to1,2 dichloroethene, MEK, and meta/para xylene due to the continuingcalibration.

F. SURROGATE RECOVERYOne surrogate, toluene-d8, was recovered at 83% (beyond the lowerlimit of 84%) in the spiked sample. This was not determined to besufficient to warrant the assignment of any data qualifiers. Allother surrogates were within the acceptance criteria.

G. SINGLE CONTROL SAMPLE (SCSi/DUPLICATE CONTROL SAMPLE (DCS)The SCS and DCS percent recoveries and relative percent differences(RPD) met the acceptance criteria for all compounds in the samples,

H. MATRIX SPIKE (MS)/MATRIX SPIKE DUPLICATE (MSP)The percent recoveries and the relative percent differences (RSD)were within the acceptance criteria for all compounds in all samplesexcept for 1,1-dichloroethene in the SLUDGE spiked sample. The %recoveries for 1,1-dichloroethene were 53 and 57% in the MS and MSD,the lower acceptance criteria is 59%. This slightly low recovery wasinsufficient to justify assigning a qualifier to the compound valuein the SLUDGE sample. Both samples reported non-detects for 1,1-dichloroethene.

I. MATRIX DUPLICATENo matrix duplicates were required or run.

J. INTERNAL STANDARDSAll internal standards met the acceptance criteria.


MEMO: File 2369065DFS52 August 19, 1993 page 3

K. OVERALL DATA QUALITY ASSESSMENT-8240 VolatilesAll of the volatile sample data included in this report wereacceptable as reported with only the following; required dataqualifiers: For the sample, FILTER CAKE, acetone, 2-butanone andMIBK were given the U qualifier due to the blank values. For samplesSLUDGE and FILTER CAKE, 1,2 dichloroethene, MEK, and meta/para xylenewere assigned the J qualifier to due to the continuing calibration.The B qualifier reported by the laboratory for toluene for bothsamples was dropped according to CLP data validation procedures.

II. METALS:Samples: SLUDGE (3.17.93)

SOLVENT LEACHED SLUDGE (Generated in lab 4.15.93)LEACHATE from SLUDGE (Generated in lab 4.15.93)FILTER CAKE (3.17.93)SOLVENT LEACHED FILTER CAKE (Generated in lab 4.15.93)LEACHATE from FILTER CAKE (Generated in lab 4.15.93)

A. HOLDING TIMESThe EPA criteria for holding time was met.

B. BLANKSThe blanks associated with the samples contained no target analytesabove the reporting limits.

C. INSTRUMENT CALIBRATIONThe calibrations met the established criteria.

D. SAMPLE SPIKE RECOVERYIn the SLUDGE sample, barium and lead were at high nativeconcentrations (>4 times the spiked concentration) so no spikerecoveries were determined. Cadmium and chromium had average percentrecoveries of 72 and 67% respectively from the spiked samples.Therefore, the sample SLUDGE was given the EPA qualifier J indicatingestimated values due to the low percent recoveries for cadmium andchromium.

In the FILTER CAKE sample, lead was at high native concentrations (>4times the spiked concentration) so no spike recoveries weredetermined. Barium and selenium had average percent recoveries of 52and 74.5% respectively from the spiked samples. Therefore, sampleFILTER CAKE was given the EPA qualifier J indicating estimated valuesdue to the low percent recoveries for barium and selenium.

In the SOLVENT LEACHED SLUDGE sample, barium and lead were at high



native concentrations (>4 times the spiked concentration) so no spikerecoveries were determined. Arsenic and chromium had average percentrecoveries of 69 and 68% respectively from the spiked samples.Therefore, the SOLVENT LEACHED SLUDGE sample was given the EPAqualifier J indicating estimated values due to the low percentrecoveries for arsenic and chromium.

m

In the SOLVENT LEACHED FILTER CAKE sample, lead was at high nativeconcentrations (>4 times the spiked concentration) so no spikerecoveries were determined. Arsenic had an average percent recoveryof 225% from the spiked samples. Therefore, the SOLVENT LEACHEDFILTER CAKE sample was given the EPA qualifier J indicating estimatedvalues due to the high percent recoveries for arsenic.

In the LEACHATE from FILTER CAKE and the LEACHATE from SLUDGE sample,lead was at high native concentrations {>4 times the spikedconcentration) so no spike recoveries were determined.

E. DUPLICATE CONTROL SAMPLEAll percent recoveries and relative percent differences were withinthe acceptance criteria.

F. OVERALL DATA QUALITY ASSESSMENT- MSTALSThe data for the samples as reported by the laboratory wereconsidered acceptable with only the addition of the following EPAdata qualifiers:

The sample, SLUDGE, was given the EPA qualifier J indicatingestimated values due to the low percent recoveries for cadmium andchromium.

The sample, FILTER CAKE, was given the EPA gua.li.fier J indicatingestimated values due to the low percent recoveries for barium andselenium.

The sample, SOLVENT LEACHED SLUDGE, was given the EPA qualifier Jindicating estimated values due to the low percent recoveries forarsenic and chromium.

The sample, SOLVENT LEACHED FILTER CAKE, was given the EPA qualifierJ Indicating estimated values due to the high percent recoveries forarsenic.

2369065\INCIN\DV1.MEMXGAP


III. CYANIDE and SULFIDESamples: SLUDGE (3.17.93)

FILTER CAKE (3.17.93)

A. HOLDING TIMESThe EPA criteria*for holding time was met.

B. BLANKSThe blanks associated with the samples did not contain cyanide orsulfur above the instrument detection limits (IDL).

C. INSTRUMENT INITIAL CALIBRATIONInitial calibration met the'established criteria.

D. INSTRUMENT CONTINUING CALIBRATIONThe continuing calibration met the established criteria.

E. SAMPLE SPIKE RECOVERYIn the SLUDGE sample, cyanide and sulfide had average percentrecoveries of 62 and 72% respectively from the spiked samples.Therefore the sample, SLUDGE, was given the EPA qualifier Jindicating estimated values due to the low percent recoveries forcyanide and sulfide.

In the FILTER CAKE sample, sulfide had an average percent recoveryof 73% from the spiked samples. Therefore the sample, FILTER CAKE,was given the EPA qualifier J indicating estimated values due to thelow percent recoveries for sulfide.

F. DUPLICATESNo duplicate data was provided.

G. LABORATORY CONTROL SAMPLEThe results of the laboratory control sample analysis (83. to 113.%)met the acceptance criteria of 80-120% recovery.

H. OVERALL DATA QUALITY ASSESSMENT- CYANIDE and SULFIDEThe sample, SLUDGE, was given the EPA qualifier J indicatingestimated values due to the low percent recoveries for cyanide andsulfide.

The sample, FILTER CAKE, was given the EPA qualifier J indicatingestimated values due to the low percent recoveries for sulfide.



MEMORANDUM

TO: Arrowhead Refinery Site Project File 23/69-065DFS52

FROM: Grant Paul (GAP)

DATE: August 18, 1993


Laboratory Report No. 28873 May 25, 1993 (Enseco)

I. TOTAL CHROMATOGRAPHABLE ORGANICS (TCP) or EXTRACTABLE PETROLEUMHYDROCARBONS

Samples: R1RCH (4.15.93)R1PFH (4.15.93)R1PSH (4.16.93)R2PFH (4.16.93)

A. HOLDING TIMESThe method extraction and analysis holding time criteria were met.

B. BLANKSThe method blanks associated with the samples was reported as NotDetected for TCO at the reporting limit of 10 mg/k.g.

C. GC INITIAL CALIBRATIONThe initial calibrations reported met the method acceptance criteria.

D. GC CONTINUING CALIBRATIONThe continuing calibrations met the method acceptance criteria.

E. SURROGATE RECOVERYDue to the required extract dilutions, the surrogate standard (ortho-terphenyl) recoveries were not determined.

F. SINGLE CONTROL SAMPLE (SCSI/DUPLICATE CONTROL SAMPLE (DCS)The SCS and DCS percent recoveries and relative percent differences(RPD) met the acceptance criteria. The DCS recovery was 69% with a7.5% relative percent difference(RPD) and the SCS recovery was 95%.

G. MATRIX SPIKE (MS)/MATRIX SPIKE DUPLICATE (MSD)No MS and MSDs were requested to be analyzed from this project'ssamples.

H. MATRIX DUPLICATENo sample duplicate data was performed for this report.



I. OVERALL DATA QUALITY ASSESSMENT-TCPThe TCO sample data included in this report required no additionalqualifiers.

II. POLYCHLORINATED BIPHENYLS (PCBS14

Samples: RlRCH (4.15.93)R1PFH (4.15.93)R1PSH (4.16.93)R2PFH (4.16.93)

A. HOLDING TIMESThe method extraction and analysis holding time criteria were met.

B. BLANKSThe method blanks associated with the samples was reported as NotDetected for PCBs at the reporting limit of 33 ug/Jcg.



E. SURROGATE RECOVERYDue to the required extract dilutions, the surrogate standard(decachlorobiphenyl) recoveries may have been influenced. Therecoveries were generally low with the range from 16.8% to 41.6%.Since EPA has only advisory limits for surrogate recovery, no actionis required.

F. SINGLE CONTROL SAMPLE fSCS)/DUPLICATE CONTROL SAMPLE (DCS)The SCS and DCS percent recoveries and relative percent differences(RPD) met the acceptance criteria. The DCS recovery was 71% with a5.1% relative percent difference(RPD) and the SCS recovery was 63%.

G. MATRIX SPIKE (MS)/MATRIX SPIKE DUPLICATE (MSP)No MS and MSDs were requested to be analyzed from this project'ssamples.

H. MATRIX DUPLICATENo sample duplicate data was performed for this report.

I. OVERALL DATA QUALITY ASSESSMENT-PCBsThe PCS sample data included in this report required no additionalqualifiers.



III. METALS: + TCLP LEAD

Samples: R1RCH (4.15.93)R1PFH (4.15.93)R1PSH (4.16.93)R2PFH (4.16.93)R1RCH (4.15.93) -Methylene chloride leachedR1PSH (4.15". 93) -Methylene chloride leachedR1RCH (4.15.93) -Methylene chloride leachateR1PSH (4.15.93) -Methylene chloride leachate


B. BLANKSThe blanks associated with the samples contained no target analytesabove the reporting limits.

C. INSTRUMENT INITIAL CALIBRATIONThe initial calibration met the established criteria.


F. SAMPLE SPIKE RECOVERYNo MS and MSDs were requested to be analyzed from this project'ssamples.

G. DUPLICATESNo duplicate sample analyses were performed for this project.

H. DUPLICATE CONTROL SAMPLE (DCS)For the solid sample analytes analyzed by ICP (arsenic, barium,cadmium, chromium, lead, and silver), the DCS percent recoveries {84-116) and relative percent differences {RPD) of 0 to 6.1% met theacceptance criteria. For the leachate sample analytes analyzed byICP (lead), the DCS percent recoveries (87-103) and relative percentdifferences {RPD) of 1.4 to 6.2% met the acceptance criteria.

For the solid sample analytes analyzed by furnace {arsenic, andselenium), the DCS percent recoveries (86-111) and relative percentdifferences (RPD) of 0 to 14% met the acceptance criteria.

For the solid sample analytes analyzed by cold vapor atomicabsorption {mercury), the DCS percent recoveries (113-119) andrelative percent differences {RPD) of 1 to 3.8% met the acceptancecriteria.



I. OVERALL DATA QUALITY ASSESSMENT- METALSThe metals sample data included in this report required no additionalqualifiers.

IV. GENERAL INORGANICS (Total Solids, Bulk Density, pH, Ignitabilitv)«*

Samples: R1RCH (4.15.93)R1PFH (4.15.93)R1PSH (4.16.93)R2PFH (4.16.93)


B. INSTRUMENT CALIBRATIONCalibration information was not provided or requested.

C. DUPLICATESFor the measure of precision, the laboratory duplicate pHanalysis data was reviewed. The duplicate data met the EPAacceptance criteria.

D. OVERALL DATA QUALITY ASSESSMENT- GENERAL INORGANICSThe general inorganic data for the samples as reported by thelaboratory was considered acceptable without the addition of any Barrdata qualifiers.



MEMORANDUM

TO: Arrowhead Refinery Site Project File 23/69-065DFS52

FROM: Grant Paul (GAP)

DATE: August 19, 1993«


Laboratory Report No. 29365 June 16, 1993 (Enseco)Note: The samples were originally designated as R1PSE (4.15.93) and R2PSE(4.21.93) on the chain of custody. This sample identification was subsequentlychanged to correctly identify the samples. Sample R2PSE was re-named R2PC(4.21.93). The other sample, R1PSE, was not analyzed but provided as a back-upsample for another report. The samples were in transit from May 12 to May 18and as a result, the PCB, pH, and TCO extraction holding time of 14 days wasexceeded.

I. TOTAL CHROMATOGRAPHABLE ORGANICS (TCP) or EXTRACTABLE PETROLEUMHYDROCARBONS

Samples: R2PC (4.21.93)

A. HOLDING TIMESThe method extraction holding time criteria was exceeded (theanalysis was requested after the holding time was exceeded).

B. BLANKSThe method blanks associated with the samples was reported as NotDetected for TCO at the reporting limit of 10 mg/kg.



E. SURROGATE RECOVERYDue to the required extract dilutions, the surrogate standard (ortho-terphenyl) recovery was not determined for the sample.

F. SINGLE CONTROL SAMPLE (SCSI/DUPLICATE CONTROL SAMPLE (DCS)The SCS and DCS percent recoveries and relative percent differences(RPD) met the acceptance criteria. The DCS average recovery was 74%with a 5.7% relative percent difference (RPD) and the SCS recovery was90%.




H. SAMPLE DUPLICATENo sample duplicate data was provided.

I. OVERALL DATA QUAlITY ASSESSMENT-TCPThe TCO sample data included in this report required no additionalqualifiers except for the J data qualifier due to the holding timeexceedance.

II. POLYCHLORINATED BIPHENYLS tPCBS)


A. HOLDING TIMESThe method extraction holding time criteria was exceeded (theanalysis was requested after the holding time was exceeded).

B. BLANKSThe method blank associated with the samples was reported as NotDetected for PCBs at the reporting limit of 33 ug/kg.



E. SURROGATE RECOVERYDue to the required extract dilutions, the surrogate standard(decachlorobiphenyl) recovery from the sample was not determined.

F. DUPLICATE CONTROL SAMPLE (DCS)The DCS percent recoveries and relative percent differences (RPD) metthe acceptance criteria. The DCS average recovery was 93% with a1.3% relative percent difference{RPD).


H. MATRIX DUPLICATENo sample duplicate data was provided.


MEMO: File 2369065DFS52 August 19, 1993 page 3

I. OVERALL DATA QUALITY ASSESSMENT-PCBsThe PCB sample data included in this report required no additionalqualifiers except for the J data qualifier due to the holding timeexceedance.

III. METALS: (Total Metals-and TCLP-lead only)

Samples: R2PC (4.21.93)R2PC EXTRACTED SOLID (Generated in lab June 7-11, 1993)R2PC EXTRACT/LEACHATE (Generated in lab June 7, 1993)

A. HOLDING TIMESThe mercury holding time criteria was exceeded (the analysis wasrequested after the holding time was exceeded).

B. BLANKSThe blanks associated with the samples contained one target analytesat or above the reporting limits. Chromium was reported at 1 mg/kgin the method blank (the reporting limit was 1 mg/kg) . Theconcentrations in the samples were greater than five times the levelof chromium in the method blank, so no data qualifier was assigned tothe chromium data and the B qualifier assigned by the laboratory wasdropped.

C. INSTRUMENT INITIAL CALIBRATIONThe initial calibration met the established criteria.


F. SAMPLE SPIKE RECOVERYNo MS and MSDs were requested to be analyzed from this project'ssamples.

G. DUPLICATESNo sample duplicate data was provided.

H. DUPLICATE CONTROL SAMPLE (DCS)For the solid sample (R2PC and R2PC EXTRACTED SOLID) analytesanalyzed by ICP (barium, cadmium, chromium, lead, and silver), theDCS percent recoveries (104-110) and relative percent differences(RPD) of 0.6 to 3.4% met the acceptance criteria.

For the solid sample (R2PC and R2PC EXTRACTED SOLID) analytesanalyzed by furnace (arsenic, and selenium), the DCS percentrecoveries (81-85) and relative percent differences (RPD) of 4.3 to5.0% met the acceptance criteria.



For the solid sample analytes ((R2PC and R2PC EXTRACTED SOLID)analyzed by cold vapor atomic absorption (mercury), the DCS percentrecoveries (100-118) and relative percent differences (RPD) of 0 to2.9% met the acceptance criteria.

For the leachate sample (R2PC EXTRACT/LEACHATE) analytes analyzed byICP (lead), the" DCS percent recovery (99) and relative percentdifference (RPD) of 3.0% met the acceptance criteria.

I. OVERALL DATA QUALITY ASSESSMENT- METALSThe metals sample data included in this report required no additionalqualifiers except for mercury which required the data qualifier J dueto holding time exceedance in samples R2PC and R2PC EXTRACTED SOLID.The B qualifier assigned by the laboratory was dropped from samplesR2PC and R2PC EXTRACTED SOLID for chromium based on the CLP datavalidation procedures.

IV. GENERAL INORGANICS (Total Solids, Bulk Density, pH, Iqnitabilitv)


A. HOLDING TIMESThe pH holding time criteria was exceeded (the analysis was revestedafter the holding time was exceeded).

B. INSTRUMENT CALIBRATIONCalibration information was not provided or requested.

C. DUPLICATESNo sample duplicate data was provided.

D. DUPLICATE CONTROL SAMPLE (DCS)For the solid sample (R2PC) pH analysis, the DCS average percentrecovery (99) and relative percent difference (RPD) of 0.7% met theacceptance criteria.

E. OVERALL DATA QUALITY ASSESSMENT- GENERAL INORGANICSThe general inorganic sample data included in this report required noadditional qualifiers except for pH which required the data qualifierJ due to holding time exceedance in sample R2PC.


7-7. Inc. Lead Removal Process Trcatability Study Laboratory Results

Six laboratory reports (three for analyses conducted by Enseco - RockyMountain Analytical Laboratory and three for analyses conducted by HuffmanLaboratories) present the laboratory results for the lead removal treatabilitystudy performed by 7-7, Inc. on April, 14-15, 1993. These six reports are asfollows:

Report Lab. ID liftbj.

028302028302

151893151893

028873028873028873028873

161693161693161693161693

029365

184293

-001-002

-04-05

-001-002-003-004

-01-02-03-04

-001

-01

<E)(E)

(H)(H)

(E)(E)(E)(E)

(H)(H)(H)(H)

(E)

(H)

Client ID

SludgeFilter Cake

Sludge 28302-1Filter Cake

R1RCHR1PFHR1PSHR2PFH

R1RCHR1PSHR1PPHR2PFH

R2PC

R2PSH

l* A~l

SludgeCake

SludgeCake

R1RC; 1.3:1 CompositeR1PF; Run #1 - FuelR1PC; Run #1 - CakeR2PF; Run #2 - Fuel

R1RC; 1.3:1 CompositeR1PF; Run #1 - CakeR1PC; Run #1 - FuelR2PF; Run #2 - Fuel

R2PC: Run #2 - Cake

R2PC; Run #2 - Cake

(E) = Enseco-Rocky Mountain Analytical Laboratory, Arvada, CO(H) = Huffman Laboratories, Golden, CO

File: RPT:C:\2369065\7-7\T-STUDY\LABRESUL.COV 8/20/93

Rocky MountainAnalytical Laboratory

ANALYTICAL RESULTS

FOR


ENSECO-RMAL NO. 028302

MAY 13, 1993

wEnsecoA CORNING Company

Reviewed by:

Enseco Incorporated4955 Yarrow StreetArvada, Colorado 80002303/421^611 Fax: 303/431-7171

; ——————— EnsecoA Ciirnm^ Compjnv

I. OVERVIEW

On March 25, 1993, Enseco-Rocky Mountain Analytical Laboratory receivedtwo samples from Barr Engineering Company.

This report presents the analytical results as well as supportinginformation to aid in the evaluation and interpretation of the data and isarranged in the following order:

I. OverviewII. Sample Description Information/Analytical Test RequestsIII. Analytical ResultsIV. Quality Control Report

A. Standard Enseco QCB. Project-Specific QC

All analyses at Enseco are performed so that the maximum concentration ofsample consistent with the method is analyzed. Dilutions are at timesrequired to avoid saturation of the detector, to achieve linearity for aspecific target compound, or to reduce matrix interferences. In this event,reporting limits are adjusted proportionately. Surrogate compounds may not bemeasurable in samples which have been diluted.

The initial work plan for Barr Engineering Company Project 23169-065DFS52(RMAL Project number 028302) was discussed with Grant Paul (Barr) and GaryWalters (RMAL) on March 25, 1993. Subsequent charges to the scope of theproject were coordinated by Cindy Patterson (RMAL) as noted below.

RMAL samples 028302-0003 through -0006 did not physically exist on receiptat the laboratory. Portions of the sludge sample (-0001) and the filter cakesample (-0002) were extracted with methylene chloride to generate leachedsolids (-0003 and -0004) and solvent leachates (-0005 and -0006).

Each original sample (-0001 and -0002) was analyzed for total RCRA metals,sulfide, percent moisture, and BTU. As directed by Grant Paul on March 30,1993, matrix spikes/matrix spike duplicates were added to all applicable

EnsecoA Ci>mmc

samples, and tentatively identified compounds were added to the volatileanalysis. As directed by Grant Paul on April 1, 1993, tests for cyanide wereadded to the original samples. All data for -0001 and -0002 is reported on adry weight basis. The BTU analyses for samples 028302-0001 and -0002 as wellas their respective matrix QC samples, were performed by Huffman Laboratorieslocated in Golden, Colorado. Huffman will be sending the report directly toBarr Engineering as directed by Grant Paul of Barr Engineering. Therefore,data for the BTU analyses are not included in this report.

Each original sample was also analyzed for medium level volatiles(methanol extracted) using a combination of Method 8240 and CLP protocols (thechain of custody lists Method 465D for volatiles). Grant Paul requested CLPprotocols; however, 1,2-dibromoethane (EDB) is not a CLP target analyte. Tomeet these criteria, the data was processed using CLP techniques for targetanalytes and Method 8240 techniques for EDB. CLP forms were not provided;although complete data deliverables are included. Standard Enseco Method 8240QC (DCS, SCS) was provided as well as requested matrix spikes and matrix spikeduplicates (MS/MSD).

Toluene-d8 surrogate recoveries in the Method 8240 analysis of 028302-0001SA, -0001MS, and -0001SD were slightly low (83-85%). In addition some ofthe spike recoveries in the MS/MSD analyses were low and somewhat variable.Since the associated laboratory QC was in control, a matrix effect in thesamples is indicated.

Cyanide recoveries in 028302-0001MS and -0001SD were also below expectedrecoveries due to matrix interference. Associated laboratory QC was incontrol.

Spike recoveries for metals were inconsistent due to matrix interferencesand elevated levels of target compounds. Spike levels used for lead wereinappropriate relative to the levels in the samples, (For future projectswhere elevated levels are known in advance, RMAL will spike with higher levelsof the analyte.) All laboratory QC for metals was in control except forsilver and sodium in DCS Lot 04 May 93-1B; this lot was used for lead analysisonly of 028302-0003 through -0006.

—————————————;————:——————————————— Enseco" L ,- -___ __ f- ____ __-~\ v_L'min£ k,i>rnpd

Summary of Metals Preparation and Results

The following procedure was followed to prepare extracted samples metalsanalysis for project 028302. The samples were homogenized and a 20 gramaliquot was placed in a glass centrifuge tube. The sample was then mixed with20 grams of methylene chlori'de and" extracted (shaken vigorously on MOOTshaker) for 30 minutes, then centrifuged for 30 minutes. The methylenechloride extract was decanted into a separate bottle while the remaining solidportion was dried at 103°C for 30 minutes. This drying step was used toremove residual solvent, and should have also removed most of the waterremaining in the sample. Sample weights are recorded in the datadeliverables. The methylene chloride extract, remaining solid portion and thetotal sample were prepared and analyzed using RMAL SOPs based on SW846 Methods3050, 6010, and the 7000 series for Hg, As, and Se.

For the total samples (-0001 and -0002) results are reported on a dryweight basis. Since the leached solids were dried for 30 minutes, theleached/extracted solids (-0003 and -0004) were reported as weighed out--indry weight units but with no correction for percent moisture. Results for thesolvent extracts were also reported as weighed out--in wet weight units withno moisture correction. The sample portion weighed included the solventdecanted plus any material which dissolved in the solvent.

The solvent extraction was first done on April 29th and results for theRCRA metals (excluding lead) on the leached solids (-0003 and -0004) werereported from this extraction. During this April 29th extraction,insufficient weights were recorded at each step to determine the amount ofsolvent and sample recovered. Since this did not effect the analysis of RCRAmetals on the leached solids, all results except lead were reported from thisextraction. Mercury analysis holding times were exceeded (Grant Paul wasnotified on April 13, 1993).

The extraction step was repeated on May 1st to produce extracted solidsand solvent extract for the analysis of lead only. The dry solids resultsobtained from the May 1st extraction did not, in all cases, agree with the

EnsecoApril 29th extraction. This indicates the extraction/decanting technique isnot very reproduceable and/or the sample matrices are not homogeneous (evenafter mixing).

A Cumini;

For summary purposes, the lead results were converted to total lead in thesample aliquot (see table below). A nominal 20 g aliquot was used for thesolvent extractions, so total results for the original sample (-0001 and-0002) are based on the dry weight portion of a 20 g aliquot. The recordedweights for the dried leached solids and leachate were used to calculate thetotal lead in the separate portions. Since the spike lead additions were solow (<l-2.5% of the amount of lead 1n the sample), the MS/MSD values were usedto calculate an approximate "average" value for the sample, MS, and MSD. Thisvalue is shown in parentheses in the table and may be a better approximationfor the total lead result. The range of lead values for the sample, MS, andMSD indicate significant variability.

Sludge

028302 mq/kg

-0001-SA 27500Total Sample

-0003-SA 8130Leached Solid

-0005-SA 4490Leachate

Lead Results for 028302

Percent AverageAverage Aliquot Lead of LeadfSA.MS.SD) Weight, o _mg_ Total mq

(24000) 12.26

(11700) 4.69

(4600) 29.06

337 (294)

38.1 11 (54.9) (19)

130 39 (134)50% (64%)

Filter Cake

028302 mq/kq

-0002-SA 6510Total Sample

-0004-SA 7780Leached Solid

-0006-SA 1970Leachate

Percent AverageAverage Aliquot Lead of LeadfSA.MS.SD) Weight, q mq Total mq

(5500)

(8400)

(2800)

15.0

7.72

24.0

97.6 (82.5)

60.1 62 (64.8) (79)

47.3 48 (67.2) (811110 (160)

EnsecoA Ci

The data indicates better recovery (close to mass balance) for the filtercake sample. This may confirm previous findings that bioremediated sampleshad higher levels of lead. However, due to the variation observed in theextraction steps and analysis {particularly of the solvent leachates), thedifferences observed may not be significant. For example, viewing the filtercake leachates (-0006SA, -0006MS, and -0006SD) as replicate samples, therelative standard deviation was 70%.

If similar analyses are requested for future samples, alternate proceduresshould be considered for oil, solid, and water separation. For example, theChevron modified oven drying technique (MOOT) can be used to obtain separatealiquotes of dry sample, volatile and non-volatile oil, and water. The sampleis heated to a high temperature, but the phase separations are more accurate.Although not normally done, the collected phases can be analyzed for variousparameters. Another phase separation option would be to use a TCLP pressurefiltration to remove filterable (Teachable) oil from the solid sample. Foroily samples, either percent oil, water, and solids or the MOOT procedure arerecommended to obtain more accurate percent moistures (as compared to thestandard oven drying technique).

; "————————————————• EnsecoII. SAMPLE DESCRIPTION INFORMATION/ANALYTICAL TEST REQUESTS

Sample Description Information

The Sample Description Information lists all of the samples received inthis project together with the internal laboratory identification numberassigned for each sample. Each project received at Enseco-RMAL is assigned aunique six digit number. Samples within the project are numberedsequentially. The laboratory identification number is a combination of thesix digit project code and the sample sequence number.

Also given in the Sample Description Information is the Sample Type(matrix), Date of Sampling (if known) and Date of Receipt at the laboratory.

Analytical Test Requests

The Analytical Test Requests lists the analyses that were performed oneach sample. The Custom Test column indicates where tests have been modifiedto conform to the specific requirements of this project.


5|EnsecoA Coming Company

May 13, 1993

Mr. Grant PaulBarr Engineering Company8300 Norman Center Drive, 1300Minneapolis, MN 55437

Dear Mr. Paul:

Enclosed is the report for two samples received at Enseco-Rocky MountainAnalytical Laboratory (RMAL) on March 25, 1993.

Included with the report is a quality control summary.

Please call if you have any questions.

Sincerely, Reviewed by:

L)^^'Cindy Patterson Gary WaltersProgram Administrator Program Manager

CP/GW/lwEnclosures

RMAL #028302

Enseco Incorporated4955 Yarrow StreetArvada, Colorado 80002303/421-6611 Fax: 303/431-7171

SAMPLE DESCRIPTION INFORMATIONfor

Barr Engineering Company

Enseco

Lab ID Client ID

028302-0001-SA028302-0001-MS028302-0001-SD028302-0001-DU028302-0002-SA028302-0002-MS028302-0002-SD028302-0002-DU028302-0003-SA028302-0003-MS028302-0003-SD028302-0004-SA028302-0004-MS028302-0004-SD028302-0005-SA028302-0005-MS028302-0005-SD028302-0006-SA028302-0006-MS028302-0006-SD

SludgeSludgeSludgeSludgeFilter CakeFilter CakeFilter CakeFilter CakeLeached solid from the sludgeLeached solid from the sludgeLeached solid from the sludgeLeached solid from filter cakeLeached solid from filter cakeLeached solid from filter cakeLeachate/extract from sludgeLeachate/extract from sludgeLeachate/extract from sludgeLeachate/extract from filter cLeachate/extract from filter cLeachate/extract from filter c

SOLIDSOLIDSOLIDSOLIDSOLIDSOLIDSOLIDSOLIDSOLIDSOLIDSOLIDSOLIDSOLIDSOLIDLEACHATELEACHATELEACHATELEACHATELEACHATELEACHATE

17 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 9317 MAR 93

Sampled ReceivedMatrix Date Time Date

25 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9326 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 9325 MAR 93

Ensecc

ANALYTICAL TEST REQUESTSfor


Lab ID:028302

0001 - 0002

0003 - 0004

0005 - 0006

GroupCode Analysis Description

A Heat of CombustionSulfide, TotalRCRA Total Metals done by ICPPrep - Total Metals, ICPMercury, Cold Vapor AAPrep - Mercury, Cold Vapor AAArsenic, Furnace AAPrep - Total Metals, Furnace AASelenium, Furnace AAPercent WaterVolatile Organics

Target Compound List (TCL)VGA Screen for Medium Level SoilsVolatiles Library Search (10 Compound TID)Cyanide, Total

B RCRA Total Metals done by ICPPrep - Total Metals, ICPMercury, Cold Vapor AAPrep - Mercury, Cold Vapor AAArsenic, Furnace AAPrep - Total Metals, Furnace AASelenium, Furnace AA

C ICP SuitePrep - Total Metals, ICP

CustomTest?

NNNNNNNNNNYYNNN

NNNNNNN

YN

—————————————;————————————;———————— EnsecoIII. ANALYTICAL RESULTS

The analytical results for this project are presented in the followingdata tables. The results are presented by sample, by test, with testsreported in the following order: GC/MS, Chromatography, Metals andInorganics.

Each data table includes sample identification information, and whenavailable and appropriate, dates sampled, received, authorized, prepared andanalyzed. The authorization data is the date when the project was defined bythe client such that laboratory work could begin. The date prepared istypically the date an extraction or digestion was initiated. For volatileorganic compounds in water, the date prepared is the date the screening of thesample was performed.

Data sheets contain a listing of the parameters measured in each test, theanalytical results and the Enseco reporting limit. Reporting limits areadjusted to reflect dilution of the sample, when appropriate. Solid and wastesamples are reported on an "as received" basis, i.e. no correction is made formoisture content.

In addition, surrogate recovery data is presented for all GC/MS analyses.The surrogate recovery is an indication of the effect of the sample matrix onthe performance of the method. The results from the Standard Enseco QA/QCProgram, which generates data which are independent of matrix effects, aregiven in Section IV.

The analytical data reported are subject to the following limitations ofthe analytical methodology:

Tentatively Identified Compounds

This report presents results for the "identification" of unknown compoundsthat were detected in the GC/MS analysis. The results from this work arepresented as "tentatively identified compounds" (TIC). The approach used forreporting TICs was based on the protocol established for this purpose in theEPA Superfund methods and on guidelines established by the American ChemicalSociety (ACS).

EnsecoA Comii\£ Compj

In summary, the mass spectrum of chromatographic peaks in concentrationsin excess of 10% of the internal standard were obtained. Normally, the numberof unknown compounds identified is limited to 10 compounds in the volatilefraction and 20 compounds in the semivolatile fraction. Each mass spectrumwas then compared to a library of over 30,000 reference spectra in acomputerized "library search*." The three "best" matches obtained by thecomputer were hardcopied along with the mass spectrum of the unknown peak.This information was then reviewed by an analyst who "identified" the compoundbased on the available information.

All identifications were based on the "Guidelines for 6C/MSIdentification" developed by the American Chemical Society (EnvironmentalScience and Technology. 1982, 16 143A). As recommended in these guidelines,identifications of unknown substances were reported with a level ofconfidence. The three levels of confidence cited in the ACS guidelines andused in this report are as follows:

Level 3: Confirmed Identification

The identification is based on the analysis of an authentic standard.

Level 2: Confident Identification

Good agreement was observed between the unknown compound and a specificlibrary spectrum.

Level 1: Tentative Identification

The unknown compound is only indicative of a specific library spectrum.

Class Identification

The unknown compound was not similar to a specific library spectrum, butit did contain ions characteristic of a class of compounds (saturatedhydrocarbon, chlorinated hydrocarbon, etc.).

EnsecoA Ci

If there were no library spectra similar to the unknown, and it could notbe assigned to a particular class of compounds, the compound is reported as"unknown."

Quantitation of TICs is based on the total ionization peak area relativeto an internal standard, assuming a response factor of one. Accordingly, thereported concentration is an estimate.

In general, mass spectrometry cannot distinguish isomers (compounds withthe same molecular formula). Therefore, an identified compound may be any oneof several different isomers.

Siloxanes

If the tentatively identified compounds in this report include somecompounds reported as "siloxanes", the following information should be used toevaluate the data. Siloxanes are common laboratory and field artifacts orcontaminants. Potential sources include silicon-based grease in the field orlaboratory plus the liquid phase coating on gas chromatography columns, aswell as other equipment in the laboratory. However, siloxanes may be presentin environmental samples from spills of silicone oils or lubricating oils withsiloxane additives.

'Volatile OrganicsTarget Compound List (TCL)

Method 8240

EnsecoA Coming Compjni

Client NameClient ID:Lab ID:Matrix:Authorized:

Parameter

Barr Engineering CompanySIudge028302-0001-SASOLID Sampled26 MAR 93 Prepared

17 MAR 9326 MAR 93

Received: 25 MAR 93Analyzed: 26 MAR 93

Dry Weight ReportingResult Units Limit

AcetoneBenzeneBromodi chloromethaneBromoformBromomethane2-Butanone (MEK)Carbon disulfideCarbon tetrachlorideChlorobenzeneChloroethaneChloroformChloromethaneDi bromochloromethane1.1-Dichloroethane1.2-Dichloroethane1.1-Dichloroethene1.2-Dichloroethene

(total)1,2-Dichloropropanecis-l,3-Dichloropropenetrans-l,3-DichloropropeneEthyl benzene2-Hexanone1,2-Dibromoethane (EDB)Methylene chloride4-Methyl -2-pentanone

(MIBK)Styrene1,1,2,2-TetrachloroethaneTetrachloroetheneToluene1.1.1-Tri chloroethane1.1.2-TrichloroethaneTrichloroetheneVinyl acetateVinyl chlorideXylenes (total)SurrogateToluene-d8

9400490NDNDND

1700NDNDNDNDNDNDNDNDNDND

NDNDNDND

3700ND230250

NDNDND2706800480ND310NDND

22000

Recovery

85

ug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kg3 a 3ug/kg

%

16008208208201600160082082082016008201600820820820820

82082082082082016001600820

160082082082082082082082016001600820

ND - Not detectedNA - Not applicable

(continued on following page)

JBJ

Reported By: Leslie Joy Approved By: MaryHelen Hand


Surrogate

Volatile OrganicsTarget Compound List (TCL)

Method 8240

Barr Engineering CompanySIudge028302-0001-SASOLID Sampled: 17 MAR 9326 MAR 93 Prepared: 26 MAR 93

Enseco


4-Bromofluorobenzenel,2-Dichloroethane-d4

Recovery

8786

Note B : Compound is also detected in the blank.Percent Moisture is 38.7%. All results and limits are reported on a dry weight basis.

Note J : Result is detected below the reporting limit or is anestimated concentration.

ND - Not detectedNA - Not applicableReported By: Leslie Joy Approved By: MaryHelen Hand

Enseco•^ C online Li>mp.irn

TENTATIVELY IDENTIFIED COMPOUNDS

FOR


SAMPLE NUMBER 028302-0001-SA

Compound Name

Acetic Acid, Methyl Ester1-Hexene, 3,4,5-Trimethyl-Benzene, 1-Ethyl-2-Methyl-Benzene, 1,2,4-Trimethyl -Benzene, 1-Ethyl-2-Methyl-Benzene, 1,2,3-Trimethyl-Benzene, 1,2,3,4-Tetramethyl-Benzene, 2-Ethyl-1,3-Dimethyl-Benzene, 1-Methyl-3 -(1-Methyl ethyl)Benzene, 1,2,3,4-Tetramethyl-

ConfidenceFraction Level

VGAVOAVOAVOAVOAVOAVOAVOAVOAVOA

EstimatedConcentration

ug/kq

24000100001600013000110002400015000130001000015000

NOTES:

Confidence Levels

Level 3 - Confirmed IdentificationLevel 2 - Confident IdentificationLevel 1 - Tentative Identification

Please refer to the discussion for further details.


Parameter

Volatile OrganicsTarget Compound List (TCL)

Method 8240Barr Engineering CompanyFilter Cake028302-0002-SASOLID Sampled: 17 MAR 9326 MAR 93 Prepared: 26 MAR 93

EnsecoA Cii


AcetoneBenzeneBromodichloromethaneBromoformBromomethane2-Butanone (MEK)Carbon disulfideCarbon tetrachlorideChlorobenzeneChloroethaneChloroformChloromethaneDi bromochloromethane1.1-Dichloroethane1.2-Dichloroethane1.1-Dichloroethene1.2-Dichloroethene

(total)1,2-Dichloropropanecis-l,3-Dichloropropenetrans-l,3-DichloropropeneEthyl benzene2-Hexanone1,2-Dibromoethane (EDB)Methylene chloride4-Methyl-2-pentanone

(MIBK)Styrene1,1,2,2-TetrachloroethaneTetrachloroetheneToluene1.1.1-Tri chloroethane1.1.2-TrichloroethaneTrichloroetheneVinyl acetateVinyl chlorideXylenes (total)Surrogate

Toluene-d8

Result5200240NDNDND

3200NDNDNDNDNDNDNDNDNDND

NDNDNDND

1100NDNDND

NDNDNDND

3500NDNDNDNDND

7800

Recovery96

Dry Weight ReportingUnits Limit

ug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kgug/kg

ND - Not detectedNA » Not applicable

Reported By: Leslie Joy

(continued on following page)

13006706706701300130067067067013006701300670670670670

67067067067067013001300670

130067067067067067067067013001300670

Approved By: MaryHelen Hand

Cllent NameClient ID:Lab ID:Matrix:Authorized:

Surrogate

'Volatile OrganicsTarget Compound List (TCL)

Method 8240Barr Engineering CompanyFilter Cake028302-0002-SASOLID Sampled: 17 MAR 9326 MAR 93 Prepared: 26 MAR 93

Enseco


4 -Bromof1uorobenzenel,2-Dichloroethane-d4

Recovery

9997

Note B : Compound is also detected in the blank.Percent Moisture is 25.2%. All results and limits are reported on a dry weight basis.Note J : Result is detected below the reporting limit or is an

estimated concentration.ND - Not detectedNA - Not applicableReported By: Leslie Joy Approved By: MaryHelen Hand

EnsecoTENTATIVELY IDENTIFIED COMPOUNDS

FOR


SAMPLE NUMBER 028302-0002-SA

Compound Name

Benzene, l-Ethyl-2-Methyl-Benzene, 1,2,4-Trimethyl-DecaneBenzene, 1,2,4-Trimethyl -Naphthalene, Decahydro-, trans-Benzene, 1-Methyl-3-Propyl-Benzene, l-Ethyl-2,4-Dimethyl-UndecaneBenzene, 1-Ethyl-3,5-Dimethyl-IH-Indene, 2,3-Dihydro-2-Methyl

Fraction

VOAVOAVOAVOAVOAVOAVOAVOAVOAVOA

ConfidenceLevel

1111122122

EstimatedConcentration

ug/kg

310045007600860029002900490015000110009100

NOTES:

Confidence Levels

Level 3 - Confirmed IdentificationLevel 2 - Confident IdentificationLevel 1 - Tentative Identification

Please refer to the discussion for further details.

—————————————— EnsecoS A Cumin,; C\.mP.im

Total Metals

Client Name: Barr Engineering CompanyClient ID: SludgeLab ID: 028302-0001-SAMatrix: SOLID Sampled: 17 MAR 93 Received: 25 MAR 93Authorized: 26 MAR 93 Prepared: See Below Analyzed: See Below

Dry Weight Reporting Analytical Prepared AnalyzedParameter Result 'Units Limit Method Date Date

Arsenic 7.3 mg/kg 1.6 7060 15 APR 93 22 APR 93Barium 3750 mg/kg 3.3 6010 15 APR 93 20 APR 93Cadmium 6.7 mg/kg 1.6 6010 15 APR 93 20 APR 93Chromium 29.0 mg/kg 3.3 6010 15 APR 93 20 APR 93Lead 27500 mg/kg 16.3 6010 15 APR 93 20 APR 93Mercury ND mg/kg 0.16 7471 12 APR 93 13 APR 93Selenium ND mg/kg 16.3 7740 15 APR 93 21 APR 93Silver ND mg/kg 3.3 6010 15 APR 93 20 APR 93

Percent Moisture is 38.7%. All results and limits are reported on a dry weight basis.ND - Not detectedNA = Not applicable

Reported By: Debra Hosford Approved By: Jeff Malecha


ParameterArsenicBariumCadmiumChromiumLeadMercurySeleniumSilver

MetalsTotal Metals

Barr Engineering CompanyFilter Cake028302-0002-SASOLID Sampled: 17 MAR 9326 MAR 93 Prepared: See Below

EnsecoCompjmA C

Received: 25 MAR 93Analyzed: See Below

Result4.9

3512.011.5

6510NDNOND

Dry Weight Reporting AnalyticalUnits Limit Method

Prepared AnalyzedDate Date

mg/kgmg/kgmg/kgmg/kgmg/kgmg/kgmg/kgmg/kg

1.31.30.671.36.70.136.71.3

70606010601060106010747177406010

15 APR 9315 APR 9315 APR 9315 APR 9315 APR 9312 APR 9315 APR 9315 APR 93

22 APR 9320 APR 9320 APR 9320 APR 9320 APR 9313 APR 9321 APR 9320 APR 93

Percent Moisture is 25.2%. All results and limits are reported on a dry weight basis.

ND - Not detectedNA = Not applicableReported By: Debra Hosford Approved By: Jeff Malecha

——————————————;————:——————————————— EnsecoMetal S A C"rTlin>: Compj

Total MetalsClient Name: Barr Engineering CompanyClient ID: Leached solid from the sludgeLab ID: 028302-0003-SAMatrix: SOLID Sampled: 17 MAR 93 Received: 25 MAR 93Authorized: 26 MAR 93 Prepared: See Below Analyzed: See Below

- Dry Wt. Reporting Analytical Prepared AnalyzedParameter Result Units Limit Method Date DateArsenic 7.6 mg/kg 5.0 7060 15 APR 93 22 APR 93Barium 2410 mg/kg 5.0 6010 15 APR 93 20 APR 93Cadmium 4.0 mg/kg 2.5 6010 15 APR 93 20 APR 93Chromium 20.1 mg/kg 5.0 6010 15 APR 93 20 APR 93Lead 8130 mg/kg 5.0 6010 04 MAY 93 11 MAY 93Mercury NO mg/kg 0.10 7471 14 APR 93 14 APR 93Selenium ND mg/kg 10.0 7740 15 APR 93 21 APR 93Silver ND mg/kg 5.0 6010 15 APR 93 20 APR 93

ND - Not detectedNA - Not applicableReported By: Debra Hosford Approved By: Jeff Malecha

——————————————;——————————————————— EnsecoMetalS A G-rnrn, 0-mp.m

Total Metals

Client Name: Barr Engineering CompanyClient ID: Leached solid from filter cakeLab ID: 028302-0004-SAMatrix: SOLID Sampled: 17 MAR 93 Received: 25 MAR 93Authorized: 26 MAR 93 Prepared: See Below Analyzed: See Below

- Dry -Wt. Reporting Analytical Prepared AnalyzedParameter Result Units Limit Method Date Date

Arsenic 6.4 mg/kg 0.50 7060 15 APR 93 22 APR 93Barium 642 mg/kg 1.0 6010 15 APR 93 20 APR 93Cadmium 2.8 mg/kg 0.50 6010 15 APR 93 20 APR 93Chromium 19.2 mg/kg 1.0 6010 15 APR 93 20 APR 93Lead 7780 mg/kg 5.0 6010 04 MAY 93 11 MAY 93Mercury ND mg/kg 0.10 7471 14 APR 93 14 APR 93Selenium ND mg/kg 10.0 7740 15 APR 93 21 APR 93Silver ND mg/kg 1.0 6010 15 APR 93 20 APR 93

ND = Not detectedNA - Not applicableReported By: Debra Hosford Approved By: Jeff Malecha

EnsecoS A Oimmi; Cumparn

Total Metals

Client Name: Barr Engineering CompanyClient ID: Leachate/extract from sludgeLab ID: 028302-0005-SAMatrix- LEACHATE Sampled: 17 MAR 93 Received: 26 MAR 93Authorized: 26 MAR 93 Prepared: See Below Analyzed: See Below

Wet wt. Reporting Analytical Prepared AnalyzedParameter Result Units " Limit Method Date Date

Lead 4490 mg/kg 5.0 6010 04 MAY 93 05 MAY 93


-— EnsecoS A Cumins Compj

Total Metals

Client Name: Barr Engineering CompanyClient ID: Leachate/extract from filter cakeLab ID: 028302-0006-SAMatrix: LEACHATE Sampled: 17 MAR 93 Received: 25 MAR 93Authorized: 26 MAR 93 Prepared: See Below Analyzed: See Below

Wet wt. Reporting Analytical Prepared AnalyzedParameter Result "Units' Limit Method Date DateLead 1970 mg/kg 5.0 6010 04 APR 93 05 MAY 93

ND = Not detectedNA = Not applicable


'General Inorganics Enseco


Parameter

Barr Engineering CompanySludge028302-0001-SASOLID Sampled: 17 MAR 9326 MAR 93 Prepared: See Below


CyanideSulfide, Total

Result4.9

ND

Qry Weight Reporting AnalyticalUnits Limit Method


mg/kgmg/kg

0.820.82

9010/9012376.2 Mod.

NANA

21 APR 9308 APR 93


ND - Not detectedNA - Not appl icableReported By: Lavon Trujillo Approved By: Pam Rosas

'General Inorganics Enseco


Parameter

Barr Engineering CompanyFilter Cake028302-0002-SASOLID Sampled: 17 MAR 9326 MAR 93 Prepared: See Below


CyanideSulfide, Total

ResultNDND

JDry Weight Reporting AnalyticalUnits Limit Method


mg/kgmg/kg

0.670.67

9010/9012376.2 Mod.

NANA

21 APR 9308 APR 93

Percent Moisture is 25.2%. All results and limits are reported on a dry weight basis.ND - Not detectedNA - Not applicable

Reported By: Lavon Trujillo Approved By: Pam Rosas

; ——————————— EnsecoA Cumine Ciininj

IV. QUALITY CONTROL REPORT

The Enseco laboratories operate under a vigorous QA/QC program designed toensure the generation of scientifically valid, legally defensible data bymonitoring every aspect of laboratory operations. Routine QA/QC proceduresinclude the use of approved methodologies, independent verification ofanalytical standards, use of duplicate Laboratory Control Samples to assessthe precision and accuracy of the methodology on a routine basis, and arigorous system of data review.

A. Standard Enseco QC

The standard laboratory QC package is designed to:

1) establish a strong, cost-effective QC program that ensures thegeneration of scientifically valid, legally defensible data

2) assess the laboratory's performance of the analytical methodusing control limits generated with a well-defined matrix

3) establish clear-cut guidelines for acceptability of analyticaldata so that QC decisions can be made immediately at the bench,and

4) provide a standard set of reportables which assures the clientof the quality of his data.

The Enseco QC program is based upon monitoring the precision and accuracyof an analytical method by analyzing a set of Duplicate Control Samples (DCS)at frequent, well-defined intervals. Each DCS is a well-characterized matrixwhich is spiked with target compounds at 5-100 times the reporting limit,depending upon the methodology being monitored. The purpose of the DCS is notto duplicate the sample matrix, but rather to provide an interference-free,homogeneous matrix from which to gather data to establish control limits.These limits are used to determine whether data generated by the laboratory onany given day is in control.

EnsecoA Cumins Ci'mpon\

Control limits for accuracy (percent recovery) are based on the average,historical percent recovery +/- 3 standard deviation units. Control limitsfor precision (relative percent difference) range from 0 (identical duplicateDCS results) to the average, historical relative percent difference + 3standard deviation units. These control limits are fairly narrow based on theconsistency of the matrix being monitored and are updated on a quarterlybasis.

For each batch of samples analyzed, an additional control measure is takenin the form of a Single Control Sample (SCS). The SCS consists of a controlmatrix that is spiked with surrogate compounds appropriate to the method beingused. In cases where no surrogate is available, (e.g., metals or conventionalanalyses) a single DCS serves as the control sample. An SCS is prepared foreach sample lot for which the DCS pair are not analyzed. The recovery of theSCS is charted in exactly the same manner as described for the DCS, andprovides a daily check on the performance of the method.

Accuracy for DCS and SCS is measured by Percent Recovery.

Measured Concentration% Recovery - —————————————————— X 100

Actual Concentration

Precision for DCS is measured by Relative Percent Difference (RPD).

I Measured Concentration DCS1 - Measured Concentration DCS2 IRPD - ———————————————————————————————————————————— X 100

(Measured Concentration DCS1 + Measured Concentration DCS2J/2

All samples analyzed concurrently by the same test are assigned the sameQC lot number. Projects which contain numerous samples, analyzed over severaldays, may have multiple QC lot numbers associated with each test. The QCinformation which follows includes a listing of the QC lot numbers associatedwith each of the samples reported, DCS and SCS (where applicable) recoveriesfrom the QC lots associated with the samples, and control limits for theselots. The QC data is reported by test code, in the order that the tests arereported in the analytical results section of this report.

; ~~~~~————————————- •':-. Enseco

B. Project-Specific QC

With this project, additional QC was requested in the form of duplicatesample analyses and/or spiked sample analyses. The use of an actual sample asthe QC matrix is termed "project-specific" QC.

Project-specific QC is valuable 1n assessing the affect of the samplematrix on the performance of the analytical method. No QC limits for accuracyand precision are assigned to data generated on actual sample matrices due tothe variability of the matrix.

The results of the duplicate and spike sample analyses follow. For matrixspike analyses, the project specific QC results contain the analytical resultsfrom both analyses along with the spike level and percent recovery. Thepercent recovery calculation is not performed if the spike level is less thanor equal to 25% of the value in the sample.

For duplicate analyses, the results from both the analyses are reportedalong with the relative percent difference (RPD). An RPD is not calculated ifone of the results is reported as ND.

EnsecoA Cumi

QC LOT ASSIGNMENT REPORTVolatile Organics by GC/MS

Laboratory QC Lot Number QC Run NumberSample Number QC Matrix QC Category (DCS) (SCS/BLANK)

028302-0001-SA SOIL 8240-S 23 MAR 93-A 26 MAR 93-A028302-0001-MS SOIL - 8240-S 23 MAR 93-A 26 MAR 93-A028302-0001-SD SOIL 8240-S 23 MAR 93-A 26 MAR 93-A028302-0002-SA SOIL 8240-S 23 MAR 93-A 26 MAR 93-A028302-0002-MS SOIL 8240-S 23 MAR 93-A 26 MAR 93-A028302-0002-SD SOIL 8240-S 23 MAR 93-A 26 MAR 93-A

DUPLICATE CONTROL SAMPLE REPORTVolatile Organics by GC/MS

EnsecoA Coming Compjm

AnalyteConcentration Accuracy Precisior

Spiked Measured Average(%) (RPD)OCS1 DCS2 AVG DCS Limits DCS L i m i t

Category: 8240-SMatrix: SOILQC Lot: 23 MAR 93-AConcentration Units: ug/kg1,1-DichloroetheneTrichloroetheneBenzeneTolueneChlorobenzene

50005000500050005000

46805220510056105510

45504700469051605180

46204960490053805340

929998108107

53-12070-11874-12976-13676-131

2.8108.48.46.2

21ie1717IE

Calculations are performed before rounding to avoid round-off errors in calculated results.

SINGLE CONTROL SAMPLE REPORTVolatile Organics by GC/MS

EnsecoA Cumini; Ci'mpj

AnalyteConcentrationSpiked Measured

Accuracy (%)SCS Limits

Category: 8240-SMatrix: SOILQC Lot: 23 MAR 93-A QC RunConcentration Units: ug/kg

l,2-Dichloroethane-d44-BromofluorobenzeneToluene-d8

26 MAR 93-A

500050005000

514050305300

103 79-126101 83-123106 84-128

Calculations are performed before rounding to avoid round-off errors in calculated results

; : ———— EnsecoA Ci'mini; Ci'mpa

METHOD BLANK REPORTVolatile Organics by GC/MS (cont.)

ReportingAnalyte Result Units Limit

Test: 8240CPM-TCL-SMatrix: SOLIDQC Lot: 23 MAR 93-A QC Run: 26 MAR 93-A

Acetone 1200 ug/kg 1000Benzene ND ug/kg 500Bromodichloromethane ND ug/kg 500Bromoform ND ug/kg 500Bromomethane ND ug/kg 10002-Butanone (MEK) 590 ug/kg 1000 JCarbon disulfide ND ug/kg 500Carbon tetrachloride ND ug/kg 500Chlorobenzene ND ug/kg 500Chloroethane ND ug/kg 1000Chloroform ND ug/kg 500Chloromethane ND ug/kg 1000Di bromochloromethane ND ug/kg 5001.1-Dichloroethane ND ug/kg 5001.2-Dichloroethane ND ug/kg 5001.1-Di chloroethene ND ug/kg 5001.2-Dichloroethene

(total) ND ug/kg 5001,2-Dichloropropane ND ug/kg 500cis-l,3-Dichloropropene ND ug/kg 500trans-l,3-Dichloropropene ND ug/kg 500Ethyl benzene ND ug/kg 5002-Hexanone ND ug/kg 10001,2-Dibromoethane (EDB) ND ug/kg 1000Methylene chloride 160 ug/kg 500 J4-Methyl-2-pentanone(MIBK) ND ug/kg 1000

Styrene ND ug/kg 5001,1,2,2-Tetrachloroethane ND ug/kg 500Tetrachloroethene ND ug/kg 500Toluene 110 ug/kg 500 J1.1.1-Tri chloroethane ND ug/kg 5001.1.2-Trichloroethane ND ug/kg 500Trichloroethene ND ug/kg 500Vinyl acetate ND ug/kg 1000Vinyl chloride ND ug/kg 1000Xylenes (total) ND ug/kg 500

J = Result is detected below the reporting limit or is anestimated concentration.

MATRIX SPECIFIC QCASSIGNMENT REPORTVolatile Organics by 6C/MS

QCSAMPLE TYPE

MATRIX SPIKE DUPLICATEMATRIX SPIKE

TEST

8240CPM-TCL-S8240CPM-TCL-S


8240CPM-TCL-S8240CPM-TCL-S

Enseco

LABORATORYSAMPLE NUMBER

028302-0001-SD028302-0001-MS

028302-0002-SD028302-0002-MS

QCLOT

23 MAR 93-A23 MAR 93-A

23 MAR 93-A23 MAR 93-A

; — — — — — — — EnsecoA Coming Cumparu

MATRIX SPIKE / MATRIX SPIKE DUPLICATE REPORTVolatile Organics by GC/MS

ConcentrationMatri x Matri x Spi ked %Recovery %

Analyte Sample Spike Spike Dup MS MSD MS MSD RPD

Test: 8240CPM-TCL-SMatrix SOLIDSample: 028302-0001Units: ug/kgBenzene 490 J 6400 6300 8200 8200 73 71 2Chlorobenzene ND 6900 6900 8200 8200 85 84 01,1-Di chloroethene ND 4300 4700 8200 8200 53 57 8Toluene 6800 16000 11000 8200 8200 107 58 60Trichloroethene 310 J 6200 6100 8200 8200 72 72 0

Test: 8240CPM-TCL-SMatrix SOLIDSample: 028302-0002Units: ug/kgBenzene 240 J 5400 5300 6700 6700 77 76 1Chlorobenzene ND 6300 5600 6700 6700 94 84 111,1-Di chloroethene ND 4400 4000 6700 6700 65 60 8To!uene 3500 8800 9000 6700 6700 79 82 4Trichloroethene ND 5300 5100 6700 6700 79 76 5

J * Result is detected below the reporting limit or is anestimated concentration.

ND - Not detectedNC = Not calculated, calculation not applicableAll results and spike amounts are reported on a dry weight basis.All calculations are performed before rounding to avoid round-offerrors in calculated results.

QC LOT ASSIGNMENT REPORTMetals Analysis and Preparation

Enseco

LaboratorySample Number028302-0001-SA028302-0001-SA028302-0001-SA028302-0001-SA028302-0001-MS028302-0001-MS028302-0001-MS028302-0001-MS028302-0001-SD028302-0001-SD028302-0001-SD028302-0001-SD028302-0002-SA028302-0002-SA028302-0002-SA028302-0002-SA028302-0002-MS028302-0002-MS028302-0002-MS028302-0002-MS028302-0002-SD028302-0002-SD028302-0002-SD028302-0002-SD028302-0003-SA028302-0003-SA028302-0003-SA028302-0003-SA028302-0003-SA028302-0003-MS028302-0003-MS028302-0003-MS028302-0003-MS028302-0003-MS028302-0003-SD028302-0003-SD028302-0003-SD028302-0003-SD028302-0003-SD028302-0004-SA028302-0004-SA028302-0004-SA028302-0004-SA028302-0004-SA028302-0004-MS028302-0004-MS028302-0004-MS

QC Matrix

SOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOIL

QC Category

ICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SICP-SHG-CVAA-SAS-FAA-S

QC Lot Number(DCS)

15 APR 93-1A12 APR 93-1B15 APR 93-1A15 APR 93-1A15 APR 93-1A12 APR 93-1815 APR 93-1A15 APR 93-1A15 APR 93-1A12 APR 93-1B15 APR 93-1A15 APR 93-1A15 APR 93-1A12 APR 93-1B15 APR 93-1A15 APR 93-1A15 APR 93-1A12 APR 93-1B15 APR 93-1A15 APR 93-1A15 APR 93-1A12 APR 93-1B15 APR 93-1A15 APR 93-1A15 APR 93-1A14 APR 93-1C15 APR 93-1A15 APR 93-1A04 MAY 93-1B15 APR 93-1A14 APR 93-1C15 APR 93-1A15 APR 93-1A04 MAY 93-IB15 APR 93-1A14 APR 93-1C15 APR 93-1A15 APR 93-1A04 MAY 93-1B15 APR 93-1A14 APR 93-1C15 APR 93-1A15 APR 93-1A04 MAY 93-IB15 APR 93-1A14 APR 93-1C15 APR 93-1A

QC Run Number(SCS/BLANK)

15 APR 93-1A12 APR 93-1B15 APR 93-1A15 APR 93-1A15 APR 93-1A12 APR 93-1B15 APR 93-1A15 APR 93-1A15 APR 93-1A •12 APR 93-1815 APR 93-1A15 APR 93-1A15 APR 93-1A12 APR 93-1B15 APR 93-1A15 APR 93-1A15 APR 93-1A12 APR 93-1B15 APR 93-1A15 APR 93-1A15 APR 93-1A12 APR 93-1B15 APR 93-1A15 APR 93-1A15 APR 93-1A14 APR 93-1C15 APR 93-1A15 APR 93-1A04 MAY 93-1B15 APR 93-1A14 APR 93-1C15 APR 93-1A15 APR 93-1A04 MAY 93-1B15 APR 93-1A14 APR 93-1C15 APR 93-1A15 APR 93-1A04 MAY 93-1615 APR 93-1A14 APR 93-1C15 APR 93-1A15 APR 93-1A04 MAY 93-1815 APR 93-1A14 APR 93-1C15 APR 93-1A

QC LOT ASSIGNMENT REPORTMetals Analysis and Preparation (cont.)

EnsecoA Com me Compare

LaboratorySample Number

028302-0004-MS028302-0004-MS028302-0004-SD028302-0004-SD028302-0004-SD028302-0004-SD028302-0004-SD028302-0005-SA028302-0005-MS028302-0005-SD028302-0006-SA028302-0006-MS028302-0006-SD

QC Matrix

SOILSOILSOILSOIL"SOILSOILSOILSOILSOILSOILSOILSOILSOIL

QC Category

SE-FAA-SICP-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SICP-SICP-SICP-SICP-SICP-SICP-S

QC Lot Number(DCS)15 APR 93-1A04 MAY 93-1B15 APR 93-1A14 APR 93-1C15 APR 93-1A15 APR 93-1A04 MAY 93-1804 MAY 93-IB04 MAY 93-IB04 MAY 93-1B04 MAY 93-1B04 MAY 93-IB04 MAY 93-16


15 APR 93-1A04 MAY 93-IB15 APR 93-1A14 APR 93-1C15 APR 93-1A15 APR 93-1A04 MAY 93-1B04 MAY 93-1604 MAY 93-IB04 MAY 93-IB04 MAY 93-IB04 MAY 93-IB04 MAY 93-1B

DUPLICATE CONTROL SAMPLE REPORTMetals Analysis and Preparation

Enseco

AnalyteConcentration

SpikedDCS1

MeasuredDCS2 AVG

Accuracy PrecisionAverage(%) (RPD)

DCS Limits DCS Limit

Category: ICP-SMatrix: SOILQC Lot: 15 APR 93-1AConcentration Units:

AluminumAntimonyArsenicBariumBeryl 1iumCadmiumCalciumChromiumCobaltCopperIronLeadMagnesiumManganeseMolybdenumNickelPotassiumSilverSodiumVanadiumZinc

mg/kg1070055.21455031291547390151122162

1540014837404231591664050104747154530

893050.31404571291427030140115157

143001333650414150155

367097.6870144491

811047.1136455129143

6910133114155

134001323530407149155339097.6909142490

852048.71384561291426970136114156

138001333590411150155

353097.6889143491

80889591100929490949690909697949487941199393

47-15318-36259-14176-12453-13168-13279-12166-13370-13070-13266-13466-13574-12674-12571-12967-13368-13276-12457-13073-12765-135

9.66.63.00.40.20.71.74.80.61.06.40.83.41.70.80.18.00.14.41.90.2

205020202020202020202020202020202020202020

Category: HG-CVAA-SMatrix: SOILQC Lot: 12 APR 93-1BConcentration Units: mg/kg

Mercury 29.0 32.1 32.9 32.5 112 52-148 2.3 20

Category: AS-FAA-SMatrix: SOILQC Lot: 15 APR 93-1AConcentration Units:

Arsenic

mg/kg145 132 134 133 92 59-141 1.5 20


DUPLICATE CONTROL SAMPLE REPORTMetals Analysis and Preparation (cont.)

EnsecoA Curmnp Cumpj


SpikedOCS1

MeasuredOCS2 AVG

Accuracy PrecisionAverage(%) (RPO)


Category: SE-FAA-SMatrix: SOILQC Lot: 15 APR 93-1AConcentration Units:

Selenium

mg/kg

143 137 132 134 94 68-132 4.1 20

Category: HG-CVAA-SMatrix: SOILQC Lot: 14 APR 93-1CConcentration Units: mg/kgMercury 29.0 31.9 32.2 32.0 111 52-148 0.9 20

Category: ICP-SMatrix: SOILQC Lot: 04 MAY 93-1BConcentration Units: mg/kg

AluminumAntimonyArsenicBariumBerylliumCadmiumCalciumChromiumCobaltCopperIronLeadMagnesiumManganeseMolybdenumNickelPotassiumSilverSodiumVanadiumZ inc

1070055.21455031291547390151122162

1540014837404231591664050104747154530

901045.6122445117144

6720146111153

141001283620406142149

351044.91040138504

959043.01164281141376490143107152

14200122

3610398141144359038.5980138487

930044.3119437116141

6610145109153

14100125

3620402141146

355041.71010138495

8780828790918996909492859795898888401359093

47-15318-36259-14176-12453-13168-13279-12166-13370-13070-13266-13466-13574-12674-12571-12967-13368-13276-12457-13073-12765-135

6.26.05.03.82.74.63.52.03.70.71.05.00.22.20.83.32.4155.90.23.5

205020202020202020202020202020202020202020


METHOD BLANK REPORTMetals Analysis and Preparation

EnsecoA Coming Company

Analyte ResultReporting

Units Limit

Test: ICP-RCRA-SMatrix: SOLIDQC Lot: 15 APR 93-1A QC Run: 15 APR'93-1A

BariumCadmiumChromiumLeadSilver

NDNDNDNDND

mg/kgmg/kgmg/kgmg/kgmg/kg

1.00.501.05.01.0

Test: HG-CVAA-SMatrix: SOLIDQC Lot: 12 APR 93-1B QC Run: 12 APR 93-1B

Mercury ND mg/kg 0.10

Test: AS-FAA-SMatrix: SOLIDQC Lot: 15 APR 93-1A QC Run: 15 APR 93-1A

Arsenic ND mg/kg 0.50

Test: SE-FAA-SMatrix: SOLIDQC Lot: 15 APR 93-1A QC Run: 15 APR 93-1A

Selenium ND mg/kg 0.50

Test: ICP-RCRA-SMatrix: SOLIDQC Lot: 15 APR 93-1A QC Run: 15 APR 93-1A


NDNDNDNDND


1.00.501.05.01.0

METHOD BLANK REPORTMetals Analysis and Preparation (cont.)

!i EnsecoA Commp Compjru


Units Limit

Test: HG-CVAA-SMatrix: SOLIDQC Lot: 12 APR 93-1B QC Run: 12 APR

Mercury ND nig/kg 0.10






Barium . NDCadmium NDChromium NDSilver ND

mg/kgmg/kgmg/kgmg/kg

1.00.501.01.0

Test: HG-CVAA-SMatrix: SOLIDQC Lot: 14 APR 93-1C QC Run: 14 APR 93-1C





EnsecoA Coming Cumpjm


Units Limit



Test: ICP-SMatrix: SOLIDQC Lot: 04 MAY 93-1B QC Run: 04 MAY 93-1B

Lead ND mg/kg 5.0


BariumCadmiumChromiumSilver

NDNDNDND

mg/kgmg/kgmg/kgmg/kg

1.00.501.01.0

Test: HG-CVAA-SMatrix: SOLIDQC Lot: 14 APR 93-1C QC Run: 14 APR 93-1C







EnsecoA Cum m j; C.>mpjni


Units Limit

Test: ICP-SMatrix: SOLIDQC Lot: 04 MAY 93-1B QC Run: 04 MAY '93-IB

Lead ND mg/kg 5.0

Test: ICP-WMatrix: LEACHATEQC Lot: 04 MAY 93-1B QC Run: 04 MAY 93-1BLead ND mg/kg 5.0

MATRIX SPECIFIC QCASSIGNMENT REPORTMetals Analysis and Preparation

EnsecoA C

QCSAMPLE TYPE TEST

MATRIX SPIKE DUPLICATE ICP-RCRA-SMATRIX SPIKE ICP-RCRA-S

MATRIX SPIKE DUPLICATE HG-CVAA-SMATRIX SPIKE HG-CVAA-S

MATRIX SPIKE DUPLICATE AS-FAA-SMATRIX SPIKE AS-FAA-S

MATRIX SPIKE DUPLICATE SE-FAA-SMATRIX SPIKE SE-FAA-S









MATRIX SPIKE DUPLICATE ICP-SMATRIX SPIKE ICP-S




028302-0001-SD028302-0001-MS

028302-0001-SD028302-0001-MS

028302-0001-SD028302-0001-MS

028302-0001-SD028302-0001-MS

028302-0002-SD028302-0002-MS

028302-0002-SD028302-0002-MS

028302-0002-SD028302-0002-MS

028302-0002-SD028302-0002-MS

028302-0003-SD028302-0003-MS028302-0003-SD028302-0003-MS

028302-0003-SD028302-0003-MS

028302-0003-SD028302-0003-MS

028302-0003-SD028302-0003-MS

028302-0004-SD028302-0004-MS

028302-0004-SD028302-0004-MS

QCLOT

15 APR 93-1A15 APR 93-1A

12 APR 93-1B12 APR 93-1B

15 APR 93-1A15 APR 93-1A

15 APR 93-1A15 APR 93-1A

15 APR 93-1A15 APR 93-1A

12 APR 93-1B12 APR 93-18

15 APR 93-1A15 APR 93-1A

15 APR 93-1A15 APR 93-1A

15 APR 93-1A15 APR 93-1A

14 APR 93-1C14 APR 93-1C

15 APR 93-1A15 APR 93-1A

15 APR 93-1A15 APR 93-1A

04 MAY 93-1B04 MAY 93-IB

15 APR 93-1A15 APR 93-1A

14 APR 93-1C14 APR 93-1C


028302-0004-SD028302-0004-MS

15 APR 93-1A15 APR 93-1A

r tnsecoA Cumin); Ci'mpon

MATRIX SPECIFIC QCASSIGNMENT REPORTMetals Analysis and Preparation (cont.)

QCSAMPLE TYPE





TEST

SE-FAA-S -SE-FAA-S

ICP-SICP-S

ICP-WICP-W

ICP-WICP-W


028302-0004-SD028302-0004-MS

028302-0004-SD028302-0004-MS

028302-0005-SD028302-0005-MS

028302-0006-SD028302-0006-MS

QCLOT

15 APR 93-1A15 APR 93-IA

04 MAY 93-1B04 MAY 93-1B

04 MAY 93- IB04 MAY 93- IB

04 MAY 93- IB04 MAY 93-18

EnsecoMATRIX SPIKE / MATRIX SPIKE DUPLICATE REPORTMetals Analysis and Preparation

Compjn\

Analyte SampleConcentration

Matrix MatrixSpike Spike Dup

Spiked %Recovery %MS MSD MS MSD RPD

Test: ICP-RCRA-SMatrix SOLIDSample: 028302-0001Units: mg/kg


37506.729.027500

ND

387011.050.0200007.9

447014.052.1246006.5

3268.2

32.681.58.2

3268.2

32.681.58.2

NC5464NC97

NC9071NC80

NC509

NC20

Test: HG-CVAA-SMatrix SOLIDSample: 028302-0001Units: mg/kgMercury ND 0.69 0.82 0.82 0.82 84 101 18

Test: AS-FAA-SMatrix SOLIDSample: 028302-0001Units: mg/kg

Arsenic 7.3 11.7 13.6 4.9 4.9 90 130 36

Test: SE-FAA-SMatrix SOLIDSample: 028302-0001Units: mg/kg

Selenium ND 5.1 3.8 4.9 4.9 103 77 30


BariumCadmiumChromium

3512.0

11.5

5507.5

39.7

4317.5

31.0

2676.7

26.7

2676.7

26.7

7482106

308373

851

36

ND = Not detectedNC = Not calculated, calculation not applicableAll results and spike amounts are reported on a dry weight basis.

All calculations are performed before rounding to avoid round-offerrors in calculated results.

; '————————————————— - EnsecoMATRIX SPIKE / MATRIX SPIKE DUPLICATE REPORTMetals Analysis and Preparation (cont.)

ConcentrationMatrix Matrix Spiked %Recovery %

Analyte Sample Spike Spike Dup MS MSD MS MSD RPDLead 6510 6180 3830 66.9 66.9 NC NC NCSilver NO 5.2 5.4 6.7 6.7 77 80 4

Test: HG-CVAA-SMatrix SOLIDSample: 028302-0002Units: mg/kgMercury NO 0.60 0.58 0.67 0.67 90 86 4

Test: AS-FAA-SMatrix SOLIDSample: 028302-0002Units: mg/kgArsenic 4.9 9.0 8.8 4.0 4.0 102 97 5


Selenium ND 2.9 3.1 4.0 4.0 72 77 7


BariumCadmiumChromiumSilver

Test: HG-CVAA-SMatrix SOLIDSample: 028302-0003Units: mg/kgMercury ND 0.42 0.42 0.50 0.50 84 85

ND = Not detectedNC - Not calculated, calculation not applicableAll results and spike amounts are reported on a dry weight basis.


24104.020.1ND

24508.5

33.74.9

20308.133.65.4

2005.020.05.0

2005.020.05.0

NC916899

NC8468108

NC809

MATRIX SPIKE / MATRIX SPIKE DUPLICATE REPORTMetals Analysis and Preparation (cont.)

1 EnsecoA Cuminfi Cumpjnv

Analyte


Sample Spike Spike Dup MS MSD MS MSD RPD

Test: AS-FAA-SMatrix SOLIDSample: 028302-0003Units: mg/kg

Arsenic 7.6 9.8 9.6 3.0 3.0 72 67


Selenium NO 3.5 2.3 3.0 3.0 117 77 41

Test: ICP-SMatrix SOLIDSample: 028302-0003Units: mg/kgLead 8130 12600 14400 50.0 50.0 NC NC NC

Test: ICP-RCRA-SMatrix SOLIDSample: 028302-0004Units: mg/kgBariumCadmiumChromiumSilver

6422.819.2ND

8237.0

35.34.0

8277.5

37.34.0

2005.020.05.0

2005.020.05.0

90858181

92949179

310122

Test: HG-CVAA-SMatrix SOLIDSample: 028302-0004Units: mg/kg

Mercury ND 0.43 0.49 0.50 0.50 87 99 13

ND - Not detectedNC - Not calculated, calculation not applicable


; ~~~————— -. EnsecoMATRIX SPIKE / MATRIX SPIKE DUPLICATE REPORTMetals Analysis and Preparation (cont.)


Analyte Sample Spike Spike Dup MS MSO MS MSD RPD

Test: AS-FAA-SMatrix SOLIDSample: 028302-0004Units: nig/kgArsenic 6.4 15.4 10.9 3.0 3.0 301 152 66

Test; SE-FAA-SMatrix SOLIDSample: 028302-0004Units: mg/kg

Selenium ND 3.1 3.0 3.0 3.0 103 100 3

Test: ICP-SMatrix SOLIDSample: 028302-0004Units: mg/kg

Lead 7780 8890 8570 50.0 50.0 NC NC NC

Test: ICP-WMatrix LEACHATESample: 028302-0005Units: mg/kgLead 4490 5810 3570 50.0 50.0 NC NC NC

Test: ICP-WMatrix LEACHATESample: 028302-0006Units: mg/kg

Lead 1970 1430 5090 50.0 50.0 NC NC NC

ND = Not detectedNC = Not calculated, calculation not applicable


QC LOT ASSIGNMENT REPORTWet Chemistry Analysis and Preparation

Enseco

LaboratorySample Number028302-0001-SA028302-0001-SA028302-0001-MS028302-0001-MS028302-0001-SD028302-0001-SD028302-0002-SA028302-0002-SA028302-0002-MS028302-0002-MS028302-0002-SD028302-0002-SD

QC Matrix

SOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOIL

QC Category

S-SCN-SS-SCN-SS-SCN-SS-SCN-SS-SCN-SS-SCN-S

QC Lot Number(DCS)

01 APR 93-1A21 APR 93-1A01 APR 93-1A21 APR 93-1A01 APR 93-IA21 APR 93-1A07 APR 93-1A21 APR 93-1A07 APR 93-1B21 APR 93-1A07 APR 93-1B21 APR 93-1A


01 APR 93-1A21 APR 93-1A01 APR 93-1A21 APR 93-1A01 APR 93-1A21 APR 93-1A07 APR 93-1A21 APR 93-1A07 APR 93-IB21 APR 93-1A07 APR 93-IB21 APR 93-1A

DUPLICATE CONTROL SAMPLE REPORTWet Chemistry Analysis and Preparation

EnsecoA Cormnu Compj

AnalyteConcentration Accuracy Precisior

Spiked Measured Average(%) (RPD)DCS1 DCS2 AVG DCS Limits DCS L i m i t

Category: S-SMatrix: SOILQC Lot: 01 APR 93-1AConcentration Units: mg/kg

Sulfide, Total 81.48 67.9 67.9 67.9 83 0-120 0.0 20C

Category: CN-SMatrix: SOILQC Lot: 21 APR 93-1AConcentration Units: mg/kgCyanide 10.0 9.90 9.70 9.80 98 75-125 2.0 2C

Category: S-SMatrix: SOILQC Lot: 07 APR 93-1AConcentration Units: mg/kg

Sulfide, Total 81.48 77.9 66.8 72.4 89 0-120 15 200

Category: S-SMatrix: SOILQC Lot: 07 APR 93-1BConcentration Units: mg/kgSulfide, Total 76.7 89.7 83.1 86.4 113 0-120 7.6 200


METHOD BLANK REPORTWet Chemistry Analysis and Preparation

EnsecoA Cummt (Ji'mn.:


Units Limit

Test: STOT-SPEC-SMatrix: SOLIDQC Lot: 01 APR 93-1A QC Run: 01 APR 93-1A

Sulfide, Total ND mg/kg 0.50

Test: CNTOT-TEC-SMatrix: SOLIDQC Lot: 21 APR 93-1A QC Run: 21 APR 93-1A

Cyanide ND mg/kg 0.50

Test: STOT-SPEC-SMatrix: SOLIDQC Lot: 01 APR 93-1A QC Run: 01 APR 93-1A


Test: CNTOT-TEC-SMatrix: SOLIDQC Lot: 21 APR 93-1A QC Run: 21 APR 93-1A

Cyanide ND mg/kg 0.50

Test: STOT-SPEC-SMatrix: SOLIDQC Lot: 07 APR 93-1A QC Run: 07 APR 93-1ASulfide, Total ND mg/kg 0.50

Test: STOT-SPEC-SMatrix: SOLIDQC Lot: 07 APR 93-18 QC Run: 07 APR 93-1B


MATRIX SPECIFIC QCASSIGNMENT REPORTWet Chemistry Analysis and Preparation

QCSAMPLE TYPE




TEST

STOT-SPEC-.SSTOT-SPEC-S

CNTOT-TEC-SCNTOT-TEC-S

STOT-SPEC-SSTOT-SPEC-S


CNTOT-TEC-SCNTOT-TEC-S

EnsecoA Citmmjt Cumpjm


028302-0001-SD028302-0001-MS

028302-0001-SD028302-0001-MS

028302-0002-SD028302-0002-MS

QCLOT

01 APR 93-1A01 APR 93-1A

21 APR 93-1A21 APR 93-1A

07 APR 93-1B07 APR 93-IB

028302-0002-SD028302-0002-MS

21 APR 93-1A21 APR 93-1A

; —————————————— S EnsecoMATRIX SPIKE / MATRIX SPIKE DUPLICATE REPORTWet Chemistry Analysis and Preparation

ConcentrationMatrix Matrix Spiked ^Recovery %

Analyte Sample Spike Spike Dup MS MSO MS MSD RPD

Test: STOT-SPEC-SMatrix SOLIDSample: 028302-0001Units: nig/kgSulfide, Total NO 2.4 3.2 3.9 3.9 62 82 29

Test: CNTOT-TEC-SMatrix SOLIDSample: 028302-0001Units: mg/kgCyanide 3.0 8.8 9.7 10.0 10.0 58 67 14

Test: STOT-SPEC-SMatrix SOLIDSample: 028302-0002Units: mg/kgSulfide, Total ND 53.7 58.3 76.7 76.7 70 76 8

Test: CNTOT-TEC-SMatrix SOLIDSample: 028302-0002Units: mg/kgCyanide ND 9.6 8.2 10.0 10.0 96 82 16

ND * Not detectedNC - Not calculated, calculation not applicableAll results and spike amounts are reported on a dry weight basis.All calculations are performed before rounding to avoid round-offerrors in calculated results.

Chain of Custody4.

1 Company8300 Norman Center DriveMinneapolis. MN 55437-1026(612) 832-2600

Jroject Number

No: N? 0769

SampleIdentification

Collection

Date Time S

Le^euS iu THK£<*V\A« Y A v G r i

Project Manager

Project Contact:

Laboratory:

'.fjfr - P.oc.Remarks/Analysis Required:

k^Mi

1ol AM f^^VfW/^l

- BTUL

Sampled By:

Ttrrn \y\rw\

Date Tim*- .

\3'.i*Received Dale Time

Received By: Relinquished By: Dale Time Time

Remarks: Samples Shipped VIAQAir Freight Q Fed. Eip.

Air Bill Number:

Distribution: While-Original Accompanies Shipment lo Lab; Yellow - Lab Coordinator; Pink-Field Copy

HUFFMAN:USTOMER #:

01570LABORATORIES, INC.Quality Analytical Services Since 1936

4630 Indiana Street • Golden, CO 80405Phone: (303) 278-4455 • FAX: (303) 278-7012

DATE 4/23/93LAB# 151893P.O.RECD 04/06/93

ANALYSIS REPORT

GRANT PAULBARR ENGINEERING COMPANY8300 NORMAN CENTER DRIVEMINNEAPOLIS MN 55437

PROJ. # 23/69-065DFS52

RECEIVEDS3

SEQUENCE/SAMPLE ID

01FC-7 28388-1

02CS-6 28388-2

03STIFF SLUDGE

04SLUDGE 28302-1

/ITROGEN-

:**AVG

JULFUR——

.% _ _ _ 0.24 - - - - - 0.16 - -

•% - - - 3.78 - - - - - 2.68 - -

;**AVG:HLORINE-•**AVG

- - - 0.16 - - - - - <0.10

- - - 6.88 - - - - - 35.17 - - - - -

**AVGVTU/LB - - - - - - 8866.- - - - - 6069.- - -

-••' -&VG

0.110.150.134.164.094.130.310.280.3037.8937.7137.80

4860.- -5116.4988.

- - - 7736,

SEQUENCE/SAMPLE ID

05FILTER CAKE*""

iTU/LB - - - - - - 6216.

;AMPLE 03 - 28388-3, SAMPLE os - 23302-2,AMPLES FC-7 28388-1 AND FILTER CAKE 28302-2 ARE NOT HOMOGENEOUS.. COMBUSTION ADDITIVE WAS USED FOR THE BTU/LB ANALYSIS. BTU/LB RESULTS ARE'HE GROSS HEATING VALUES. BTU/LB RESULTS FOR SMAPLES FC7-28388-1, CS-6 28388-2.ND STIFF SLUDGE 28388-3 HAVE BEEN CORRECTED FOR SULFUR CONTENT (BTU/LB RESULTS'OR SAMPLES SLUDGE 28302-1 AND FILTER CAKE 28302-2 HAVE NOT BEEN CORRECTED FOR'OSSIBLE SULFUR CONTENT.AW DATA ATTACHED.ITROGEN: STANDARD #3 IS ACETANILIDE (THEORY 10.36% N).

STANDARD #125 IS NICOTINIC ACID P-TOLUENESULFONATE (THEORY 4.743% N)•ULFUR: STANDARD 4.18% IS IN A COAL MATRIX (THEORY 4.18% S).IHLORINE: STANDARD #6 IS P-CHLORO-BENZOIC ACID (THEORY 22.64% CL) ..SH: STANDARD 10.51% IS IN A COAL MATRIX (THEORY 10.51% ASH).

STANDARD 11.04% IS IN A COAL MATRIX (THEORY 11.04% ASH)..TU/LB: STANDARD #4 IS BENZOIC ACID (THEORY 11372.4 BTU/LB).

Enseco Incorporated

ANALYTICAL RESULTS

A Coming CompanyBARR ENGINEERING


MAY 25, 1993

Reviewed by:

lary Walters

Enseco Incorporated4955 Yarrow StreetArvada, Colorado 80002303/421 -6611 Fax: 303/431 -7171


%EnsecoA Corning Company via- 11 K

May 25, 1993

Mr. Paul TaylorBarr Engineering8300 Norman Center DriveMinneapolis, MN 55437

Dear Mr. Taylor:

Enclosed is the report the four samples received at Enseco-Rocky MountainAnalytical Laboratory (RMAL) on April 22, 1993.

Included with the report is a quality control summary.

Please call if you have any questions.

Sincerely, Reviewed by:

Cindy PattersonProgram Administrator

Enclosures

RMAL 1028873

Gary waitersProgram Manager

Enseco Incorporated4955 Yarrow StreetArvada, Colorado 80002303/421-6611 Fax: 303/431-7171

: ————— EnsecoI. OVERVIEW ACO^C

On April 23, 1993, Enseco-Rocky Mountain Analytical Laboratory receivedfour samples from Barr Engineering Company.

This report presents the analytical results as well as supportingInformation to aid in the evaluation and interpretation of the data and isarranged in the following order:

I. OverviewII. Sample Description Information/Analytical Test RequestsIII. Analytical ResultsIV. Quality Control Report

The bulk density analysis was performed at Hauser Chemical ResearchIncorporated locate in Boulder, Colorado.

All analyses at Enseco are performed so that the maximum concentration ofsample consistent with the method 1s analyzed. Dilutions are at timesrequired to avoid saturation of the detector, to achieve linearity for aspecific target compound, or to reduce matrix interferences. In this event,reporting limits are adjusted proportionately. Surrogate compounds may not bemeasurable in samples which have been diluted.

A smaller sample volume was extracted for the Extractable PetroleumHydrocarbon GC/FID analysis due to the oily nature of the samples' matrix.Samples -0001 through -0003 could not be concentrated below final extractvolume of 10.0 ml. In addition all samples required an analytical dilutiondue to the concentration present beyond the linear range of the Instrument.The reporting limits are adjusted relative to these dilutions. Surrogatecompounds could not be measured due to the necessary dilution.

Only one gram of sample was extracted for the 8080 PCB analysis forsamples -0001, -0002, and -0004 and five grams for sample -0003 due to theoily nature of the samples. In addition, samples 028873-0001 and -0003

———————————————————————————————— EnsecoA Comms Ct'mpa

required dilutions due to the concentration of target compounds present beyondthe linear range of the instrument. The reporting limits are adjustedaccordingly. All samples had low surrogate recovery.

Samples -0001, -0003, and -0005 required dilutions for the total RCRAmetals analysis due to the concentration of lead in the samples beyond thelinear range of the instrument. The reporting limits are adjustedaccordingly. There was limited sample volume for sample -0003. The methylenechloride extraction and lead analysis was performed from the first samplereceived. The total and TCLP analysis for this sample was performed from theadditional sample volume received on May 18, 1993. Samples -0001, -0002,-0004 and -0007 were diluted for the total arsenic analysis due to matrixinterferences. Sample -0003 was diluted for the mercury analysis due to theconcentration of mercury present 1n the sample beyond the linear range of theinstrument. Sample -0003 had lead reported at 8.9 mg/L for the TCLP analysis,and the regulatory limit is 5.0 mg/L.

The pH analysis of samples -0002 and -0004 could not be performed using apH probe to obtain an accurate pH due to the oily nature of these samples andthe possibility of the destruction of the probe. pH strips were used toobtain the pH for these samples. The associated QC was performed by using theprobe. The NACE corrosivity test could not be performed on sample -0003 sinceit was not a liquid waste. The analysis is only applicable to liquid wastesamples.

Samples -0002 and -0004 exhibited a characteristic of hazardous waste.The ignitability results for the samples were 113° F and 95° F. Theregulatory level is 140° F.

RMAL samples 028873-0005 through -0008 did not physically exist on receiptat the laboratory. A portion of samples (-0001) and (-0003) were extractedwith methylene chloride to generate leached solids (-0005) and (-0006) and asolvent leachate (-0007) and (-0008).

EnsecoA Coming Citmpanv


The following procedure was followed to prepare extracted samples metalsanalysis for project 028873. The samples were homogenized and a 20 gramaliquot was placed in a glass centrifuge tube. The sample was then mixed with20 grams of methylene chloride and extracted (shaken vigorously on MOOTshaker) for 30 minutes, then centrifuged for 30 minutes. The methylenechloride extract was decanted into a separate bottle while the remaining solidportion was dried at 103°C for 30 minutes. This drying step was used toremove residual solvent, and should have also removed most of the waterremaining in the sample. Sample weights are recorded in the datadeliverables. The methylene chloride extract, remaining solid portion and thetotal sample were prepared and analyzed using RMAL SOPs based on SW846 Methods3050, 6010, and the 7000 series for Hg, As, and Se.

The total sample results are reported on a dry weight basis. Since theleached solids were dried for 30 minutes, the leached/extracted solids werereported as weighed out—in dry weight units but with no correction forpercent moisture. Results for the solvent ext-acts were also reported asweighed out—in wet weight units with no moisture correction. The sampleportion weighed included the solvent decanted plus any material whichdissolved in the solvent.

For summary purposes, the lead results were converted to total lead in thesample aliquot (see table below). A nominal 20 g aliquot was used for thesolvent extractions, so total results for the original samples are based onthe dry weight portion of a 20 g aliquot. The recorded weights for the driedleached solids and leachate were used to calculate the total lead in theseparate portions.


EnsecoA Commc Com pant

-0001-SATotal Sample

-0005-SALeached Solid

-0007-SALeachate

Total

-0003-SATotal Sample*

-0006-SALeached Solid

-0008-SALeachate

Total

ma/kg

16600'

13700

2990

22000

2060

6960

Aliquotyelaht. a

12.5

4.87

28.0

13.3

3.23

27.3

Lead

207

66.7

83.7

293

6.65

190

Percent ofTotal

32.2

40.4

72.6%

2.3

65.1

67.4%

* Initial sample aliquot (before solvent leach) was 14.84 grams due tolimited sample size.

:——————————————— EnsecoA Commp Company

II, SAMPLE DESCRIPTION INFORMATION/ANALYTICAL TEST REQUESTS


The Sample Description Information lists all of the samples received inthis project together with the internal laboratory identification numberassigned for each sample. Each project received at Enseco - RMAL is assigneda unique six digit number. Samples within the project are numberedsequentially. The laboratory identification number is a combination of thesix digit project code and the sample sequence number.



, The Analytical Test Requests lists the analyses that were performed oneach sample. The Custom Test column Indicates where tests have been modifiedto conform to the specific requirements of this project.

EnsecoA Ci'mmi; Compim



Lab ID028873-028873-028873-028873-028873-028873-028873-028873-

•0001-SA•0002-SA•0003-SA•0004-SA•0005-SA•0006-SA•0007-SA•0008-SA

Client ID

R1RCHR1PFHR1PSHR2PFHR1RCHR1PSHR1RCHR1PSH

Leached solidsLeached solidsextract/1eachateextract/1eachate

Sampled ReceivedMatrix Date Time DateSOLIDSOLIDSOLIDSOLIDSOLIDSOLIDLEACHATELEACHATE

1515161615161516

APRAPRAPRAPRAPRAPRAPRAPR

9393939393939393

1115140811141114

:00:00:00:00:00:00:00:00

2222222222222222

APRAPRAPRAPRAPRAPRAPRAPR

9393939393939393

EnsecoA Corninc Compjm

ANALYTICAL TEST REQUESTS Page 1 of 2for


Lab ID: Group Custom028873 Code Analysis Description Test?

0001 A RCRA Total Metals done by ICP NPrep - Total Metals, ICP NArsenic, Furnace AA NPrep - Total Metals, Furnace AA NSelenium, Furnace AA NExtractable Petroleum Hydrocarbons NPrep - Hydrocarbons by GC NPCBs NPrep - PCBs by GC NPercent Water NMercury, Cold Vapor AA NPrep - Mercury, Cold Vapor AA NTotal Solids (TS) N

0003 B RCRA Total Metals done by ICP NPrep - Total Metals, ICP NArsenic, Furnace AA NPrep - Total Metals, Furnace AA NSelenium, Furnace AA NExtractable Petroleum Hydrocarbons NPrep - Hydrocarbons by GC NPCBs NPrep - PCBs by GC NPercent Water NToxicity Characteristic Metals YDigestion for Metals from a TCLP leachate NTCLP Extraction / Metals Aliquot NIgnitability, Closed Cup NBulk Density N

PH HMercury, Cold Vapor AA NPrep - Mercury, Cold Vapor AA NTotal Solids (TS) N

0002 , 0004 C RCRA Total Metals done by ICP NPrep - Total Metals, ICP NArsenic, Furnace AA NPrep - Total Metals, Furnace AA NSelenium, Furnace AA NPCBs NPrep - PCBs by GC NPercent Water »pH N

EnsecoA Coffline Compam

ANALYTICAL TEST REQUESTS Page 2 of 2for



Bulk Density NToxicity Characteristic Metals YDigestion for Metals from a TCLP leachate NTCLP Extraction / Metals Aliquot NMercury, Cold Vapor AA NPrep - Mercury, Cold Vapor AA NTotal Solids (TS) NIgnitability, Closed Cup NExtractable Petroleum Hydrocarbons NPrep - Hydrocarbons by GC N

0005 - 0006 D RCRA Total Metals done by ICP NPrep - Total Metals, ICP NMercury, Cold Vapor AA NPrep - Mercury, Cold Vapor AA NArsenic, Furnace AA NPrep - Total Metals, Furnace AA NSelenium, Furnace AA N

0007 - 0008 E ICP Suite YPrep - Total Metals, ICP N

——————————————:—————————————————— EnsecoA Ciimin Com pa m

III. ANALYTICAL RESULTS

The analytical results for this project are presented in the followingdata tables. Each data table includes sample identification information, andwhen available and appropriate, dates sampled, received, authorized, preparedand analyzed. The authorization data is the date when the project was definedby the client such that laboratory work could begin. The date prepared istypically the date an extraction or digestion was initiated. For volatileorganic compounds in water, the date prepared is the date the screening of thesample was performed.

Data sheets contain a listing of the parameters measured in each test, theanalytical results and the Enseco reporting limit. Reporting limits areadjusted to reflect dilution of the sample, when appropriate.

The analytical data for this project have been corrected for the moisturecontent of the sample using the formula below:

Analytical Result___100% - % Moisture of sample * Result (dry weight)

Both the analytical results and the reporting limits have been adjusted.Because the moisture content can vary from sample to sample, reporting limitsmay also vary accordingly. The adjustment is performed automatically in LIMSby entering the unconnected values and the percent moisture. Accordingly,results in raw data, if submitted as a part of this report, will reflectvalues before the correction for the moisture content.

Surrogate recovery data is presented for all GC/MS analyses. Thesurrogate recovery is an indication of the affect of the sample matrix on theperformance of the method. The results from the Standard Enseco QA/QCProgram, which generates data which are independent of matrix effects, isgiven in Section IV.

———————— EnsecoA Cumm£ Compj

The analytical data reported are subject to the following limitations ofthe analytical methodology:

Extractable Petroleum Hydrocarbons by GC/FID

This method is based on a methylene chloride extraction of a samplefollowed by capillary column gas chromatography with flame ionizationdetection. Extractable Petroleum Hydrocarbons are reported as TotalChromatographable Organics (TCO). The TCO result was based on the entire areaunder the chromatogram as compared to a synthetic standard, ortho-terphenyl.The detection limit is based on the response of diesel #2/fuel oil #2.Reporting limits for other products may vary and can be determined. Inparticular, reporting limits for motor oils and lubricating oils will behigher.

In addition to functioning as the calibration standard, ortho-terphenyl isused as the surrogate standard. It 1s spiked into each sample to provide anevaluation of recovery for each sample. This recovery may be affected bymatrix interference or sample dilution.

The composition of various petroleum products may vary depending onrefinery operation, seasonal additives, and crude oil sources. If, on thejudgment of the analyst, the fingerprint of the sample matched the fingerprintof one of the petroleum products listed below, the product is reported in thereport footnote. In addition, the footnote contains the carbon range and anyother pertinent information on the sample. The target petroleum productsinclude:

GasolineAviation GasolineKerosenePaint ThinnerTurpentineFuel Oil 12 and Diesel 12Fuel Oil 14Fuel Oil #6Coal TarCreosoteLubricating OilsMotor OilsVegetation HydrocarbonsAsphalt

————————————— EnsecoExtractable Petroleum Hydrocarbons ACorfimcCom^

Method GC/FIDClient Name: Barr Engineering CompanyClient ID: R1RCHLab ID: 028873-0001-SAMatrix: SOLID Sampled: 15 APR 93 Received: 22 APR 93Authorized: 22 APR 93 Prepared: 28 APR 93 Analyzed: 18 MAY 93

Dry Weight ReportingParameter Result Units Limit

Total ChromatographableOrganics 350000 mg/kg 15000 1

Surrogate Recovery

o-Terphenyl ND %

Note 1 : QUALITATIVE ID: This sample has GC/FID characteristics forwhich reliable identification of a product could not beachieved. Sample resembles a hydrocarbon product occurringwithin the n-alkane range C18-C36.


ND - Not detectedNA * Not applicable

Reported By: Stan Dunlavy Approved By: Denise Howe

~ " ~ — — ™ — — — — — — — — — — r- r~\ CO/ "Y"\

Extractable Petroleum Hydrocarbons *c™™*comra

Method GC/FID

Client Name: Barr Engineering CompanyClient ID: R1PFHLab ID: 028873-0002-SAMatrix: SOLID Sampled: 15 APR 93 Received: 22 APR 93Authorized: 22 APR 93 Prepared: 28 APR 93 Analyzed: 18 MAY 93

ReportingParameter Result Units LimitTotal Chromatographable

Organics 59000 mg/kg 9900 1

Surrogate Recoveryo-Terphenyl ND %

Note 1 : QUALITATIVE ID: This sample has GC/FID characteristics thatare similar to PS-6 gasoline and an unidentifiable product.Sample resembles a hydrocarbon product occurring within then-alkane range C8-C11 and C18-C32.

ND - Not detectedNA * Not applicableReported By: Stan Dunlavy Approved By: Denise Howe

"" ""'™"———————— r* nc v"y \Extractable Petroleum Hydrocarbons *c«mmBcomrJ

Method GC/FIDClient Name: Barr Engineering CompanyClient ID: R1PSHLab ID: 028873-0003-SAMatrix: SOLID Sampled: 16 APR 93 Received: 22 APR 93Authorized: 22 APR 93 Prepared: 28 APR 93 Analyzed: 18 MAY 93

Dry Weight ReportingParameter Result Units LimitTotal Chromatographable

Organics 260000 mg/kg 4400 1Surrogate Recoveryo-Terphenyl ND %

Note 1 : QUALITATIVE ID: This sample has GC/FID characteristics forwhich reliable identification of a product could not beachieved. Sample resembles a hydrocarbon product occurringwithin the n-alkane range C14-C36.




" ' "~——— EnsecoExtractable Petroleum Hydrocarbons A 0,™, c,mp,

Method GC/FIDClient Name: Barr Engineering CompanyClient ID: R2PFHLab ID: 028873-0004-SAMatrix: SOLID Sampled: 16 APR 93 Received: 22 APR 93Authorized: 22 APR 93 Prepared: 28 APR 93 Analyzed: 18 MAY 93

ReportingParameter Result Units LimitTotal Chromatographable


Surrogate Recoveryo-Terphenyl ND %

Note 1 : QUALITATIVE ID: This sample has GC/FID characteristics thatare similar to PS-6 gasoline and an unidentifiable product.Sample resembles a hydrocarbon product occurring within then-alkane range C8-C11 and C20-C32.

ND - Not detectedNA * Not applicable



PCBs

Method 8080Barr Engineering CompanyR1RCH028873-0001-SASOLID Sampled: 15 APR 9322 APR 93 Prepared: 29 APR 93

EnsecoA Ci>

Received: 22 APR 93Analyzed: 19 MAY 93

Parameter

AroclorAroclorAroclorAroclorAroclorAroclorAroclor

1016122112321242124812541260

Result

NDNDNDND

12000NDND


ug/kgug/kgug/kgug/kgug/kgug/kgug/kg

6400640064006400640064006400

Percent Moisture is 37.7%. All results and limits are reported on a dry weight basis.ND - Not detectedNA - Not applicableReported By: Stan Dunlavy Approved By: Denise Howe

5/Enseco"* A Coming Compony

Client Name:Client ID:Lab ID:Matrix:Authorized:

Parameter

Aroclor 1016Aroclor 1221Aroclor 1232Aroclor 1242Aroclor 1248Aroclor 1254Aroclor 1260

PCBs

Method 8080

Barr Engineering CompanyR1PFH028873-0002-SASOLID Sampled: 15 APR 9322 APR 93 Prepared: 29 APR 93


Result

NDNDNDND

1200NDND

Wet Weight ReportingUnits Limit

ug/kgug/kgug/kgug/kgug/kgug/kgug/kg

970970970970970970970

ND * Not detectedNA » Not applicableReported By: Stan Dunlavy

Approved By: Denise Howe


PCBsMethod 8080

Barr Engineering CompanyR1PSH028873-0003-SASOLID Sampled: 16 APR 9322 APR 93 Prepared: 29 APR 93

EnsecoA Ci'mmR Cumponv


ParameterAroclorAroclorAroclorAroclorAroclorAroclorAroclor

1016122112321242124812541260

Result

NDNDNDND

1300NDND


ug/kgug/kgug/kgug/kgug/kgug/kg

880880880880880880880




;S?Enseco— A Coming Company

PCBsMethod 8080


Parameter

Aroclor 1016Aroclor 1221Aroclor 1232Aroclor 1242Aroclor 1248Aroclor 1254Aroclor 1260

Barr Engineering CompanyR2PFH028873-0004-SAS2°2L1DPR 93

16 APR 9329 APR 93


ResultNDNDNDND

1400NDND

Wet Weight ReportingUnits Limit

ug/kgug/kgug/kgug/kgug/jcgug/kgug/kg

970970970970970970970

ND = Not detectedNA = Not applicableReported By: Stan Dunlavy

Approved By: Denise Howe

EnsecoA Corr"nK Comp.im

Total MetalsClient Name: Barr Engineering CompanyClient ID: R1RCHLab ID: 028873-0001-SAMatrix: SOLID Sampled: 15 APR 93 Received: 22 APR 93Authorized: 22 APR 93 Prepared: See Below Analyzed: See Below

Drv Weight Reporting Analytical Prepared AnalyzedParameter Result Units Limit Method Date DateArsenic ND mg/kg 4.0 7060 10 MAY 93 12 MAY 93Barium 2520 mg/kg 3.2 6010 10 MAY 93 13 MAY 93Cadmium 3.0 mg/kg 1.6 6010 10 MAY 93 13 MAY 93Chromium 15.9 mg/kg 3.2 6010 10 MAY 93 13 MAY 93Lead 16600 mg/kg 16.1 6010 10 MAY 93 13 MAY 93Mercury ND mg/kg 0.16 7471 06 MAY 93 11 MAY 93Selenium ND mg/kg 16.1 7740 10 MAY 93 11 MAY 93Silver ND mg/kg 3.2 6010 10 MAY 93 13 MAY 93

Percent Moisture 1s 37.7%. All results and limits are reported on a dry weight basis.

ND - Not detectedNA * Not applicableReported By: Jeff Malecha Approved By: Debra Hosford

"ivEnseco™" A Coming Company

Metal s

Total Metals


ParameterArsenicBariumCadmiumChromiumLeadMercurySeleniumSilver

Barr Engineering CompanyR1PFH028873-0002-SAS2°2L$R 93

15 APR 93See Below

Received:Analyzed:

Wet Weight .Renting AnalyticalResult Units Liim

22 APR 93See Below


NDNDNDND29.5NDNDND

mg/kgrag/kgmg/kgmg/kgmg/kgmg/kgmg/kgmg/kg

5.01.00.50

2.32.01.0

70606010601060106010747177406010

10 MAY 9310 MAY 9310 MAY 9310 MAY 9310 MAY 9306 MAY 9310 MAY 9310 MAY 93


ND » Not detectedNA * Not applicableReported By: Oeff Malecha

Approved By: Debra Hosford

^•Enseco*** A Coming Company


ParameterArsenicBariumCadmi urnChromiumLeadMercurySeleniumSilver

Metals

Total Metals

Barr Engineering CompanyR2PFH028873-0004-SA Sampied: 16 APR 931§LAPR 93 PrSp5r.ds See Below

Received:Analyzed

ResultNONDNDND8.4NDNDND

Wet Weight Reporting AnalyticalUnits • Limit Method

22 APR 93See BelowPrepared AnalyzedDate Date

rag/kgmg/kgrog/kgmg/kgmg/kgmg/kgmg/kgmg/kg

2.01.00.501.05.02.52.01.0

70606010601060106010747177406010



ND - Not detectedNA - Not applicableReported By: Jeff Malecha

Approved By: Debra Hosford

" ———————- EnsecoA Cuminc Cumpo

Total MetalsClient Name: Barr Engineering CompanyClient ID: R2PFHLab ID: 028873-0004-SAMatrix: SOLID Sampled: 16 APR 93 Received: 22 APR 93Authorized: 22 APR 93 Prepared: See Below Analyzed: See Below

Dry Weight Reporting Analytical Prepared AnalyzedParameter Result Units Limit Method Date DateArsenic ND mq/kg 49.3 7060 10 MAY 93 12 MAY 93Barium ND mg/kg 24.6 6010 10 MAY 93 13 MAY 93Cadmium ND mg/kg 12.3 6010 10 MAY 93 13 MAY 93Chromium ND mg/kg 24.6 6010 10 MAY 93 13 MAY 93Lead 207 mg/kg 123 6010 10 MAY 93 13 MAY 93Mercury ND mg/kg 2.5 7471 06 MAY 93 11 MAY 93Selenium ND mg/kg 49.3 7740 10 MAY 93 11 MAY 93Silver ND mg/kg 24.6 6010 10 MAY 93 13 MAY 93


ND - Not detectedNA - Not applicableReported By: Jeff Malecha Approved By: Debra Hosford

~~~————————————— EnsecoM6t 3 I S A Cuminc (.nmfM

Total MetalsClient Name: Barr Engineering CompanyClient ID: R1RCH Leached solidsLab ID: 028873-0005-SAMatrix: SOLID Sampled: 15 APR 93 Received: 22 APR 93Authorized: 22 APR 93 Prepared: See Below Analyzed: See Below

Dry Weight Reporting Analytical Prepared AnalyzedParameter Result Units Limit Method Date DateArsenic ND mg/kg 5.0 7060 18 MAY 93 18 MAY 93Barium 486 mg/kg 2.0 6010 05 MAY 93 17 MAY 93Cadmium 3.5 mg/kg 1.0 6010 05 MAY 93 17 MAY 93Chromium 222 mg/kg 2.0 6010 05 MAY 93 17 MAY 93Lead 13700 mg/kg 10.0 6010 05 MAY 93 17 MAY 93Mercury ND mg/kg 0.10 7471 06 MAY 93 11 MAY 93Selenium ND mg/kg 20.0 7740 18 MAY 93 19 MAY 93Silver ND mg/kg 2.0 6010 05 MAY 93 17 MAY 93

PERCENT MOISTURE RESULTS ARE NOT AVAILABLE FOR THIS SAMPLEND - Not detectedNA - Not applicableReported By: Steven Gouy Approved By: Debra Hosford

————————————————:—————————————————— EnsecoMat al C A t-"minK Compjiu

Total MetalsClient Name: Barr Engineering CompanyClient ID: R1PSH Leached solidsLab ID: 028873-0006-SAMatrix: SOLID Sampled: 16 APR 93 Received: 22 APR 93Authorized: 22 APR 93 Prepared: See Below Analyzed: See Below

Dry Weight Reporting Analytical Prepared AnalyzedParameter Result Units Limit Method Date DateArsenic ND mg/kg 10.0 7060 18 MAY 93 18 MAY 93Barium 270 mg/kg 1.0 6010 05 MAY 93 17 MAY 93Cadmium 1.1 mg/kg 0.50 6010 05 MAY 93 17 MAY 93Chromium 4.9 mg/kg 1.0 6010 05 MAY 93 17 MAY 93Lead 2060 mg/kg 5.0 6010 05 MAY 93 17 MAY 93Mercury 0.97 mg/kg 0.20 7471 12 MAY 93 13 MAY 93Selenium ND mg/kg 20.0 7740 18 MAY 93 19 MAY 93Silver ND mg/kg 1.0 6010 05 MAY 93 17 MAY 93

PERCENT MOISTURE RESULTS ARE NOT AVAILABLE FOR THIS SAMPLE

ND - Not detectedNA - Not applicableReported By: Steven Gouy Approved By: Debra Hosford

• '. —————————— EnsecoHO* 3 I S A Cumini: Companv

Total MetalsClient Name: Barr Engineering CompanyClient ID: RIRCH extract/1eachateLab ID: 028873-0007-SAMatrix: LEACHATE Sampled: 15 APR 93 Received: 22 APR 93Authorized: 22 APR 93 Prepared: See Below Analyzed: See Below

. Wet.wt. Reporting Analytical Prepared AnalyzedParameter Result Units Limit Method Date DateLead 2990 mg/kg 5.0 6010 05 MAY 93 17 MAY 93

ND - Not detectedNA • Not applicableReported By: Steven Gouy Approved By: Debra Hosford

-————— EnsecoS A Commc Compjiu

Total Hetals

Client Name: Barr Engineering CompanyClient ID: R1PSH extract/1eachateLab ID: 028873-0008-SAMatrix: LEACHATE Sampled: 16 APR 93 Received: 22 APR 93Authorized: 22 APR 93 Prepared: See Below Analyzed: See Below

. Wet wt. Reporting Analytical Prepared AnalyzedParameter Result Units Limit Method Date DateLead 6960 mg/kg 5.0 6010 05 MAY 93 17 MAY 93

ND - Not detectedNA • Not applicableReported By: Steven Gouy Approved By: Debra Hosford

• "—-——— |— nc voToxicity Characteristic Metals Acon>,npComPJTCLP Leachate

Client Name: Barr Engineering CompanyClient ID: R1PFHLab ID: 028873-0002-SA Sampled: 15 APR 93 Leached: 30 APR 93Matrix: SOLID Received: 22 APR 93 Prepared: See Below

Authorized: 22 APR 93 Analyzed: See BelowReporting Analytical Prepared Analyzed

Parameter Result Units Limit Method Date DateLead 1.9 mg/L 0.50 6010 12 MAY 93 13 MAY 93


• " ~ " — ~ — — -—~™ r " no (T"Toxiclty Characteristic Metals AcommRa,mr,n,TCLP Leachate

Client Name: Barr Engineering CompanyClient ID: R1PSHLab ID: 028873-0003-SA Sampled: 16 APR 93 Leached: 20 MAY 93Matrix: SOLID Received: 22 APR 93 Prepared: See Below

Authorized: 22 APR 93 Analyzed: See BelowReport1ng Analyti cal Prepared Analyzed

Parameter Result Units Limit Method Date DateLead 8.9 mg/L O.SO 6010 20 MAY 93 20 MAY 93 z

Note z : Sample exhibits a characteristic of hazardous waste.ND - Not detectedNA - Not applicableReported By: Steven Gouy Approved By: Debra Hosford

"———————;————————— EnsecoToxicity Characteristic Metals *cUm,nBa™^TCLP Leachate

Client Name: Barr Engineering CompanyClient ID: R2PFHLab ID: 028873-0004-SA Sampled: 16 APR 93 Leached: 30 APR 93Matrix: SOLID Received: 22 APR 93 Prepared: See Below

Authorized: 22 APR 93 Analyzed: See BelowReporting Analytical Prepared Analyzed

Parameter Result Units Limit Method Date DateLead 1.8 mg/L 0.50 6010 12 MAY 93 13 MAY 93



ParameterTotal Solids

Barr EngineeringR1RCH028873-0001 -SASOLID22 APR 93

Result

62.3

General Inorganics

Company

Sampled: 15 APR 93 ReceivedPrepared: See Below Analyzed

Reporti ng Analyti calUnits Limit Method% 0.1 160.3 Mod.

. hriseccA Cumin); Corr

: 22 APR 93: See BelowPrepared AnalyzedDate Date

NA 01 MAY 9;

ND * Not detectedNA - Not applicableReported By: Adam Alban Approved By: Debra Hosford

General InorganicsEnsecoA CominK Compam


ParameterBulk DensityIgnitabilitypflTotal Solids

Barr Engineering CompanyR1PFH028873-0002-SASOLID Sampled: 15 APR 9322 APR 93 Prepared: See Below

Received: 22 APR 93Analyzed: See Below

Result UnitsReporting Analytical

Limit MethodPrepared AnalyzedDate Date

0.8005 g/cc113 deg. F8.0 units4.4 % 0.1

ASTM D7010109045/ASTM160.3 Mod,

NANANANA

03 MAY 9321 MAY 9329 APR 9301 MAY 93

Note z : Sample exhibits a characteristic of hazardous waste.ND - Not detectedNA - Not applicableReported By: Adam Alban Approved By: Debra Hosford

General Inorganics EnsecoA Coming: Company


ParameterBulk DensityIgnitabilitypflTotal Solids

Barr Engineering CompanyR1PSH028873-0003-SASOLID Sampled: 16 APR 9322 APR 93 Prepared: See Below


Result UnitsReporting AnalyticalLimit Method


1.2723 g/cc>160 Sea. F11.0 units89.6 X 0.1

ASTM D7010109045/ASTM160.3 Mod,

NANANANA

03 MAY 9321 MAY 93 o29 APR 9301 MAY 93

Note o : This test is unreliable for any sample other than anon-aqueous liquid.

ND * Not detectedNA - Not applicableReported By: Adam Alban Approved By: Debra Hosford

General InorganicsEnsecoA Cuminp Cumpjnv


ParameterBulk DensityIgnitabilitypfiTotal Solids

Barr Engineering CompanyR2PFH028873-0004-SASOLID Sampled: 16 APR 9322 APR 93 Prepared: See Below


Result UnitsReporting Analytical

Limit MethodPrepared AnalyzedDate Date

0.7995 g/cc95 deg. F8.0 units4.1 % 0.1

ASTM 07010109045/ASTM160.3 Mod.

NANANANA

03 MAY 9321 MAY 93 z29 APR 9301 MAY 93

Note z : Sample exhibits a characteristic of hazardous waste.ND * Not detectedNA * Not applicableReported By: Adam Alban Approved By: Debra Hosford

:—————————————————— EnsecoA Coming Companv

IV. QUALITY CONTROL REPORT

The Enseco laboratories operate under a vigorous QA/QC program designed toensure the generation of scientifically valid, legally defensible data bymonitoring every aspect of laboratory operations. Routine QA/QC proceduresinclude the use of approved methodologies, independent verification ofanalytical standards, use of duplicate Laboratory Control Samples to assessthe precision and accuracy of the methodology on a routine basis, and arigorous system of data review.







———————————————:—————————————————— EnsecoA Coming Compa

Control limits for accuracy (percent recovery) are based on the average,historical percent recovery +/- 3 standard deviation units. Control limitsfor precision (relative percent difference) range from 0 (identical duplicateDCS results) to the average, historical relative percent difference + 3standard deviation units. These control limits are fairly narrow based on theconsistency of the matrix being monitored and are updated on a quarterlybasis.

For each batch of samples analyzed, an additional control measure is takenin the form of a Single Control Sample (SCS). The SCS consists of a controlmatrix that is spiked with surrogate compounds appropriate to the method beingused. In cases where no surrogate is available, (e.g., metals or conventionalanalyses) a single DCS serves as the control sample. An SCS is prepared foreach sample lot for which the DCS pair are not analyzed. The recovery of theSCS is charted in exactly the same manner as described for the DCS, andprovides a daily check on the performance of the method.


Measured Concentration% Recovery - ———————————————— X 100

Actual ConcentrationPrecision for DCS is measured by Relative Percent Difference (RPD).

I Measured Concentration DCS1 * Measured Concentration DCS2 IRPD « —————————————————————————————————————————— X 100

(Measured Concentration DCS1 + Measured Concentration DCS2J/2


QC LOT ASSIGNMENT REPORTOrganics by Chromatography

EnsecoA Citrnmp Companv

LaboratorySample Number028873-0001-SA028873-0002-SA028873-0003-SA028873-0004-SA

QC Matrix

WASTEWASJEWASTEWASTE

QC Category

TCO-WTCO-WTCO-WTCO-W

QC Lot Number(DCS)28 APR 93-1A28 APR 93-1A28 APR 93-1A28 APR 93-1A


28 APR 93-1A28 APR 93-1A28 APR 93-1A28 APR 93-1A

DUPLICATE CONTROL SAMPLE REPORTOrganics by Chromatography

EnsecoA Coming Compinv

AnalyteConcentration Accuracy Precision

Spi ked Measured Average(%) (RPD)DCS1 DCS2 AVG DCS Limits DCS Limit

Category: TCO-WMatrix: WASTEQC Lot: 28 APR 93-1AConcentration Units: mg/kgTotal ChromatographableOrganics 50.0 35.8 33.2 34.5 69 33-144 7.5 33


~~—— _ EnsecoA Commfi Compjm

SINGLE CONTROL SAMPLE REPORTOrganics by Chromatography

Concentration Accuracy(%)Analyte Spiked Measured SCS Limits

Category: TCO-WMatrix: WASTEQC Lot: 28 APR 93-1A QC Run: 28 APft 93-1AConcentration Units: mg/kgo-Terphenyl 2.00 K90 95 54-141

Calculations are performed before roundlng to avoid round-off errors in calculated results

METHOD BLANK REPORTOrganics by Chromatography

EnsecoA Coming Ci'mpa


Units Limit

Test: TCO-FID-WMatrix: SOLIDQC Lot: 28 APR 93-1A QC Run:

Total Chromatographabl eOrganics

28 APR 93-1A

ND mg/kg 10

Test: TCO-FID-WMatrix: SOLIDQC Lot: 28 APR 93-1A QC Run: 28 APR 93-1A

Total ChromatographableOrganics ND mg/kg 10

Test: TCO-FID-WMatrix: SOLIDQC Lot: 28 APR 93-1A QC Run: 28 APR 93-1A


EnsecoA Commp Compjnv

QC LOT ASSIGNMENT REPORTSemivolatile Organics by GC


028873-0001-SA SOIL PCB-S 06 APR 93-1A 29 APR 93-1A028873-0002-SA SOIL PCB-S 06 APR 93-1A 29 APR 93-1A028873-0003-SA SOIL PCB-S 06 APR 93-1A 29 APR 93-1A028873-0004-SA SOIL PCB-S 06 APR 93-1A 29 APR 93-1A

EnsecoA Commc Ci'mpa

DUPLICATE CONTROL SAMPLE REPORTSemivolatile Organics by GC

Concentration FusionSPlked CS2 AVG DCS Limits DCS LimitAnalyte DCS1 DCS2

Category: PCB-S

QC Lot': 06 APR 93-1AConcentration Units: ug/kg

167 121 115 H8 71 49-130 5.1 20Aroclor 1254 lb/


•——— EnsecoA CommR Companv

SINGLE CONTROL SAMPLE REPORTSemivolatile Organics by GC


Category: PCB-SMatrix: SOILQC Lot: 06 APR 93-1A QC Run: 29 APR 93-1AConcentration Units: ug/kg

Aroclor 1254 167 106 63 49-130


EnsecoMETHOD BLANK REPORTSemivolatile Organics by GC

* -i 4. ReportingAnalyte Result Units Limit

Test: 8080-PCB-SMatrix: SOLIDQC Lot: 06 APR 93-1A QC Run: 29 APR 93-1A

Aroclor 1016 ND uq/kg 33Aroclor 1221 NO ug/kg 33Aroclor 1232 NO ug/kg 33Aroclor 1242 ND ug/kg 33Aroclor 1248 ND ug/kg 33Aroclor 1254 ND ug/kg 33Aroclor 1260 NO ug/kg 33


Aroclor 1016 ND ug/kg 33Aroclor 1221 ND ug/kg 33Aroclor 1232 ND ug/kg 33Aroclor 1242 ND ug/kg 33Aroclor 1248 ND ug/kg 33Aroclor 1254 ND ug/kg 33Aroclor 1260 NO ug/kg 33


Aroclor 1016 NO ug/kg 33Aroclor 1221 ND ug/kg 33Arocl°r 33Aroclor 1242 NO ug/kg 33Aroclor 1248 ND ug/kg 33Aroclor 254 ND ug/kg 33Aroclor 1260 ND ug/kg 33

EnsecoA Coming Company


LaboratorySample Number028873-028873-028873-028873-028873-028873028873028873028873028873028873028873028873-028873-028873-028873-028873-028873-028873-028873-028873-028873028873028873028873028873028873028873028873

0001-SA0001-SA0001-SA0001-SA0002-SA-0002-SA-0002-SA-0002-SA-0002-SA-0003-SA-0003-SA-0003-SA-0003-SA-0003-SA-0004-SA-0004-SA-0004-SA0004-SA0004-SA0005-SA-0005-SA. 0005-SA-0005-SA-0006-SA-0006-SA-0006-SA-0006-SA-0007-SA-0008-SA

QC MatrixSOILSOILSOIL •SOILSOILSOILSOILLEACHATESOILSOILSOILSOILLEACHATESOILSOILSOILSOILLEACHATESOILSOILSOILSOILSOILSOILSOILSOILSOILSOILSOIL

QC CategoryQC Lot Number(DCS)


ICP-SAS-FAA-SSE-FAA-SHG-CVAA-SICP-SAS-FAA-SSE-FAA-SICP-TLHG-CVAA-SICP-SAS-FAA-SSE-FAA-SICP-TLHG-CVAA-SICP-SAS-FAA-SSE-FAA-SICP-TLHG-CVAA-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-SICP-S

12 MAY 93-lA10 MAY 93-1810 MAY 93-1806 MAY 93-1812 MAY 93-lA10 MAY 93-1810 MAY 93-1812 MAY 93-lA06 MAY 93-1819 MAY 93-lA19 MAY 93-lA19 MAY 93-lA20 MAY 93-lA24 MAY 93-lA12 MAY 93-lA10 MAY 93-1810 MAY 93-1812 MAY 93-lA06 MAY 93-1804 MAY 93-1C06 MAY 93-1818 MAY 93-lA18 MAY 93-lA04 MAY 93- 1C12 MAY 93-lD18 MAY 93-lA18 MAY 93-lA04 MAY 93-1C04 MAY 93-1C

12 MAY 93-lA10 MAY 93-1810 MAY 93-1806 MAY 93-1812 MAY 93-lA10 MAY 93-1810 MAY 93-1812 MAY 93-lA06 MAY 93-1819 MAY 93-lA19 MAY 93-lA19 MAY 93-lA20 MAY 93-lA24 MAY 93-lA12 MAY 93-lA10 MAY 93-1810 MAY 93-1812 MAY 93-lA06 MAY 93-1804 MAY 93-1C06 MAY 93-1818 MAY 93-lA18 MAY 93-lA04 MAY 93-1C12 MAY 93-lD18 MAY 93-lA18 MAY 93-lA04 MAY 93-1C04 MAY 93 -1C

EnsecoA Cu



Solked5P DCS1Measured

DCS2 AVG

Accuracy PrecisionAverage**) (RPD)DCS Limits DCS Limit

Category: ICP-SMatrix: SOILQC Lot: 12 MAY 93-1AConcentration Units: mg/kg

AluminumAntimonyArsenicBariumBeryl 1i urnCadmiumCalciumChromiumCobaltCopperIronLeadMagnesiumManganeseMolybdenumNickelPotassiumSilverSodiumVanadiumZinc

1070055.21455031291547390151122162

1540014837404231591664050104747154530

1100056.31685231681628280170138194

16800145

41204771912044540108310177544

1090059.11745271661638280171137190

1670014440704761912034200109281175548

1090057.71715251671638280171137192

16700144

41004761912044370108296176546

10210511810412910611211311311910997no11312012310810440114103

47-15318-36259-14176-12453-13168-13279-12166-13370-13070-13266-13466-13574-12674-12571-12967-13368-13276-12457-13073-12765-135

0.84.83.60.81.10.50.00.60.32.50.60.31.20.20.30.47.80.89.60.80.7

205020202020202020202020202020202020202020

Category: AS-FAA-S»«_j.—2.. . CftTI

no/*Concentration Units: mg/kg

Arsenic 145 144 132 138 96 59-141 8.7

Category: SE-FAA-SMatrix: SOILQC Lot: 10 MAY 93-1BConcentration Units: mg/kg

Selenium

Calculations are performed before

143 130 114 122 86 68-132 13 20

rounding to avoid round-off errors 1n calculated results.

DUPLICATE CONTROL SAMPLE REPORTMetals Analysis and Preparation (cont.Metals Analysi


Spiked MeasuredOCS1 DCS2

EnsecoA Cumins Company

Accuracy PrecisionAverage(%) (RPD

AVG DCS Limits DCS Limit

Category: HG-CVAA-S

8*13;Concentration Units:

Mercury

mg/kg29.0 33.7 35.0 34.4 118 52-148 3.8 20

Category: ICP-TLMatrix: LEACHATEQC Lot: 12 MAY 93- 1AConcentration Units: mg/L

Al umi numAntimonyArsenicBariumBeryl 1 1 urnCadmiumChromiumCobaltCopperIronLeadManganeseNickelSilverVanadiumZinc

20.05.005.0020.00.5000.5002.005.002.5010.05.005.005.000.3205.005.00

18.04.344.3517.10.4740.4821.734.322.198.684.374.594.470.3364.714.57

18.14.424.2417.00.4730.4961.694.352.198.664.314.564.490.3454.724.56

18.04.384.2917.10.4730.4891.714.332.198.674.344.584.480.3414.724.57

908886859598868788878792901069491

75-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-125

0.51.82.60.40.22.82.00.80.20.31.40.50.52.80.30.2

20202020202020202020202020202020

Cateory: ICP-S

Concentration Units: mg/kg

AluminumAntimonyArsenicBariumBerylliumCadmiumCalciumChromi urnCobalt

1070055.21455031291547390151122

1100068.11595471511718430169138

1080065.51565341461718220164134

1090066.81585401481718330167136

102121109107115111113110112

47-15318-36259-14176-12453-13168-13279-12166-13370-130

1.53.81.92.43.60.42.52.72.7

205020202020202020

°mrs

DUPLICATE CONTROL SAMPLE REPORTMetals Analysis and Preparation (cont.Metals Analysi


Spiked MeasuredDCS1 DCS2

EnsecoA Civnini; Ci>mpjm

Accuracy PrecisionAverage(%) (RPD)


Category: ICP-S


CopperIronLeadMagnesiumManganeseMolybdenumNickelPotassiumSilverSodiumVanadiumZinc

Category: AS-FAA-SKt= 8*Y93-1AConcentration Units: mg/kg

Arsenic

Category: SE-FAA-S93-1A


Selenium

Category: ICP-TLMatrix/ LEACHATEQC Lot: 20 MAY 93- 1AConcentration Units: mg/L

AluminumAntimonyArsenicBariumBeryl 1 i urn

1621540014837404231591664050104747154530

1901740016842904741801914050121926170601

188170001624240462175186

4010120815167592

1891720016542604681781894030120871169597

117112111114111112114100116117109113

70-13266-13466-13574-12674-12571-12967-13368-13276-12457-13073-12765-135

1.22.53.71.42.52.82.90.90.6132.01.5

202020202020202020202020

145

143

162 162 162 111 59-141 0.0

132 135 133 93 68-132 2.1 20

20.05.005.0020.00.500

19.04.644.3618.60.362

18.74.674.5918.50.368

18.84.664.4718.60.365

9493899373

75-12575-12575-12575-12575-125

1.60.65.10.31.6


DUPLICATE CONTROL SAMPLE REPORTMetals Analysis and Preparation (cont.


Spiked MeasuredOCS1 DCS2

EnsecoA Coming Companv

Accuracy PrecisionAveraae(i) (RPO


Category: ICP-TLMatrix: LEACHATEQC Lot: 20 MAY 93-1AConcentration Units: mg/L

Cadmi urnChromiumCobaltCopperIronLeadManganeseNickelSilverVanadiumZinc

Category: HG-CVAA-S


Mercury

0.5002.005.002.5010.05.005.005.000.5005.005.00

0.9382.064.672.5410.15.294.674.64

0.4114.945.36

0.7871.934.542.4910.04.974.604.620.4554.895.27

0.8632.004.602.5110.15.134.634.630.4334.915.31

1731009210110110393938798106

75-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-125

186.72.72.10.86.21.40.4101.11.7

2020202020202020202020

29.0 34.4 34.7 34.5 119 52-148 1.0

Category: ICP-SK" 0 93-10Concentration Units: mg/kgAluminumAntimonyArsenicBariumBeryl 1 1 urnCadmiumCalciumChromiumCobaltCopperIronLeadMagnesiumManganese

C,H,U,,onS „

1070055.21455031291547390151122162

154001483740423

681035.01384461311376640126112158

113001273250375

688033.51304541311416780128114158

114001293300381

685034.2134450131139

6710127113158

113001283280378

64629389102909184929874878889

47-15318-36259-14176-12453-13168-13279-12166-13370-13070-13266-13466-13574-12674-125

1.04.36.11.70.42.72.11.81.70.21.02.11.51.5

Ift. " """""" "'""

DUPLICATE CONTROL SAMPLE RETORTMetals Analysis and Preparation (cont.)


DCS1

EnsecoA C timing Comparu

Accuracy PrecisionAveraaeW (RPp


Category: ICP-SMatrix: SOILQC Lot: 04 MAY 93-1CConcentration Units: mg/kgMolybdenumNickelPotassiumSilverSodiumVanadiumZinc

1591664050104747154530

144154327094.4860137445

146156323096.6890139454

145155325095.5875138450

919380921179085

71-12967-13368-13276-12457-13073-12765-135

1.21.11.12.33.51.22.0

20202020202020

Category: AS-FAA-SMatrix: SOILQC Lot: 18 MAY 93-1AConcentration Units: mg/kg

Arsenic 145 142 124 133 92 59-141 14 20

Category: SE-FAA-SMatrix: SOILQC Lot: 18 MAY 93-1AConcentration Units: mg/kgSelenium 143 142 131 136 95 68-132 8.1 20

Category: HG-CVAA-S93-10 /hConcentration Units: mg/kg

Mercury 29.0 33.2 32.5 32.8 113 52-148 2.1 20



Analyte

Test: ICP-RCRA-S;: SOLID.: 12 MAY 93-1A QC Run: 12 MAY 93-1A


Test: AS-FAA-S! 10LMAY 93-1B QC Run: 10 MAY 93-1B

Arsenic

Test: SE-FAA-Si 10LMAY 93-1B QC Run: 10 MAY 93-1B

Selenium

Test: HG-CVAA-S! SNBv 93-1B QC Run: 06 MAY 93-1B

Mercury

Test: ICP:RCRA-S93-1A QC Run: 12 MAY 93-1A

BariumCadmi urnChromiumLeadSilver

lesult

•1A

NDNDNDNDND

-IB

ND

[-IB

ND

MB

ND

3-1A

NDNDNDNDND

Units


mg/kg

mg/kg

mg/kg


„ ____ __ ———— _ —————— I— T~*CO/"V~\————— cnbtxoA Cominp Company

ReportingLimit

1.00.501.05.01.0

0.50

0.50

0.10

1.00.501.05.01.0

- EnsecoA Cominc Comp-im



Units Limit

Test: AS-FAA-SMatrix: SOLIDQC Lot: 10 MAY 93-1B QC Run: 10 MAY 93-1B

Arsenic NO mg/kg 0.50

Test: SE-FAA-S! WWY 93-18 QC Run: 10 MAY 93-1B


Test: ICP-OTC-TCLP-LMatrix: SOLIDQC Lot: 12 MAY 93-1A QC Run: 12 MAY 93-1A

Lead ND mg/L 0.50

Test: HG-CVAA-S93-1B QC Run: 06 MAY 93-1B


Test: ICP-RCRA-S! 19LMAY 93-1A QC Run: 19 MAY 93-1A


NDNDNDNDND


1.00.501.05.01.0

Enseco



Units Limit

Test: AS-FAA-Si 19LMAY 93-1A QC Run: 19 MAY 93-1A


Test: SE-FAA-S! 19 MAY 93-1A QC Run: 19 MAY 93-1A

Selenium ND 0.50

Test: ICP-OTC-TCLP-Lt! 20LMAY93-1A QC Run: 20 MAY 93-1 A

Lead ND mg/L 0.50

Test: HG-CVAA-Sl 24LMAY 93-1A QC Run: 24 MAY 93-1A


Test: ICP-RCRA-S93-1C QC Run: 04 MAY 93-1C

BariumCadmi urnChromiumLeadSilver

NDNDNDNDND


1.00.501.05.01.0

EnsecoA Comini;



Units Limit

Test: HG-CVAA-SMatrix: SOLIDQC Lot: 06 MAY 93-1B QC Run: 06 MAY 93-18

Mercury

Test: AS-FAA-SMatrix: SOLIDQC Lot: 18 MAY 93-1A QC Run: 18 MAY 93-1A

Arsenic

ND mg/kg 0.10

ND mg/kg 0.50

Test: SE-FAA-SQC^ot! 18LMAY 93-1A QC Run: 18 MAY 93-1A


Test: HG-CVAA-S! 12LMAY 93-1D QC Run: 12 MAY 93-1D


Test: ICP-WMatrix: LEACHATEQC Lot: 04 MAY 93-1C QC Run: 04 MAY 93-1C

LeadND mg/kg 5.0


EnsecoA Ci'tninj; C"ompjn\

LaboratorySample Number028873-0002-SA028873-0003-SA028873-0004-SA

QC MatrixAQUEOUSAQUEOUSAQUEOUS

QC CategoryPH-APH-APH-A

QC Lot Number(DCS)

29 APR 93-1A29 APR 93-1A29 APR 93-1A


EnsecoDUPLICATE CONTROL SAMPLE REPORTWet Chemistry Analysis and Preparation


Spiked Measured Average(%) (RPD)DCS1 DCS2 AVG DCS Limits DCS Limit

Category: PH-AMatrix: AQUEOUSQC Lot: 29 APR 93-1AConcentration Units: unitsPH 9.10 9.09 9.13 9.11 100 98-102 0.4

Calculations are performed before founding to avoid round-off errors in calculated results.

iZtfllf* Chain °f Custody *- -BynemgCDOfay8300 Norman Center DriveMinneapolis, MN 55437-1026(612) 832-2600

Project Numberz.^/.c.n, .o.t.-s^ N9 " " 0 8 0 6

SampleIdentification

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Laboratory:. €»OSt(0: fcVAM-^^£MVMJ

Remarks/Analysis Required:

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Received by Lab: Dale Time

-Received by LA . Dale Time

^v^Ôi ^f^^^^^C,// yfefa S/<KAir^bilft Number: ^ 7

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Distribution: While-Original Accompanies Shipment to Lab; Yellow - Lab Coordinalon Pink-Field Copy

CHAIN OF CUSTODYBARR ENGINEERING CO.7803 QLENROY ROADMINNEAPOLIS, MN 65439

PROJECT NUMBER N? 01791<2l3l/l<«l^ | • \&\<* )5 IffltJFtll&l 5 |2.NO:

SAMPLEIDENTIFICATION

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SAMPLES SHIPPED VIAO AIR FREIQHTDFED, EXP.DSAMPLEflD OTHER- ——————————————————

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PROJECT MANAGER:

PROJECT CONTACT:

LABORATORY:

REMARKS/ANALYSIS REQUIRED:

MM^ T rr Y^n?feAUk.~A S^ufc. *n-va^,

•

RECEIVED BY LAB: OATE TIME

RECEIVED BY LAB; DATE TIME

4 /iS^? " ^? fWRECCIVEkB^ LAB: DATE TIME

AIR BILL NUMBER:

; WHITE-ORIGINAL ACCOMPANIES SHIPMENT ?o LAB. RETURNS TO BAnn WITH RESULTS: YELLOW-LAB COPY; PINK-LAB COORDINATOR; GOLD-FIELD COPY

CUSTOMER #:01571

HUFFMANLABORATORIES, INCQualify Analytical Services Since 1936

4630 Indiana Street • Golden, CO 80403Phone: (303) 278-4455 • FAX: (303) 278-7012

FILE COPYDATE 4/30/93LAB# 161693P.O.RECD 04/21/93

ANALYSIS REPORT

R. PAUL TAYLORBARR ENGINEERING COMPANY8300 NORMAN CENTER DRIVEMINNEAPOLIS, MN 55437

PROJ. # 23/69-065DFS52

ti'C.

ttff 0 3

SEQUENCE/SAMPLE ID

SULFUR-CHLORINE-

BTU/LB

T •?-..; . -N-!'

01\R1RCH",

- 0.18 - -- 2.69 - -- <0.10 - -— 1 1 1 *> — —-LX . J--Jami _ _ — -

; r •? '•'. • ^x.02

R1PSBE;

0 *\ A.24 -•j • -/ j.

- - - <0.10 -A f *\ A- - - 46.34 -

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17,-t^?, - -^T

03^RIPFH

- - - - 0.05 - -- - - - 0.01 - -- - - - <0.10 - -- - _ _ 0 32 — -w • -J ft

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R2PFH

- - - 0.06- - - 0.02- - - <0.10_ — — ft 07

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- - 1 T71 R

THE SAMPLES ARE NOT HOMOGENEOUS.A COMBUSTION ADDITIVE WAS USED ON BTU/LB ANALYSIS FOR SAMPLES R1RCH AND R1PSH,BTU/LB RESULTS ARE THE GROSS HEATING VALUES (AND HAVE BEEN CORRECTED FORSULFUR CONTENT ACCORDING TO ASTM D2015).

Rocky Mounta inAnalytical Laboratory

ANALYTICAL RESULTS

FOR .

BARR ENGINEERING


JUNE 16, 1993

A CORNING Company

Reviewed by:

Enseco Incorporated4955 Yarrow StreetArvada, Colorado 80002303/421-6611 Fax; 303/431-7171

————————————————————————————~———— EnsecoA CuminR Compjnv

Introduction

This report presents the analytical results as well as supportinginformation to aid in the evaluation and interpretation of the data and isarranged in the following order:

o Sample Description Informationo Analytical Test Requestso Analytical Resultso Quality Control Report

The bulk density analysis was performed by Hauser Chemical Research,Incorporated located in Boulder, Colorado,

All analyses at Enseco are performed so that the maximum concentration ofsample consistent with the method is analyzed. Dilutions are at timesrequired to avoid saturation of the detector, to achieve linearity for aspecific target compound, or to reduce matrix interferences. In this event,reporting limits are adjusted proportionately. Surrogate compounds may not bemeasurable in samples which have been diluted.

The sample identification present on the chain of custody is incorrect.As directed by Paul Taylor of Barr Engineering on May 21, 1993, Enseco-RMALreport 029365 was changed to reflect the correct sample identification.

Sample 029365-0001 required a dilution for the GC 8080 PCB analysis due tothe concentration of target compounds present in the sample. The reportinglimits are adjusted accordingly. Aroclor 1242 was reported since the patternmatch was slightly better than that of Aroclor 1016. The concentration ofAroclor 1242 may be slightly biased high due to the presence of Aroclor 1260.The holding time was missed due to the length of time between samplearrival/collection and initial request.

Sample 029365-0001 could not be concentrated below a final volume of 10 mlfor the Extractable Petroleum Hydrocarbon GC/FID analysis due to the oilysample matrix. In addition, the sample required an analytical dilution due to

EnsecoA Csnnine Compjm

the concentration of target compounds present in the sample. The reportinglimits are adjusted accordingly. Surrogates were not reportable due to thenecessary dilution. The holding time for this analysis was also missed due tothe length of time between sample arrival/collection and request for theanalysis.

RMAL samples 028892-0002-through -0003 did not physically exist on receiptat the laboratory. A portion of sample (-0001) was extracted with methylenechloride to generate leached solids (-0002) and a solvent leachate (-0003).

Samples -0001 and -0002 required dilutions for the ICP metals analysis dueto the concentration of lead present in the samples. Sample -0001 alsorequired a dilution for the TCLP lead analysis due to the concentration oflead in the leachate. Lead was reported at 5.0 mg/L. The regulatory level is5.0 mg/L. Reporting limits are adjusted relative to the dilutions. Chromiumwas present in the laboratory ICP preparation blank (lot 07 JUN 93-1C) at 1.0nig/kg. Chromium was reported in samples -0001 and -0002 at 48.2 mg/kg and48.1 mg/kg respectively. Samples -0001 and -0002 required dilutions for thearsenic and selenium analysis due to matrix interference. These two sampleswere also diluted for the mercury analysis due to concentrations of mercurypresent in the samples beyond the linear range of the instrument. The holdingtimes for the mercury analysis were missed. The holding time expired for thisanalysis due to the length of time between sampling/receipt and the initialrequest.


The following procedure was followed to prepare extracted samples metalsanalysis for project 029365. The samples were homogenized and a 20 gramaliquot was placed in a glass centrifuge tube. The sample was then mixed with20 grams of methylene chloride and extracted (shaken vigorously on MOOTshaker) for 30 minutes, then centrifuged for 30 minutes. The methylenechloride extract was decanted into a separate bottle while the remaining solidportion was dried at 103°C for 30 minutes. This drying step was used toremove residual solvent, and should have also removed most of the water

EnsecoA Coming Compj

remaining in the sample. Sample weights are recorded in the datadeliverables. The methylene chloride extract, remaining solid portion and thetotal sample was prepared and analyzed using RMAL SOPs based on SW846 Methods3050, 6010, and the 7000 series for Hg, As, and Se.

For the total sample (-0001) results are reported on a dry weight basis.Since the leached solids were dried for 30 minutes, the leached/extractedsolids (-0002) were reported as weighed out--in dry weight units but with nocorrection for percent moisture. Results for the solvent extracts were alsoreported as weighed out--in wet weight units with no moisture correction. Thesample portion weighed included the solvent decanted plus any material whichdissolved in the solvent.

For summary purposes, the lead results were converted to total lead in thesample aliquot (see table below). A nominal 20 g aliquot was used for thesolvent extractions, so total results for the original sample (-0001) arebased on the dry weight portion of a 20 g aliquot. The recorded weights forthe dried leached solids and leachatc were used to calculate the total lead inthe separate portions.


Aliquot Lead029265 mq/kq Weight, q mq

-0001-SA 20400 15.09 308Total Sample

-0002-SA 25600 15.98 408Leached Solid

-0003-SA 3610 11.55 41.7Leachate

A Curnint;———————————————— Enseco


The Sample Description Information lists all of the samples received inthis project together with the internal laboratory identification numberassigned for each sample. Each project received at Enseco-RMAL is assigned aunique six digit number. Samples within the project are numberedsequentially. The laboratory identification number is a combination of thesix digit project code and the sample sequence number.



The Analytical Test Requests lists the analyses that were performed oneach sample. The Custom Test column indicates where tests have been modifiedto conform to the specific requirements of this project.



EnsecoA Cuminc Compjm

Lab ID

029365-0001-SA029365-0002-SA029365-0003-SA

Client IDR2PCR2PC EXTRACTED SOLIDR2PC EXTRACT/LEACHATE

Sampled ReceivedMatrix Date Time DateSOLID 21 APR 93 15:00 18 MAY 93SOLID 21 APR 93 15:00 18 MAY 93LEACHATE 21 APR 93 15:00 18 MAY 93

EnsecoA Cummi; Ci'mp.im

ANALYTICAL TEST REQUESTSfor



0001 A RCRA Total Metals done by ICP NPrep - Total Metals, ICP NArsenic, Furnace AA NPrep - Total Metals, Furnace AA NSelenium, Furnace AA NExtractable Petroleum Hydrocarbons NPrep - Hydrocarbons by GC NPCBs NPrep - PCBs by GC NPercent Water NToxicity Characteristic Metals YDigestion for Metals from a TCLP leachate NTCLP Extraction / Metals Aliquot NIgnitability, Closed Cup NBulk Density NpH NMercury, Cold Vapor AA NPrep - Mercury, Cold Vapor AA NTotal Solids (TS) N

0002 B RCRA Total Metals done by ICP NPrep - Total Metals, ICP NMercury, Cold Vapor AA NPrep - Mercury, Cold Vapor AA NArsenic, Furnace AA NPrep - Total Metals, Furnace AA NSelenium, Furnace AA N

0003 C ICP Suite YPrep - Total Metals, ICP N

EnsecoA Cumins Cumpijm

Analytical Results

The analytical results for this project are presented in the followingdata tables. Each data table includes sample identification information, andwhen available and appropriate, dates sampled, received, authorized, preparedand analyzed. The authorization data is the date when the project was definedby the client such that laboratory work could begin.

Data sheets contain a listing of the parameters measured in each test, theanalytical results and the Enseco reporting limit. Reporting limits areadjusted to reflect dilution of the sample, when appropriate. Solid and wastesamples are reported on an "as received" basis, i.e. no correction is made formoisture content.

The results from the Standard Enseco QA/QC Program, which generates datawhich are independent of matrix effects, are provided subsequently.


ParameterAroclor 1016Aroclor 1221Aroclor 1232Aroclor 1242Aroclor 1248Aroclor 1254Aroclor 1260

PCBs

Method 8080Barr Engineering CompanyR2PC029365-0001-SASOLID Sampled: 21 APR 9321 MAY 93 Prepared: 25 MAY 93

EnsecoA Coming (_t>mpjm

Received: 18 MAY 93Analyzed: 08 JUN 93

Result

NDNDND650NDND400

Dry Weight ReportingUnits Limitug/kgug/kgugAgug/kgugAgug/kg

200200200200200200200

Percent Moisture is 1.7%. All results and limits are reported on a dry weight basis.ND - Not detectedNA - Not applicableReported By: Stan Dunlavy Approved By: Denise Howe

——————————————————————-——————————————____________________ pExtractable Petroleum Hydrocarbons

Method GC/FID

Client Name: Barr Engineering CompanyClient ID: R2PCLab ID: 029365-0001-SAMatrix: SOLID Sampled: 21 APR 93 Received: 18 MAY 93Authorized: 21 MAY 93 Prepared: 25 MAY 93 Analyzed: 03 OUN 93

Dry Weight ReportingParameter - - Result Units LimitTotal Chromatographable


Surrogate Recovery

o-Terphenyl ND %

Note 1 : QUALITATIVE ID: This sample has GC/FID characteristics thatare similar to motor oil.Sample resembles a hydrocarbon product occurring within then-alkane range C18-C36.

Percent Moisture is 1.7%. All results and limits are reported on a dry weight basis.ND = Not detectedNA - Not applicable


—————— EnsecoToxicity Characteristic Metals *cumm*C^F™

TCLP Leachate

Client Name: Barr Engineering CompanyClient ID: R2PCLab ID: 029365-0001-SA Sampled: 21 APR 93 Leached: 03 JUN 93Matrix: SOLID Received: 18 MAY 93 Prepared: See Below

Authorized: 21 MAY 93 Analyzed: See Below

Reporting Analytical Prepared AnalyzedParameter Result "Units- Limit Method Date DateLead 5.0 mg/L 0.50 6010 07 JUN 93 09 JUN 93 z

Note z : Sample exhibits a characteristic of hazardous waste.


——————————————————————————•——————— EnsecoMetal S A Cumins Compjnv

Total Metals

Client Name: Barr Engineering CompanyClient ID: R2PCLab ID: 029365-0001-SAMatrix: SOLID Sampled: 21 APR 93 Received: 18 MAY 93Authorized: 21 MAY 93 Prepared: See Below Analyzed: See Below

Dry Weight Reporting Analytical Prepared AnalyzedParameter Result "Units' Limit Method Date Date

Arsenic 12.6 mg/kg 5.1 7060 09 JUN 93 10 JUN 93Barium 220 mg/kg 5.1 6010 07 JUN 93 08 JUN 93Cadmium 2.9 mg/kg 2.5 6010 07 JUN 93 08 JUN 93Chromium 48.2 mg/kg 5.1 6010 07 JUN 93 08 JUN 93 BLead 20400 mg/kg 25.4 6010 07 JUN 93 08 JUN 93Mercury 2.7 mg/kg 0.51 7471 04 JUN 93 07 JUN 93Selenium ND mg/kg 5.1 7740 09 JUN 93 09 JUN 93Silver ND mg/kg 5.1 6010 07 JUN 93 08 JUN 93

Percent Moisture is 1.7%. All results and limits are reported on a dry weight basis.Note B : Compound is also detected in the blank.ND * Not detectedNA - Not applicableReported By: Debra Hosford Approved By: Jeff Malecha

——————————————————————————————————— Enseco... -i A Cumini: C.mipJmMetals

Total Metals

Client Name: Barr Engineering CompanyClient ID: R2PC EXTRACTED SOLIDLab ID: 029365-0002-SAMatrix: SOLID Sampled: 21 APR 93 Received: 18 MAY 93Authorized: 21 MAY 93 Prepared: See Below Analyzed: See Below

Dry Wt. Reporting Analytical Prepared AnalyzedParameter Result "Units" Limit Method Date Date

Arsenic 14.9 mg/kg 5.0 7060 09 JUN 93 10 JUN 93Barium 555 mg/kg 5.0 6010 07 JUN 93 08 JUN 93Cadmium ND mg/kg 2.5 6010 07 JUN 93 08 JUN 93Chromium 48.1 mg/kg 5.0 6010 07 JUN 93 08 JUN 93 BLead 25600 mg/kg 25.0 6010 07 JUN 93 08 JUN 93Mercury 2.1 mg/kg 0.50 7471 11 JUN 93 11 JUN 93Selenium ND mg/kg 10.0 7740 09 JUN 93 09 JUN 93Silver ND mg/kg 5.0 6010 07 JUN 93 08 JUN 93

Note B : Compound is also detected in the blank.


•———————————————— EnsecoMetal s A Ci"Tiin>; c"mpj

Total Metals

Client Name: Barr Engineering CompanyClient ID: R2PC EXTRACT/LEACHATELab ID: 029365-0003-SAMatrix: LEACHATE Sampled: 21 APR 93 Received: 18 MAY 93Authorized: 21 MAY 93 Prepared: See Below Analyzed: See Below

Wet wt. Reporting Analytical Prepared AnalyzedParameter Result 'Units- Limit Method Date Date

Lead 3610 mg/kg 5.0 6010 07 OUN 93 08 JUN 93

ND = Not detectedNA - Not applicable


——————————————————— EnsecoGeneral Inorganics ACornmcCiim^m

Client Name: Barr Engineering CompanyClient ID: R2PCLab ID: 029365-0001-SAMatrix: SOLID Sampled: 21 APR 93 Received: 18 MAY 93Authorized: 21 MAY 93 Prepared: See Below Analyzed: See Below

Reporting Analytical Prepared AnalyzedParameter Result 'Units- Limit Method Date Date

Bulk Density 0.8286 g/cc -- ASTM D70 NA 03 JUN 93Ignitability >160 deg F -- 1010 NA 07 JUN 93 oTotal Solids 98.3 % 0.1 160.3 Mod. NA 25 MAY 93pH 10.4 units -- 9045/ASTM NA ^ 25 MAY 93

Note o : This test is unreliable for any sample other than anon-aqueous 1iquid.

ND = Not detectedNA - Not applicableReported By: Lavon Trujillo Approved By: Pam Rosas

EnsecoA Cumins Compjni

Quality Control Report

The Enseco laboratories operate under a vigorous QA/QC program designed toensure the generation of scientifically valid, legally defensible data bymonitoring every aspect of laboratory operations. Routine QA/QC proceduresinclude the use of approved methodologies, independent verification ofanalytical standards, use of Duplicate Control Samples to assess the precisionand accuracy of the methodology on a routine basis, and a rigorous system ofdata review.







EnsecoA Cuminc Cumpam

Control limits for accuracy (percent recovery) are based on the average,historical percent recovery +/- 3 standard deviation units. Control limitsfor precision (relative percent difference) range from 0 (identical duplicateDCS results) to the average, historical relative percent difference + 3standard deviation units. These control limits are fairly narrow based on theconsistency of the matrix being monitored and are updated on a quarterlyBasis.

For each batch of samples analyzed, an additional control measure is takenin the form of a Single Control Sample (SCS). The SCS consists of a controlmatrix that is spiked with either representative target compounds or surrogatecompounds appropriate to the method being used. An SCS is prepared for eachsample lot for which the DCS pair are not analyzed.


Measured Concentration% Recovery » —————————————————— X 100

Actual Concentration

Precision for DCS is measured by Relative Percent Difference (RPD).

| Measured Concentration DCS1 - Measured Concentration DCS2 IRPD - —————————————————————————————————————————— X 100

(Measured Concentration DCS1 + Measured Concentration DCS2)/2


EnsecoA Coming Ciimpjrn

QC LOT ASSIGNMENT REPORTSemivolatile Organics by GC

Laboratory QC Lot Number QC Run NumberSample Number QC Matrix QC Category (DCS) (SCS/BLANK)029365-0001-SA SOIL PCB-S 25 MAY 93-1A 25 MAY 93-1A

DUPLICATE CONTROL SAMPLE REPORTSemivolatile Organics by GC

EnsecoA Ci>mm>: Cumpj


Spiked Measured Average{%) (RPD)DCS1 DCS2 AVG DCS Limits' DCS Limit

Category: PCB-SMatrix: SOILQC Lot: 25 MAY 93-1AConcentration Units: ug/kg

Aroclor 1254 167 157 155 156 93 49-130 1.3 20


METHOD BLANK REPORTSemivolatile Organics by GC

EnsecoA Cumim; CiimfM

Analyte Result UnitsRe

Test: 8080-PCB-SMatrix: SOLIDQC Lot: 25 MAY 93-1A QC Run: 25 MAY 93-1AAroclorAroclorAroclorAroclorAroclorAroclorAroclor

1016122112321242124812541260

NONDNDNDNDNDND

ug/kgug/kgug/kgug/kg

ug/kg

33333333333333

Enseco

QC LOT ASSIGNMENT REPORTOrganics by Chromatography

i ahnratnrv QC Lot Number QC Run Numbersimple Number QC Matrix QC Category (DCS) (SCS/BLANK)029365-0001-SA WASTE TCO-W 25 MAY 93-1A 25 MAY 93-1A

DUPLICATE CONTROL SAMPLE REPORTOrganics by Chromatography

EnsecoA Gimme Compjru

AnalyteConcentrati on Accuracy Preci si on

Spiked Measured Average(%) (RPD)DCS1 DCS2 AVG DCS Limits DCS Limit

Category: TCO-W .Matrix: WASTEQC Lot: 25 MAY 93-1AConcentration Units: mg/kgTotal ChromatographableOrganics 50.0 38.0 35.9 37.0 74 33-144 5.7 33

Calculations are performed before roundlng to avoid round-off errors in calculated results.

———————— EnsecoA Comirii; Ci>mpjrn

SINGLE CONTROL SAMPLE REPORTOrganics by Chromatography


Category: TCO-WMatrix: WASTEQC Lot: 25 MAY 93-1A QC Run: 25 MAY 93-1AConcentration Units: mg/kg

o-Terphenyl 2.00 1.81 90 54-141


METHOD BLANK REPORTOrganics by Chromatography

EnsecoA Corning Compani


Units Limit

Test: TCO-FID-WMatrix: SOLIDQC Lot: 25 MAY 93-1A QC Run: 25 MAY 93-1A



EnsecoA Coming Coinpj

LaboratorySample Number029365-0001-SA029365-0001-SA029365-0001-SA029365-0001-SA029365-0001-SA029365-0002-SA029365-0002-SA029365-0002-SA029365-0002-SA029365-0003-SA

QC Matrix

SOILSOILSOIL-LEACHATESOILSOILSOILSOILSOILSOIL

QC CategoryICP-SAS-FAA-SSE-FAA-SICP-TLHG-CVAA-SICP-SHG-CVAA-SAS-FAA-SSE-FAA-SICP-S

QC Lot Number(DCS)

07 JUN 93-1C09 JUN 93-1C09 JUN 93-1C07 JUN 93-1A04 JUN 93-1B07 JUN 93-1C11 JUN 93-4B09 JUN 93-1C09 JUN 93-1C07 JUN 93-1C


07 JUN 93-1C09 JUN 93-1C09 JUN 93-1C07 JUN 93-1A04 JUN 93-1B07 JUN 93-1C11 JUN 93-4B09 JUN 93-1C09 JUN 93-1C07 JUN 93-1C


-. EnsecoA CummR Cumpam


Spiked Measured Average(%) . (RPD)DCS1 DCS2 AVG DCS Limits DCS Limit

Category: ICP-SMatrix: SOILQC Lot: 07 JUN 93-1CConcentration Units: rag/kg

AluminumAntimonyArsenicBariumBerylliumCadmiumCalciumChromiumCobaltCopperIronLeadMagnesiumManganeseMolybdenumNickelPotassiumSilverSodiumVanadiumZinc

1070055.21455031291547390151122162

1540014837404231591664050104747154530

1130067.41655231471617720167131188

17800157

41204641711804700112939168572

1120065.51525201451607660165129183

17500152

4010461170177

4170111877166572

1120066.41585211461607690166130186

1760015540704621711794430112908167572

105120109104113104104110106115115105109109107108109108122108108

47-15318-36259-14176-12453-13168-13279-12166-13370-13070-13266-13466-13574-12674-12571-12967-13368-13276-12457-13073-12765-135

1.22.87.70.61.40.30.81.31.62.51.43.42.80.80.51.6120.86.91.10.1

Category: AS-FAA-SMatrix: SOILQC Lot: 09 JUN 93-1CConcentration Units: mg/kg

Arsenic 145 120 115 118 81 59-141 4.3 20

Category: SE-FAA-SMatrix: SOILQC Lot: 09 JUN 93-1CConcentration Units: mg/kgSelenium 143 124 118 121 85 68-132 5.0 20


DUPLICATE CONTROL SAMPLE REPORTMetals Analysis and Preparation (cont.)

EnsecoA Cu


SpikedDCS1

MeasuredDCS2 AVG

Accuracy PrecisionAverage(%) . (RPD)


Category: ICP-TL-Matrix: LEACHATEQC Lot: 07 JUN 93-1AConcentration Units: mg/LAluminumAntimonyArsenicBariumBerylliumCadmiumChromiumCobaltCopperIronLeadManganeseNickelSilverVanadiumZinc

20.05.005.0020.00.5000.5002.005.002.5010.05.005.005.000.5005.005.00

19.74.855.4719.10.5200.4331.994.802.5610.05.044.884.840.5325.215.10

19,74.785.2819.10.5070.4941.984.732.529.824.894.834.790.5525.195.06

19.74.815.3719.1

0.5140.4631.984.762.549.914.964.854.820.5425.205.08

98961079610393999510299999796108104102

75-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-12575-125

0.11.53.40.02.6130.21.41.41.83.01.21.03.60.50.7

2020202020202020202020202020•2020

Category: HG-CVAA-SMatrix: SOILQC Lot: 04 JUN 93-16Concentration Units: mg/kg

Mercury 29.0 29.0 29.0 29.0 100 52-148 0.0 20

Category: HG-CVAA-SMatrix: SOILQC Lot: 11 JUN 93-4BConcentration Units: mg/kgMercury 29.0 33.8 34,8 34.3 118 52-148 2.9 20



EnsecoA Cormni; Cuimpj

Analyte Result ReportingUnits Limit

Test: ICP-RCRA-SMatrix: SOLID •QC Lot: 07 JUN 93-1C QC Run: 07 OUN 93-1CBariumCadmiumChromiumLeadSilver *

NDND1.0NDND


1.00.501.05.01.0

Test: AS-FAA-SMatrix: SOLIDQC Lot: 09 JUN 93-1C QC Run: 09 JUN 93-1C


Test: SE-FAA-SMatrix: SOLIDQC Lot: 09 JUN 93-1C QC Run: 09 JUN 93-1C


Test: ICP-OTC-TCLP-LMatrix: SOLIDQC Lot: 07 JUN 93-1A QC Run: 07 JUN 93-1ALead ND mg/L 0.50

Test: HG-CVAA-SMatrix: SOLIDQC Lot: 04 JUN 93-1B QC Run: 04 JUN 93-IB




Units Limit

EnsecoA Coming Compj

Test: ICP-RCRA-SMatrix: SOLID •QC Lot: 07 JUN 93-1C QC Run: 07 JUN 93-1C


NDND1.0NDND


1.00.501.05.01.0

Test: HG-CVAA-SMatrix: SOLIDQC Lot: 11 JUN 93-4B QC Run: 11 JUN 93-4B


Test: AS-FAA-SMatrix: SOLIDQC Lot: 09 JUN 93-1C QC Run: 09 JUN 93-1C


Test: SE-FAA-SQC Lot! 09 JUN 93-1C QC Run: 09 JUN 93-1C


Test: ICP-WMatrix: LEACHATEQC Lot: 07 JUN 93-1C QC Run: 07 JUN 93-1C

Lead ND mg/kg 5.0

EnsecoA Coming Ci'mpd



029365-0001-SA AQUEOUS PH-A 25 MAY 93-18

EnsecoA Ci>minj; CompjTn

DUPLICATE CONTROL SAMPLE REPORTWet Chemistry Analysis and Preparation


Spiked Measured Average(%) . (RPD)DCS1 DCS2 AVG DCS Limits DCS Limit

Category: PH-A •Matrix: AQUEOUSQC Lot: 25 MAY 93-1BConcentration Units: units

pH 9.10 8.98 9.04 9.01 99 98-102 0.7


9ARR ENGINEERING CO.7803 GLENROY ROADMINNEAPOLIS, MN 65439

PROJECT NUMBER N? 01791- -^ > _ *. * ' bktt!LL>HUll »- —<2i3i/iki^ i - icnfeis flOHRHlalSia

NO;

SAMPLEIDENTIFICATION

R\?Sr

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RECEIVED BY:

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DATE

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SAMPLES SHIPPED VIAD AIR FRE1QHTDFED. EXP.D 3 AMPLER

:n*— — ——————— - —— — — - ———TO

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PROJECT MANAGER:

PROJECT CONTACT:

LABORATORY:

REMARKS/ANALYSIS REQUIRED:

UM&XA s^T /iS^S1

ftAW^ s^up.. *wi.»,

RECEIVED BY LAB: DATE TIME

RECEIVED BY LAB; DATE TIME

ReceiVEQiBY LAB: DATE TIME

AIR BILL NUMBER:

OISTRieUTIONi WHITE-OFNQINAL ACCOMPANIES SHIPMENT TO LAB. fiETURNS TO BAItft WITH RESULTS: YELLOW-LAB COPY; PINK-LAB COOROIMATOFI; QOtO-F)(?LO COPY

HUFFMAN FILE COPYCUSTOMER #: LABORATORIES, INC. DATE 6/4/93

01571 Quality Analytical Services Since 1936 LAB# 184293

4630 Indiana Street-Golden, CO 80403Phone: (303) 278-4455 • FAX: (303) 278-7012

ANALYSIS REPORT ' •----'—

JUN 0 7 53R. PAUL TAYLORBARR ENGINEERING COMPANY8300 NORMAN CENTER DRIVEMINNEAPOLIS MN 55437

SEQUENCE/SAMPLE ID

MTTPnnPN— — — —— — *•W JL 1 K\J\3CiCt

A^H— — — — — — —nTTT/T.R _ —

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———— *T*

—————— %9

01R2PSH

- - - 0.20— — T QTJ . 7 J

- - - 0.16- - - 50.44

- - -7T*A

THE BTU/LB VALUE IS CORRECTED FOR SULFUR CONTENT

BARR ENGINEERING CO MEMO RE: CLP DATA VALIDATION … · Waste Management Division Office of...

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