TETRA TECH NUS, INC ^. !' 'i,.;u RttoidiCentel r · TETRA TECH NUS, INC ^. !' 'i,.;u RttoidiCentel...

TETRA TECH NUS, INC. ^ !' ' i , . ;ul RttoidiCenter 55 Jonspin Road • Wilmington, MA 01887-1020 SI I h: ^/,.-vv'/;,•„. "^ (978) 658-7899 • FAX (978) 658-7870 • www.tetratech.com BR.LAK: -,

Ms. Christine Clark November 13, 2001 Page 2

• Blanks • Surrogate Compounds • Internal Standards • Matrix Spike/Matrix Spike Duplicate • Laboratory Control Sample

NA • Field Duplicates NA • Sensitivity Check NA • PE Samples/Accuracy Check NA • Target Compound Identification

• Compound Quantitation and Reported Quantitation Limits • Tentatively Identified Compounds

* • System Performance

• - All criteria were met for this parameter.

Note: Worksheets are not included for parameters that have met criteria or for criteria that are not applicable (NA) to the method.

The following information was used to generate the Data Validation Memorandum attachments:

Table I: Recommendation Summary Table - summarizes validation recommendations

Table II: Overall Evaluation of Data - summarizes site DQOs and potential usability issues

Data Summary Tables: Summarize accepted, qualified, and rejected data

Overall Evaluation of Data and Potential Usability Issues

Following is a summary of the site DQOs:

* Data Use - sludge/soil analyses will be used for streamlined human health and ecological risk; TCLP analyses will be used to determine disposal characteristics.

Volatiles

The following list summarizes the measurement error associated with analysis: instrument calibration variability, and method blank contamination.

* The non-detected results for 1,2-dibromo-3-chloropropane in all the samples are rejected (R) due to poor initial and continuing calibration instrument response.

* The non-detected results for dichlorodifluoromethane, and chloromethane in all the samples are estimated (UJ) due to instrument calibration variability.

Ms. Christine Clark November 13, 2001 PageS

* The positive methylene chloride result in sample D02848 is considered to be non-detect due to method blank contamination. The result was not affected.

TCLP - Volatiles

The following list summarizes the TCLP - volatile measurement error associated with analysis: instrument calibration variability.

* The non-detected results for 2-butanone in samples D028248, and D02849 are estimated (UJ) due to instrument calibration variability.

Semivolatiles

The following list summarizes the semivolatile measurement error associated with analysis: instrument calibration, and method blank contaminants

* The non-detected results for benzaldehyde in all samples are estimated (UJ) due to instrument calibration variability.

* The non-detected results for atrazine and 2,2'-oxybis(1-chloropropane) in samples D02847, D02848 are estimated (UJ) due to instrument calibration variability.

* The non-detected results for benzaldehyde, 3,3'-dichlorobenzidine, di-n-octylphthalate, indeno(1,2,3-cd)pyrene, dibenzo(a,h)anthracene, and benzo(g,h,i)perylene in samples D02849, D02850, and D02851 are estimated (UJ) due to instrument calibration variability.

* The positive bis(2-ethylhexyl)phthalate results in the sludge/soil samples are considered to be non-detect due to method blank contamination. The results were not affected.

TCLP - Semivolatiles

The following list summarizes the TCLP - semivolatile measurement error associated with analysis: holding times, internal standards, matrix spike recoveries.

* The positive and non-detected results in all sludge samples are estimated (J, UJ) due to exceeded technical holding times. The results may be biased low or false negative.

* The non-detected results for 2,4,6-trichlorophenol and 2,4-dinitrotoluene in sample D02848 are estimated (UJ) due to low internal standard recoveries. The results may be false negative.

* The positive result for 2,4,5-trichlorophenol in sample D02848 is estimated (J) due to poor matrix spike recovery. The result may be biased low.

* The positive result for 4-methylphenol in sample D02848 is estimated (J) due to poor matrix spike recovery. The result may be biased high.


Pesticide/PCBs

The following list summarizes the pesticide/PCB measurement error associated with analysis: holding times, surrogate recoveries, laboratory control sample recovery.

* The positive and non-detected results in sample D02847 are estimated (J, UJ) due to exceeded technical holding times. The results may be biased low or false negative.

* The non-detected results for PCBs in sample D02847 are estimated (UJ) due to low surrogate recovery.

* The positive and non-detected results for pesticides in sample D02848 are estimated (J, UJ) due to low surrogate recovery.

4 The positive and non-detected pesticide and PCB results are estimated (J, UJ) in samples D02848, D02849, D02850, and D02851 due to low laboratory control sample recoveries. The results may be biased low or false negative.

TCLP - Pesticides

The following list summarizes the TCLP - pesticide measurement error associated with analysis: holding times.

» The non-detected results in all sludge samples are estimated (J, UJ) due to exceeded technical holding times. The results may be biased low or false negative.

Data Completeness

The laboratory was contacted on November 2, and 6, 2001 due to missing log sheets, missing TCLP extraction blanks, incorrect dilution factors, and. incorrect percent recoveries for the GPC Calibration Verification standard. Resubmitals were received on November 9, 2001.

Preservation and Technical Holding Times


All sludge samples were leached 5 days beyond the 14-day technical holding time. The positive and non-detected results are estimated (J, UJ). The results may be biased low or false negative.

Pesticide/PCBs

The laboratory re-extracted all of the sludge/soils samples 15-16 days beyond the technical holding time. The re-extracts were performed due to various technical problems including poor surrogate recovery, LCS recovery, and chromatography in both the field samples and the associated extraction QC samples. Professional judgement was used to report the least affected analysis on the data summary table and apply qualifications as noted in this data validation memo. The positive and non-detected results in sample D02847 are estimated (J, UJ) due to an exceeded technical holding times. The results may be biased low or false negative.

Ms. Christine Clark November 13, 2001 PageS

TCLP - Pesticide/PCBs

All sludge samples were leached 5 days beyond the 14-day technical holding time. The positive and non-detected results are estimated (J, UJ). The results may be biased low or false negative.

Initial and Continuing Calibrations

Volatiles

The following table summarizes the volatile compounds that failed to meet the initial calibration (1C) criterion of RRF > 0.050; continuing calibration (CC) criteria of %D < 25, RRF > 0.050:

MS-12 MS-12 Action Affected Instrument

Samples

Compound 1C CC " (+) NDs

9/2/01 9/15/01

1 ,2-Dibromo-3-chloropropane RRF 0.041 RRF 0.041 R D02846, D02847, D02848, D02849, D02850, D02851

Dichlorodifluoromethane %D - 67.8 UJ D02846, D02847, D02848, D02849, D02850, D02851

Chloromethane %D -34.8 UJ D02846, D02847, D02848, D02849, D02850, D02851

TCLP - Volatiles

The following table summarizes the TCLP volatile compounds that failed to meet the continuing calibration (CC) criterion of %D < 25:

MS-12 Action Affected Instrument

Samples

Compound CC NDs (+)

9/14/01

2-Butanone %D 42.0 UJ D02848, D02849

Semivolatiles

The following tables summarize the semivolatile compounds that failed to meet the initial calibration (1C) criterion of %RSD < 30; continuing calibration (CC) criterion of %D < 25:


Instrument MS-10 MS- 11 MS-10 Action Affected

Samples

Compound 1C

8/20/01

1C

9/14/01

CC

9/21/01

(+) NDs

Benzaldehyde %RSD 34.9 %D 30.8 UJ D02847, D02848, D02849, D02850, D02851

Atrazine %RSD 102.3 %D 78.7 UJ D02847, D02848

2,2'-oxybis(1 -chlorophenol) %D -30.0 UJ D02847, D02848

MS-11 Action Affected Instrument

Samples

Compound CC (+) NDs

9/17/01

Benzaldehyde %D 36.7 UJ D02849, D02850, D02851

3,3'-Dichlorobenzidine %D -29.0 UJ D02849, D02850, D02851

Di-n-octylphthalate %D 46.4 UJ D02849, D02850, D02851

lndeno(1 ,2,3-cd)pyrene %D -28.8 UJ D02849, D02850, D02851

Dibenzo(a,h)anthracene %D -33.1 UJ D02849, D02850, D02851

Benzo(g,h ,i)perylene %D -28.1 UJ D02849, D02850, D02851

The following table summarizes the level of blank contamination detected in the laboratory and field blanks associated with these samples.

Compound Type of Maximum Action Level CRQL Blank Concentration (pg/Kg) (Mg/Kg)

(M9/Kg)

Methylene chloride Method blank 130 1300 250

Blank action was applied to sample D02848 due to methylene chloride blank contamination. Since methylene chloride is a common laboratory contaminant, the 10x rule applies. The data may have been biased high or false positive.

The following actions apply for blank contamination:

Ms. Christine Clark November 13, 2001 Page?

• Accept values > Action Level. • Report as (U) values > CRQL and < Action Level. • Report CRQL (U) values < CRQL and < Action Level.

Semivolatiles

The following table summarizes the level of blank contamination detected in the laboratory and field blanks associated with the sludge/soil samples.

Compound Type of Maximum Action Level CRQL

Blank Concentration (MQ/Kg) (Mg/Kg) (no/Kg)

bis(2-Ethylhexyl)phthalate Method blank 240 2400 170

Blank actions were applied to the samples due to bis(2-ethylhexyl)phthalate blank contamination. Since bis(2-ethylhexyl)phthalate is a common laboratory contaminant, the 10x rule applies. The data may have been biased high or false positive.

The following actions apply for blank contamination:

• Accept values > Action Level. • Report as (U) values > CRQL and < Action Level. • Report CRQL (U) values < CRQL and < Action Level.

Surrogate Compounds

Pesticide/PCBs

The following table summarizes the pesticide/PCB surrogate compound recoveries that did not meet QC limits:

Sample ID TCX (column 1)

%REC

TCX (column 2)

%REC

DCB (column 1)

%REC

DCB (column 2)

%REC

Action

(+) ND

D02847 6923 0 UJ

D02848 415 0 J UJ

QC Limits 30-150 30-150 30-150 30-150

Since the QC limits are advisory, professional judgement was used to estimate (UJ) the non-detected PCB results in sample D02847, and estimate (J, UJ) the positive and non-detected pesticide results in sample D02848. The bias is undetermined.

Ms. Christine Clark November 13, 2001 Page8

Internal Standards


The following table summarizes the internal standard recoveries that did not meet QC limits:

Internal Standard IS Acceptable Action* Affected

Area Range (+) ND Sample

Acenapthtene-d10 146902 199687-798746 UJ D02848

* Action applies only to those compounds associated with the non-compliant internal standard.

Sample D02848 was not reanalyzed and no matrix effect was demonstrated. The non-detected results for 2,4,6-trichlorophenol and 2,4-dinitrotoluene in sample D02848 are estimated (UJ) due to low internal standard recoveries. The results may be false negative.

Matrix Spike

TCLP - Semivolatile

The following table summarizes the TCLP - semivolatile matrix spiking compound recoverie that did not meet QC limits in the matrix spike analysis of sample D02848:

Compound MS QC Action %REC Limits

(+) ND

2,4,5-Trichlorophenol -140 58-95 J

4-Methylphenol 135 29-96 J

The positive result for 2,4,5-trichlorophenol is estimated (J) in sample D02848 due to low matrix spike recovery. The result may be biased low.

The positive result for 4-methylphenol is estimated (J) in sample D02848 due to high matrix spike recovery. The result may be biased high.

Laboratory Control Sample

Pesticides

The following tables summarize the pesticide compound recoveries that did not meet QC limits in the laboratory control samples:


PLCS01

Compound MS QC Action Affected samples %REC Limits

(+) ND

Gamma-BHC 23 46-127 J UJ D02849, D02850, D02851

Heptachlor 26 35-130 J UJ D02849, D02850, D02851

Aldrin 23 34-132 J UJ D02849, D02850, D02851

Dieldrin 28 31 .-134 J UJ D02849, D02850, D02851

Endrin 26 42.-139 J UJ D02849, D02850, D02851

PLCS02

Compound MS QC Action Affected samples %REC Limits

(+) ND

Gamma-BHC 26 46-127 J UJ D02848

Heptachlor 28 35-130 J UJ D02848

Aldrin 25 34-132 J UJ D02848

Endrin 30 42.-139 J UJ D02848

Professional judgement was used to estimate (J, UJ) the positive and non-detected results for pesticides and PCBs in samples D02848, D02849, D02850, and D02851 due to low laboratory control sample recoveries. The results may be biased low.

Compound Quantitation and Reported Quantitation Limits

Volatiles

In order to account for the low percent solids in some of the volatile field samples, and to ensure that the required quantitation limits were achieved, the sampler attempted to increase sample sizes accordingly. No field samples had < 30 % solids.

Semivolatiles/ Pesticide/PCBs

In order to account for the low percent solids in the semivolatile field samples, and to ensure that the required quantitation limits were achieved, the laboratory reduced the final extract volume to 250 ul for semivolatiles and 2.5 ml for pesticide/PCB samples with moisture content below 50 percent. For samples that had moisture content between 50 and 80 percent the laboratory increased the sample extraction size and reduced the final extract volume to 250 ^L for semivolatiles and 2.5 ml for pesticide/PCB. The pesticide/PCB samples D02847 and D02848 were extracted with increased sample size using soxhlet extraction reducing the final extract volume to 2.5 ml because of the high percent moisture in these samples


System Performance

No analytical data quality trends or problems were encountered.

Please contact D. Wielandt at (978) 658-7899 if you have any questions regarding this information.

Sincerely,

Dan Wielandt Data Validator

D

"Lucy Gtjzman RAC Lead Chemist

PMO-

Tables: Table I: Recommendation Summary Table Table II: Overall Evaluation of Data Data Summary Tables

Enclosures: Data Validation Worksheets Communication/Phone Logs Field Sampling Notes (Included in Case No. 0234H, SDG No. D02098-IB) Technical Specification No. S01-RAC1-179 (Included in Case 0242H, SDG D02820) CSF Audit (DC-2 Form) DQO Summary Form

c: N. Handler (EPA) w/o enc. D. Baxter (TtNUS) w/o enc. File N41 11 -2.6 w/ enc.

Ms. Christine Clark November 13,2001 Page 11

TABLE I Recommendation Summary Table for Volatiles

Mohawk Tannery Site DAS Case 0242H, SDG D02846

TABLE I: RECOMMENDATION SUMMARY TABLE

Sample Number Matrix Qualifiers

D02846 Aqueous/Rinsate Blank J1R1

D02847 Sludge J1R1

D02848 Sludge J1'2 R1

D02849 Sludge J1R1

D02850 Soil J1R1

D02851 Soil J1R1

J1 Continuing calibration criterion (%D > 25): Estimate (UJ) non-detected results for dichlorodifluoromethane, and chloromethane due to instrument calibration variability.

Method blank contamination: Qualify the positive methylene chloride result CRQL (U) due to method blank contamination. The data may have been biased high or false positive.

R1 Initial and/or Continuing calibration criterion (RRF < 0.050): Reject (R) non-detected results for 1,2-dibromo-3-chloropropane due to poor instrument response.


TABLE I Recommendation Summary Table for TCLP Volatiles




D02847 Sludge A

D02848 Sludge J1

D02849 Sludge J1

A Accept the data

J1 Continuing calibration criterion (%D > 25): Estimate (UJ) non-detected results for 2-butanone due to instrument calibration variability.


TABLE! Recommendation Summary Table for Semivolatiles



Sample Number Matrix Qualifiers jl.2,3 D02847 Sludge

J1.2.3.5 D02848 Sludge

D02849 Sludge J1'4

J1.4.5 D02850 Soil jl.4,5 D02851 Soil

J1 Initial calibration criterion (%RSD > 30) and continuing calibration criterion (%D > 25): Estimate (UJ) non-detected results for benzaldehyde due to instrument calibration variability.

Initial calibration criterion (%RSD > 30) and continuing calibration criterion (%D > 25): Estimate (UJ) non-detected results atrazine due to instrument calibration variability.

Continuing calibration criterion (%D > 25): Estimate (UJ) non-detected results for 2,2'-oxybis(1-chlorophenol) due to instrument calibration variability.

Continuing calibration criterion (%D > 25): Estimate (UJ) non-detected results for benzaldehyde, 3,3'-dichiorobenzidine, di-n-octylphthalate, indeno(1,2,3-cd)pyrene, dibenzo(a,h)anthracene, and benzo(g,h,i)perylene due to instrument calibration variability.

Method blank contamination: Qualify the positive bis(2ethylhexyl)phthalate results as CRQL (U) due to method blank contamination. The data may have been biased high or false positive.


TABLE I Recommendation Summary Table for TCLP Semivolatiles




J1D02847 Sludge

jl.2.3 D02848 Sludge

D02849 Sludge J1

J1 Holding time criterion: Estimate (J, UJ) the positive and non-detected results due to exceeded technical holding time.

Internal Standard recovery criteria: Estimate (UJ) the non-detected results for 2,4,6-trichlorophenol, and 2,4-dinitrotoluene due to low internal standard recoveries.

MS/MSD recovery criterion: Estimate (J) the positive results for 4methylphenol due to high MS percent recovery, and estimate (J) the positive result for 2,4,5-trichlorophenol due to low MS percent recovery.


TABLE I Recommendation Summary Table for Pesticide/PCBs




D02847 Sludge J1'2

D02848 Sludge J3'4

D02849 Sludge J4

D02850 Soil J4

D02851 Soil J4

J1 Holding time criterion: Estimate (J, UJ) the positive and non-detected results due to exceeded technical holding time.

Surrogate recovery criterion: Estimate (UJ) the non-detected results for PCBs due to poor surrogate recovery.

J3 Surrogate recovery criterion: Estimate (J, UJ) the positive and non-detected results for pesticides due to poor surrogate recovery.

J4 Laboratory control sample recovery criterion: Estimate (J, UJ) the positive and non-detected pesticide results due to low recovery.


TABLE I Recommendation Summary Table for TCLP Pesticides




D02847 Sludge J1

D02848 Sludge J1

D02849 Sludge J1

J1 Holding time criterion: Estimate (UJ) the non-detected results due to exceeded technical holding time.


TABLE II Overall Evaluation of Volatile


VOLATILE ORGANICS

DQO (list all Sampling Measurement Error Sampling Potential DQOs) and/or Variability Usability

Analytical ** Issues Method

Appropnate Yes or No

Analytical Sampling Error Error*

Yes, modified Refer to Refer to The non-detected results for 1 ,2-dibromo-3-chloropropane in all the Evaluate analytical qualifications qualifications samples are rejected (R) due to poor initial and continuing human health method CLP in R/S key In R/S key calibration instrument response and ecological SOW

J12 nsk OLM04 2, and R1 The non-detected results for dichlorodifluoromethane, and sampling

chloromethane in all the samples are estimated (UJ) due to Determine procedures instrument calibration variability Disposal are

characteristics appropriate The positive methylene chloride result in sample D02848 is for all considered to be non-detect due to method blank contamination samples The results were not affected

The evaluation of "sampling error" cannot be completely assessed in data validation Sampling variability is not assessed in data validation


TABLE II Overall Evaluation ofTCLP -Volatile


TCLP - VOLATILE ORGANICS

DQO (list all DQOs) Sampling and/or Measurement Error Sampling Potential Analytical Method Variability Usability

Appropriate ** Issues Yes or No


Evaluate human health and ecological risk

Yes, analytical method 1311 and the modified method CLP SOW

Refer to qualifications in R/S key:

Refer to qualifications In R/S key:

The non-detected results for 2butanone in samples D028248, and D02849 are estimated (UJ) due to

OLM04.2, and J1 instrument calibration variability. Determine Disposal sampling characteristics. procedures are

appropriate for all samples.

The evaluation of "sampling error" cannot be completely assessed in data validation. Sampling variability is not assessed in data validation.


TABLE II Overall Evaluation of Semivolatile


SEMIVOLATILE ORGANICS

DQO (list all DQOs)


Determine Disposal characteristics.

Sampling and/or Analytical Method

Appropriate Yes or No

Yes, modified analytical method CLP SOW OLM04.2, and sampling procedures are appropriate for all samples.

Measurement Error Sampling Variability

**

Analytical Error

Sampling Error*



jl.2.3.4,5

Potential Usability Issues

The non-detected results for benzaldehyde in all samples are estimated (UJ) due to instrument calibration variability.

The non-detected results for atrazine and 2,2'-oxybis(1-chloropropane) in samples D02847, D02848 are estimated (UJ) due to instrument calibration variability.

The non-detected results for benzaldehyde, 3,3'-dichlorobenzidine, di-n-octylphthalate, indeno(1 ,2,3-cd)pyrene, dibenzo(a,h)anthracene, and benzo(g,h,i)perylene in samples D02849, D02850, and D02851 are estimated (UJ) due to instrument calibration variability.

The positive bis(2-ethylhexyl)phthalate results in the sludge/soil samples are considered to be non-detect due to method blank contamination. The results were not affected.



TABLE II Overall Evaluation of TCLP - Semivolatile


TCLP - SEMIVOLATILE ORGANICS

DQO (list all DQOs) Sampling and/or Measurement Error Sampling Potential Analytical Method Variability Usability

Appropriate ** Issues Yes or No



Yes, analytical method 131 land modified method CLP SOW



The positive and non-detected results in all sludge samples are estimated (J, UJ) due to


OLM04.2, and sampling procedures are

jl.2.3 exceeded technical holding times. The results may be biased low or false negative.

appropriate for all samples. The non-detected results for

2,4,6-trichlorophenol and 2,4dinitrotoluene in sample D02848 are estimated (UJ) due to low internal standard recoveries. The results may be false negative.

The positive result for 2,4,5trichlorophenol in sample D02848 is estimated (J) due to poor matrix spike recovery. The result may be biased low.

The positive result for 4methylphenol in sample D02848 is estimated (J) due to poor matrix spike recovery. The result may be biased high.



TABLE II Overall Evaluation of Pesticide/PCB


PESTICE/PCB ORGAN ICS

DQO (list all DQOs)





Yes, modified analytical method CLP SOW OLM04.2, and sampling procedures are appropriate for all samples.

Measurement Error Sampling Variability

*•*

Analytical Error

Sampling Error*



j1.2,3.4

Potential Usability Issues

The positive and non-detected results in sample D02847 are estimated (J, UJ) due to exceeded technical holding times. The results may be biased low or false negative.

The non-detected results for PCBs in sample D02847 are estimated (UJ) due to low surrogate recovery.

The positive and non-detected results for pesticides in sample D02848 are estimated (J, UJ) due to low surrogate recovery.

The positive and non-detected pesticide and PCB results are estimated (J, UJ) in samples D02848, D02849, D02850, and D02851 due to low laboratory control sample recoveries. The results may be biased low or false negative.



DQO (list all DQOs)



TABLE II Overall Evaluation of TCLP - Pesticide




Yes, analytical method 1311 and modified method CLP SOW OLM04.2, and sampling procedures are appropriate for all samples.

TCLP - PESTICIDE ORGANICS

Measurement Error


Refer to Refer to qualifications qualifications in R/S key: In R/S key:

J1

Sampling Potential Variability Usability

#* Issues

The non-detected results in all sludge samples are estimated (J, UJ) due to exceeded technical holding times. The results may be biased low or false negative.


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Transcript of TETRA TECH NUS, INC ^. !' 'i,.;u RttoidiCentel r · TETRA TECH NUS, INC ^. !' 'i,.;u RttoidiCentel...