TITTABAWASSEE RIVER RESIDENTIAL FLOODPLAIN SAMPLING

TITTABAWASSEE RIVER RESIDENTIAL FLOODPLAIN SAMPLING SAGINAW COUNTY, MICHIGAN

DATA VALIDATION REPORT Date: June 12, 2008 Laboratory: Pace Analytical, Minneapolis, Minnesota Laboratory Work Order #: 1072198 Data Validation Performed By: Paul Swift, PhD, PE, Weston Solutions, Inc. (Weston) Weston Analytical Work Order #/TDD #: 20405.016.012.0407.00/S05-0012-0803-014 This data validation report has been prepared by a qualified Weston quality assurance chemist independent of the project, under the START III Region V contract. This report documents the data validation for 17 soil samples collected for the Tittabawassee River Residential Floodplain Sampling Site. The samples were analyzed for polychlorinated dibenzo-p-dioxins (PCDD) and polychlorinated dibenzofurans (PCDF) following the laboratory’s Standard Operating Procedure (SOP) Preparation and Analysis of Samples for the Determination of Dioxins and Furans, S-MN-H-002 rev 09 (Pace Analytical 2008) based on U.S. Environmental Protection Agency (U.S. EPA) Method 1613B. A quality assurance (QA) level IV data package was received from Pace Analytical. The data validation was conducted in general accordance with the U.S. EPA Analytical Services Branch “National Functional Guidelines for Chlorinated Dibenzo-p-Dioxins and Chlorinated Dibenzofurans Data Review” (U.S.EPA 2005) and project-specific criteria required by the project Quality Assurance Project Plan (QAPP; Weston 2008). The attachment contains the results summary sheets. DIOXINS AND FURANS BY U.S. EPA METHOD 1613B 1. Samples

The following table summarizes the soil samples for which this data validation was conducted.

Samples Lab ID Date

Collected Date

Extracted Date

Analyzed FPS-EU002-B-016-01-042208D 1072198001 04/22/2008 05/20/2008 05/22/2008 FPS-EU002-B-017-01-042208 1072198002 04/22/2008 05/20/2008 05/22/2008 FPS-EU002-B-018-01-042208 1072198003 04/22/2008 05/20/2008 05/22/2008 FPS-EU002-B-019-01-042208 1072198004 04/22/2008 05/20/2008 05/22/2008 FPS-EU002-B-020-01-042208 1072198005 04/22/2008 05/20/2008 05/22/2008 FPS-EU002-B-021-01-042208 1072198006 04/22/2008 05/20/2008 05/22/2008 FPS-EU002-B-022-01-042208 1072198007 04/22/2008 05/20/2008 05/22/2008 FPS-EU002-B-023-01-042208 1072198008 04/22/2008 05/20/2008 05/22/2008 FPS-EU002-B-024-01-042208 1072198009 04/23/2008 05/20/2008 05/22/2008 FPS-EU002-B-025-01-042208 1072198010 04/23/2008 05/20/2008 05/22/2008 FPS-EU002-B-026-01-042208 1072198011 04/23/2008 05/20/2008 05/22/2008 FPS-EU002-B-027-01-042208 1072198012 04/23/2008 05/20/2008 05/22/2008 FPS-EU002-B-027-01-042208D 1072198013 04/23/2008 05/20/2008 05/22/2008 FPS-EU002-B-028-01-042208 1072198014 04/23/2008 05/20/2008 05/22/2008

Data Validation Report Tittabawassee River Residential Floodplain Sampling Site Pace Analytical Laboratory Work Order #: 1072198

Samples Lab ID Date Collected

Date Extracted

Date Analyzed

FPS-EU002-B-029-01-042208 1072198015 04/23/2008 05/20/2008 05/22/2008 FPS-EU002-B-030-01-042208 1072198016 04/23/2008 05/20/2008 05/22/2008 FPS-EU002-B-031-01-042208 1072198017 04/23/2008 05/20/2008 05/22/2008

2. Holding Times

The data validation guidance states that soil samples must be stored at 4°C (± 2°C) in the dark from the time of collection until extraction for up to a period of one year. No results were qualified on this basis.

3. System Performance Checks

The perfluorokerosene (PFK) standards were evaluated and the reviewer verified that the resolving power was approximately 10,000. A Window Defining Mixture (WDM) was analyzed as required and descriptor switching times were established. The chromatographic peak separation between the 2,3,7,8-tetrachlorodibenzofuran (TCDF) peak and the 2,3,4,7-TCDF peak was resolved with a valley of ≤ 25%. The continuing calibration standard met the quality control (QC) criteria for retention time (RT), relative retention time (RRT), and ion abundance ratio.

4. Initial Calibration Results

The relative standard deviations (RSD) for the relative response factors (RRF) were less than 20% for the 2,3,7,8-substitued compounds and 35% for the other compounds as required.

5. Continuing Calibration Results

The measured RRFs of each analyte were within the QC limit of ± 25% difference (%D) for the 2,3,7,8-substitued compounds and ± 35% D for all other compounds of the mean values established during initial calibration.

Data Validation Report Tittabawassee River Residential Floodplain Sampling Site Pace Analytical Laboratory Work Order #: 1072198 6. Identification Criteria

The following identification criteria have been spot-checked for in the investigative samples associated with this work order.

• The RRTs for the 2,3,7,8-substituted compounds were within the appropriate RRT windows.

• From the Selected Ion Current Profiles (SICP), it was verified that the ion current responses for the two quantitation ions for each analyte maximize simultaneously (within the same 2 seconds).

• From the SICPs, it was verified that for each analyte ion listed, the S/N ratio is ≥ 2.5:1 and that the detector was not saturated.

• The ion abundance ratios are within the criteria listed in Table A.4 of the data validation guidance, with the exceptions listed in Item 10 below..

7. Blank Results

A method blank was analyzed with the samples as required and was free of target compound contamination above the reporting limit, with the following exceptions. 1,2,3,7,8-PeCDD was recovered from the MB sample at a concentration above the RL but below the PQL. This analyte was detected in sample FPS-EU002-B-016-01-042208D at a concentration less than 10-times the blank concentration, and was reported as not-detected (U) at the reported concentration. 1,2,4,7,8-HxCDD was recovered from the MB sample at a concentration above the RL but below the PQL. This analyte was detected in sample FPS-EU002-B-022-01-042208 at a concentration less than 10-times the blank concentration, and was reported as not-detected (U) at the reported concentration

8. Laboratory Control Sample (LCS) Results

Recoveries of all congeners from the LCS and LCS duplicate recoveries were within the laboratory-established QC limits. Recoveries of congeners from the project-specific LCS sample also met all recovery criteria.

Data Validation Report Tittabawassee River Residential Floodplain Sampling Site Pace Analytical Laboratory Work Order #: 1072198 9. Matrix Spike (MS) and Matrix Spike Duplicate (MSD) Results

Sample FPS-EU002-R-021-01-041008 was prepared for MS/MSD analysis. Congener recoveries and relative percent difference (RPD) values were within the QC limits specified in the project QAPP, with the following exceptions.

The congener recoveries that exceeded the QAPP recovery criteria were present in the parent sample at concentrations that significantly exceeded (greater than a factor of four) the concentration of the spike added. No data were qualified on this basis.

10. Compound Quantitation

The individual and total Toxic Equivalents (TEQ) concentrations were calculated correctly using the appropriate toxicity equivalency factors (TEF).

A second column confirmation was performed for detections of 2,3,7,8-TCDF.

The recoveries of the internal standards were within the QC limits. For cases where the corresponding ion abundance ratios were outside the QC limits, the laboratory correctly calculated the expected maximum possible concentration (EMPC) values.

For cases where interference was observed due to the presence of polychlorinated diphenyl ether compounds, the laboratory flagged the data as ‘E’. These interferences were confirmed by the reviewer, and the data flags were removed and replaced with either the ‘UJ’ or ‘J’ flag to indicate that the reported detection limit or concentration, respectively, is an estimated value. In the opinion of the reviewer, these data may exhibit possible high bias.

11. Overall Assessment of Data

The data are ACCEPTABLE for use based on the information available for review. In general, the data required no qualification in addition to that applied by the laboratory; the reviewer replaced laboratory data flags with data validation qualifiers consistent with those provided by the Functional Guidelines (EPA 2005).

ATTACHMENT

PACE ANALYTICAL RESULTS SUMMARY

REPORT OF LABORATORY ANALYSISThis report shall not be reproduced, except in full,

without the written consent of Pace Analytical Services, Inc.

Pace Analytical Services, Inc.1700 Elm Street - Suite 200

Minneapolis, MN 55414

Tel: 612-607-1700Fax: 612- 607-6444

Lab Sample ID

Injected ByFilename

Total Amount Extracted% MoistureDry Weight ExtractedICAL IDCCal Filename(s)Method Blank ID

Client's Sample ID FPS-EU002-B-016-01-042208D1072198001D80522A07CVS

15.912.1 g

10.2 gD80520GC1D80521B16BLANK-16406

MatrixDilutionCollectedReceivedExtractedAnalyzed

SoilNA04/22/200804/26/200805/20/200805/22/2008 17:28

Client - Weston Solutions, Inc.Method 1613 Sample Analysis Results

NativeIsomers

Concng/Kg ng/Kg

RL InternalStandards Added

ng's PercentRecovery

EMPCng/Kg

2,3,7,8-TCDF 61.00 0.081 2,3,7,8-TCDF-13C 2.00 101-----Total TCDF 140.00 0.081 2,3,7,8-TCDD-13C 2.00 84-----

1,2,3,7,8-PeCDF-13C 2.00 912,3,7,8-TCDD ----- 0.092 2,3,4,7,8-PeCDF-13C 2.00 93I0.23Total TCDD 3.30 0.092 1,2,3,7,8-PeCDD-13C 2.00 94-----

1,2,3,4,7,8-HxCDF-13C 2.00 941,2,3,7,8-PeCDF 31.00 0.060 1,2,3,6,7,8-HxCDF-13C 2.00 87-----2,3,4,7,8-PeCDF 27.00 0.065 2,3,4,6,7,8-HxCDF-13C 2.00 88-----Total PeCDF 91.00 0.062 1,2,3,7,8,9-HxCDF-13C 2.00 91-----

1,2,3,4,7,8-HxCDD-13C 2.00 811,2,3,7,8-PeCDD 0.50 0.065 1,2,3,6,7,8-HxCDD-13C 2.00 80BJ-----Total PeCDD 0.85 0.065 1,2,3,4,6,7,8-HpCDF-13C 2.00 83J-----

1,2,3,4,7,8,9-HpCDF-13C 2.00 791,2,3,4,7,8-HxCDF 22.00 0.039 1,2,3,4,6,7,8-HpCDD-13C 2.00 86-----1,2,3,6,7,8-HxCDF 4.10 0.057 OCDD-13C 4.00 69J-----2,3,4,6,7,8-HxCDF 3.40 0.042 J-----1,2,3,7,8,9-HxCDF 4.10 0.038 1,2,3,4-TCDD-13C 2.00 NAJ-----Total HxCDF 56.00 0.044 1,2,3,7,8,9-HxCDD-13C 2.00 NA-----

1,2,3,4,7,8-HxCDD 0.45 0.067 2,3,7,8-TCDD-37Cl4 0.20 91J-----1,2,3,6,7,8-HxCDD 1.50 0.088 J-----1,2,3,7,8,9-HxCDD 0.84 0.110 J-----Total HxCDD 10.00 0.090-----

1,2,3,4,6,7,8-HpCDF 41.00 0.039 Total 2,3,7,8-TCDD-----1,2,3,4,7,8,9-HpCDF 2.70 0.053 Equivalence: 20 ng/KgJ-----Total HpCDF 89.00 0.046 (Using 2005 WHO Factors - Using PRL/2 where ND)-----

1,2,3,4,6,7,8-HpCDD 30.00 0.084-----Total HpCDD 54.00 0.084-----

OCDF 73.00 0.100-----OCDD 330.00 0.073-----

Conc = Concentration (Totals include 2,3,7,8-substituted isomers).EMPC = Estimated Maximum Possible ConcentrationRL = Reporting Limit.

ND = Not DetectedNA = Not ApplicableNC = Not Calculated

Results reported on a dry weight basis and are valid to no more than 2 significant figures.J = Value below calibration rangeB = Less than 10x higher than method blank levelI = Interference present

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Client's Sample ID FPS-EU002-B-017-01-0422081072198002D80522A08CVS

17.512.9 g

10.6 gD80520GC1D80521B16BLANK-16406


SoilNA04/22/200804/26/200805/20/200805/22/2008 18:20


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg


1,2,3,7,8-PeCDF-13C 2.00 892,3,7,8-TCDD 3.1 0.097 2,3,4,7,8-PeCDF-13C 2.00 93-----Total TCDD 100.0 0.097 1,2,3,7,8-PeCDD-13C 2.00 92-----


1,2,3,4,7,8-HxCDD-13C 2.00 751,2,3,7,8-PeCDD 5.8 0.049 1,2,3,6,7,8-HxCDD-13C 2.00 73-----Total PeCDD 59.0 0.049 1,2,3,4,6,7,8-HpCDF-13C 2.00 79-----

1,2,3,4,7,8,9-HpCDF-13C 2.00 771,2,3,4,7,8-HxCDF 310.0 0.120 1,2,3,4,6,7,8-HpCDD-13C 2.00 80-----1,2,3,6,7,8-HxCDF 44.0 0.130 OCDD-13C 4.00 67-----2,3,4,6,7,8-HxCDF 44.0 0.110-----1,2,3,7,8,9-HxCDF 63.0 0.100 1,2,3,4-TCDD-13C 2.00 NA-----Total HxCDF 630.0 0.110 1,2,3,7,8,9-HxCDD-13C 2.00 NA-----

1,2,3,4,7,8-HxCDD 4.5 0.120 2,3,7,8-TCDD-37Cl4 0.20 87J-----1,2,3,6,7,8-HxCDD 12.0 0.063-----1,2,3,7,8,9-HxCDD 7.2 0.100-----Total HxCDD 120.0 0.093-----

1,2,3,4,6,7,8-HpCDF 240.0 0.110 Total 2,3,7,8-TCDD-----1,2,3,4,7,8,9-HpCDF 24.0 0.190 Equivalence: 380 ng/Kg-----Total HpCDF 510.0 0.150 (Using 2005 WHO Factors - Using PRL/2 where ND)-----


OCDF 400.0 0.170-----OCDD 1700.0 0.160-----



Results reported on a dry weight basis and are valid to no more than 2 significant figures.J = Value below calibration range

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17.412.8 g

10.6 gD80520GC1D80521B16BLANK-16406


SoilNA04/22/200804/26/200805/20/200805/22/2008 19:12


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg




1,2,3,4,7,8-HxCDD-13C 2.00 811,2,3,7,8-PeCDD 2.9 0.085 1,2,3,6,7,8-HxCDD-13C 2.00 80J-----Total PeCDD 22.0 0.085 1,2,3,4,6,7,8-HpCDF-13C 2.00 85-----


1,2,3,4,7,8-HxCDD 3.1 0.150 2,3,7,8-TCDD-37Cl4 0.20 100J-----1,2,3,6,7,8-HxCDD 7.4 0.051-----1,2,3,7,8,9-HxCDD 3.9 0.087 J-----Total HxCDD 47.0 0.097-----



OCDF 330.0 0.120-----OCDD 1100.0 0.220-----




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17.612.8 g

10.6 gD80520GC1D80521B16BLANK-16406


SoilNA04/22/200804/26/200805/20/200805/22/2008 20:03


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg






1,2,3,4,7,8-HxCDD 2.5 0.079 2,3,7,8-TCDD-37Cl4 0.20 97J-----1,2,3,6,7,8-HxCDD 6.6 0.120-----1,2,3,7,8,9-HxCDD 4.6 0.063 J-----Total HxCDD 51.0 0.086-----



OCDF 170.0 0.120-----OCDD 980.0 0.130-----




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15.712.4 g

10.4 gD80520GC1D80521B16BLANK-16406


SoilNA04/22/200804/26/200805/20/200805/22/2008 20:55


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg






1,2,3,4,7,8-HxCDD ----- 0.082 2,3,7,8-TCDD-37Cl4 0.20 85I1.41,2,3,6,7,8-HxCDD 4.20 0.078 J-----1,2,3,7,8,9-HxCDD 1.70 0.110 J-----Total HxCDD 15.00 0.090-----



OCDF 230.00 0.130-----OCDD 660.00 0.160-----



Results reported on a dry weight basis and are valid to no more than 2 significant figures.J = Value below calibration rangeI = Interference present

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Client's Sample ID FPS-EU002-B-021-01-0422081072198006F80522B_12SMT

20.513.0 g

10.3 gF80318F80522B_01BLANK-16406


SoilNA04/22/200804/26/200805/20/200805/22/2008 18:33


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg






1,2,3,4,7,8-HxCDD 1.3 0.26 2,3,7,8-TCDD-37Cl4 0.20 90J-----1,2,3,6,7,8-HxCDD 6.9 0.38-----1,2,3,7,8,9-HxCDD ----- 0.39 I3.2Total HxCDD 37.0 0.34-----



OCDF 370.0 0.17-----OCDD 1600.0 0.30-----




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18.612.8 g

10.4 gF80318F80522B_01BLANK-16406


SoilNA04/22/200804/26/200805/20/200805/22/2008 13:18


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg


1,2,3,7,8-PeCDF-13C 2.00 732,3,7,8-TCDD 0.58 0.094 2,3,4,7,8-PeCDF-13C 2.00 79J-----Total TCDD 5.00 0.094 1,2,3,7,8-PeCDD-13C 2.00 87-----



1,2,3,4,7,8,9-HpCDF-13C 2.00 831,2,3,4,7,8-HxCDF 18.00 0.290 1,2,3,4,6,7,8-HpCDD-13C 2.00 95-----1,2,3,6,7,8-HxCDF 7.10 0.320 OCDD-13C 4.00 80-----2,3,4,6,7,8-HxCDF 2.90 0.210 J-----1,2,3,7,8,9-HxCDF 6.40 0.190 1,2,3,4-TCDD-13C 2.00 NA-----Total HxCDF 65.00 0.250 1,2,3,7,8,9-HxCDD-13C 2.00 NA-----

1,2,3,4,7,8-HxCDD 0.34 0.220 2,3,7,8-TCDD-37Cl4 0.20 87BJ-----1,2,3,6,7,8-HxCDD 1.70 0.250 J-----1,2,3,7,8,9-HxCDD ----- 0.200 I0.88Total HxCDD 9.00 0.220-----

1,2,3,4,6,7,8-HpCDF 71.00 0.320 Total 2,3,7,8-TCDD-----1,2,3,4,7,8,9-HpCDF 3.40 0.410 Equivalence: 26 ng/KgJ-----Total HpCDF 120.00 0.370 (Using 2005 WHO Factors - Using PRL/2 where ND)-----


OCDF 79.00 0.150-----OCDD 270.00 0.180-----



Results reported on a dry weight basis and are valid to no more than 2 significant figures.J = Value below calibration rangeB = Less than 10x higher than method blank levelI = Interference present

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19.11.04 g

0.841 gF80318F80522B_01BLANK-16406


SoilNA04/22/200804/26/200805/20/200805/22/2008 14:03


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg


1,2,3,7,8-PeCDF-13C 2.00 722,3,7,8-TCDD 9.4 1.20 2,3,4,7,8-PeCDF-13C 2.00 78J-----Total TCDD 80.0 1.20 1,2,3,7,8-PeCDD-13C 2.00 85-----


1,2,3,4,7,8-HxCDD-13C 2.00 841,2,3,7,8-PeCDD 16.0 3.10 1,2,3,6,7,8-HxCDD-13C 2.00 93J-----Total PeCDD 56.0 3.10 1,2,3,4,6,7,8-HpCDF-13C 2.00 91J-----


1,2,3,4,7,8-HxCDD 4.6 3.80 2,3,7,8-TCDD-37Cl4 0.20 88J-----1,2,3,6,7,8-HxCDD 27.0 3.90 J-----1,2,3,7,8,9-HxCDD ----- 3.10 I22Total HxCDD 130.0 3.60-----



OCDF 1700.0 0.83-----OCDD 5000.0 2.40-----




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19.312.9 g

10.4 gF80318F80522B_01BLANK-16406


SoilNA04/23/200804/26/200805/20/200805/22/2008 14:48


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg









OCDF 580.0 0.18-----OCDD 2400.0 0.30-----




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12.711.7 g

10.2 gF80318F80522B_01BLANK-16406


SoilNA04/23/200804/26/200805/20/200805/22/2008 15:33


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg









OCDF 270.0 0.18-----OCDD 1000.0 0.23-----




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15.412.2 g

10.3 gF80318F80522B_01BLANK-16406


SoilNA04/23/200804/26/200805/20/200805/22/2008 16:19


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Concng/Kg ng/Kg



EMPCng/Kg









OCDF 450.0 0.150-----OCDD 1800.0 0.240-----




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22.513.0 g

10.1 gF80318F80522B_01BLANK-16406


SoilNA04/23/200804/26/200805/20/200805/22/2008 17:04


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg






1,2,3,4,7,8-HxCDD 8.0 0.81 2,3,7,8-TCDD-37Cl4 0.20 95-----1,2,3,6,7,8-HxCDD 38.0 1.00-----1,2,3,7,8,9-HxCDD ----- 0.59 I25Total HxCDD 210.0 0.80-----



OCDF 2700.0 0.20-----OCDD 7300.0 0.57-----



Results reported on a dry weight basis and are valid to no more than 2 significant figures.I = Interference present

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Client's Sample ID FPS-EU002-B-027-01-042308D1072198013F80522B_11SMT

22.613.0 g

10.0 gF80318F80522B_01BLANK-16406


SoilNA04/23/200804/26/200805/20/200805/22/2008 17:49


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Concng/Kg ng/Kg



EMPCng/Kg









OCDF 2400.0 0.29-----OCDD 8500.0 0.44-----




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Client's Sample ID FPS-EU002-B-028-01-0423081072198014F80523A_09SMT

17.412.7 g

10.5 gF80318F80523A_01BLANK-16406


SoilNA04/23/200804/26/200805/20/200805/23/2008 06:31


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg









OCDF 400.0 0.15-----OCDD 1700.0 0.22-----




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Client's Sample ID FPS-EU002-B-029-01-0423081072198015F80524B_05BAL

18.812.9 g

10.5 gF80318F80524A_18BLANK-16406


Soil504/23/200804/26/200805/20/200805/24/2008 17:47


NativeIsomers

Concng/Kg ng/Kg



EMPCng/Kg






1,2,3,4,7,8-HxCDD 7.8 2.70 2,3,7,8-TCDD-37Cl4 0.20 99-----1,2,3,6,7,8-HxCDD 25.0 1.80-----1,2,3,7,8,9-HxCDD 12.0 1.30-----Total HxCDD 130.0 2.00-----



OCDF 1200.0 0.96-----OCDD 4900.0 2.00-----



Results reported on a dry weight basis and are valid to no more than 2 significant figures.

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Lab Sample ID

Injected ByFilename



18.712.7 g

10.3 gF80318F80523A_01BLANK-16406


SoilNA04/23/200804/26/200805/20/200805/23/2008 08:00


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1,2,3,4,7,8-HxCDF-13C 2.00 691,2,3,7,8-PeCDF ----- 1.20 1,2,3,6,7,8-HxCDF-13C 2.00 70E16002,3,4,7,8-PeCDF 1000.0 1.10 2,3,4,6,7,8-HxCDF-13C 2.00 67-----Total PeCDF 1600.0 1.20 1,2,3,7,8,9-HxCDF-13C 2.00 71-----



1,2,3,4,7,8-HxCDD 7.1 0.75 2,3,7,8-TCDD-37Cl4 0.20 80-----1,2,3,6,7,8-HxCDD 36.0 0.82-----1,2,3,7,8,9-HxCDD 13.0 1.10-----Total HxCDD 200.0 0.91-----



OCDF 1900.0 0.42-----OCDD 7100.0 0.51-----



Results reported on a dry weight basis and are valid to no more than 2 significant figures.E = PCDE Interference

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15.912.1 g

10.2 gF80318F80523A_01BLANK-16406


SoilNA04/23/200804/26/200805/20/200805/23/2008 08:45


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OCDF 1900.0 0.74-----OCDD 5500.0 0.32-----




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Injected ByFilename


Client's Sample ID FPS-EU002-B-031-01-042308 (Dup)1072198017-DUPF80523A_13SMT

15.912.3 g

10.4 gF80318F80523A_01BLANK-16406


SoilNA04/23/200804/26/200805/20/200805/23/2008 09:30


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OCDF 2400.0 1.30-----OCDD 9400.0 0.29-----




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Lab Sample IDSample Filename

Client's Sample ID FPS-EU002-B-031-01-0423081072198017F80523A_12

Client: Weston Solutions, Inc.

Duplicate Analysis Results

Client's Duplicate IDLab Duplicate IDDuplicate Filename F80523A_13

1072198017-DUPFPS-EU002-B-031-01-042308 (Dup)

CompoundSample Conc.

ng/KgRPD

%Duplicate Conc.

ng/Kg

2,3,7,8-TCDF 11000 7100 41.5Total TCDF 23000 14000 49.1

2,3,7,8-TCDD 8.5 7.3 14.4Total TCDD 130 150 14.8

1,2,3,7,8-PeCDF 3000 2400 21.12,3,4,7,8-PeCDF 4400 3000 36.4Total PeCDF 13000 10000 19.7

1,2,3,7,8-PeCDD 13 19 33.8Total PeCDD 100 130 24.1

1,2,3,4,7,8-HxCDF 2100 1500 34.01,2,3,6,7,8-HxCDF 580 450 24.92,3,4,6,7,8-HxCDF 240 180 26.51,2,3,7,8,9-HxCDF 550 400 32.4Total HxCDF 4800 3400 33.0

1,2,3,4,7,8-HxCDD 6.6 8.4 24.61,2,3,6,7,8-HxCDD 32 46 35.51,2,3,7,8,9-HxCDD ND ND NATotal HxCDD 170 240 32.7

1,2,3,4,6,7,8-HpCDF 2100 2600 23.11,2,3,4,7,8,9-HpCDF 170 160 3.9Total HpCDF 3700 4900 27.1

1,2,3,4,6,7,8-HpCDD 490 710 36.6Total HpCDD 840 1200 37.4

OCDF 1900 2400 22.4OCDD 5500 9400 51.4

Conc = Concentration RPD = Relative Percent Difference NA = Not Applicable ND = Not Detected

RPD calculations are based on unrounded intermediate data. Consequently, it may not be possible to precisely reconstruct the resultantvalues from the rounded concentration results, due to rounding errors.

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TITTABAWASSEE RIVER RESIDENTIAL FLOODPLAIN SAMPLING SAGINAW COUNTY, MICHIGAN

DATA VALIDATION REPORT Date: June 17, 2008 Laboratory: TestAmerica, West Sacramento, California Laboratory Work Order #: G8E030179 Data Validation Performed By: Lisa Graczyk, Dynamac Corporation (Dynamac), subcontractor to Weston Solutions, Inc. (Weston) Weston Analytical Work Order #/TDD #: 20405.016.012.0407.00/S05-0012-0803-014 This data validation report has been prepared by Dynamac, a Weston subcontractor, under the START III Region V contract. This report documents the data validation for 18 soil samples collected for the Tittabawassee River Residential Floodplain Sampling Site that were analyzed for dioxins and furans using U.S. Environmental Protection Agency (U.S. EPA) Method 1613B. A quality assurance (QA) level IV data package was received from TestAmerica. The data validation was conducted in general accordance with the U.S. EPA Analytical Services Branch “National Functional Guidelines for Chlorinated Dibenzo-p-Dioxins and Chlorinated Dibenzofurans Data Review” dated September 2005. The attachment contains the results summary sheets. DIOXINS AND FURANS BY U.S. EPA METHOD 1613B 1. Samples

The following table summarizes the soil samples for which this data validation was conducted.

Samples Lab ID Date

Collected Date

Extracted Date

Analyzed FPS-EU002-H-002-01-042808 G8E030179-001 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-H-003-01-042808 G8E030179-002 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-H-004-01-042808 G8E030179-003 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-H-005-01-042808 G8E030179-004 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-H-006-01-042808 G8E030179-005 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-H-007-01-042808 G8E030179-006 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-H-007-01-042808D G8E030179-007 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-H-008-01-042808 G8E030179-008 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-G-012-01-042808 G8E030179-009 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-G-013-01-042808 G8E030179-010 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-G-014-01-042808 G8E030179-011 4/28/2008 5/17/2008 5/30/2008 FPS-EU002-G-014-01-042808D G8E030179-012 4/28/2008 5/17/2008 5/31/2008 FPS-EU002-G-015-01-042808 G8E030179-013 4/28/2008 5/17/2008 5/31/2008 FPS-EU002-G-016-01-042808 G8E030179-014 4/28/2008 5/17/2008 5/31/2008 FPS-EU002-G-017-01-042808 G8E030179-015 4/28/2008 5/17/2008 5/31/2008

Data Validation Report Tittabawassee River Residential Floodplain Sampling Site TestAmerica Laboratory Work Order #: G8E030179

Samples Lab ID Date Collected

Date Extracted

Date Analyzed

FPS-EU002-G-018-01-042808 G8E030179-016 4/28/2008 5/17/2008 5/31/2008 FPS-EU002-G-019-01-042808 G8E030179-017 4/28/2008 5/17/2008 5/31/2008 FPS-EU001-W-14-01-041608 G8E030179-018 4/16/2008 5/17/2008 5/31/2008

2. Holding Times

The data validation guidance states that soil samples must be stored at 4°C (± 2°C) in the dark from the time of collection until extraction for up to a period of one year. Samples were stored properly and analyzed within the one-year recommended holding time limit.

3. System Performance Checks

The perfluorokerosene (PFK) standards were checked manually and it was verified that the resolving power was approximately 10,000. A Window Defining Mixtrue (WDM) was analyzed by TestAmerica as required. The chromatographic peak separation between the 2,3,7,8-tetrachlorinated dibenzofuran (TCDF) peak and the 2,3,4,7-TCDF peak was resolved with a valley of ≤ 25%. The continuing calibration standard meets the quality control (QC) criteria for retention time (RT), relative retention time (RRT), and ion abundance ratio.

4. Initial Calibration Results

The relative standard deviations (RSD) for the relative response factors (RRF) were less than 20 percent as required.

5. Continuing Calibration Results

The measured RRFs of each analyte were within the QC limit of ± 20% difference (%D) of the mean values established during initial calibration.


6. Identification Criteria

The following identification criteria have been spot-checked for in the investigative samples associated with this work order.

• The RRTs for the 2,3,7,8-substituted compounds were within the appropriate RRT windows.

• From the Selected Ion Current Profiles (SICP), it was verified that the ion current responses for the two quantitation ions for each analyte maximize simultaneously (within the same 2 seconds).

• From the SICPs, it was verified that for each analyte ion listed, the S/N ratio is ≥ 2.5:1 and that the detector was not saturated.

• For target compounds detected above the reporting limit, the ion abundance ratios are within the criteria listed in Table A.4 of the data validation except for one internal standard in one of the samples. TestAmerica used theoretical areas for the internal standard to quantitate associated compounds in the associated sample. No qualification is required.

7. Blanks

A method blank was analyzed with the samples as required and was free of target compound contamination above the reporting limit except for a minor detect of octachlorinated dibenzo-p-dioxin (OCDD) at 0.46 picogram per gram (pg/g). Because all detections of OCDD in the samples were much greater than the blank concentration, no qualifications are required. The laboratory flagged all OCDD results with at “B” to indicate that it was detected in the blank.

8. Laboratory Control Sample (LCS) Results

The LCS and LCS duplicate recoveries were within the laboratory-established QC limits.

9. Laboratory Fortified Blank (Sensitivity Check)

The project-specific laboratory fortified blank was within the QAPP-established QC limit of 60 to 140 percent recovery for target compounds.

10. Matrix Spike (MS) and Matrix Spike Duplicate (MSD) Results

TestAmerica analyzed an MS and MSD using sample FPS-EU002-H-004-01-042808 as the spiked sample. The results were within the QC limits specified by the laboratory and in the project-specific QAPP.

Data Validation Report Tittabawassee River Residential Floodplain Sampling Site TestAmerica Laboratory Work Order #: G8E030179 11. Duplicates

The laboratory duplicate was within the QAPP QC limits of 25 percent relative percent difference (RPD) except for the following compounds: total tetrachlorinated dibenzo-p-dioxins (TCDD); total pentachlorinated dibenzo-p-dioxins (PeCDD); total hexachlorinated dibenzo-p-dioxins (HxCDD); and 1,2,3,6,7,8-hexachlorinated dibenzofuran (HxCDF). Detected results for these compounds were flagged “J” as estimated in the sample used for the duplicate, FPS-EU002-H-007-01-042808.

There are two field duplicates associated with this work order (identified with a “D” suffix). The field duplicate results and investigative sample results were within the QC limits set in the Quality Assurance Project Plan of 50 RPD except for as follows.

In sample FPS- EU002-H-007-01-042808 and its duplicate, the RPD for the following compounds were outside the QC limit: total TCDD; total PeCDD; total HxCDD; and 1,2,3,4,7,8,9- heptachlorinated dibenzofuran (HpCDF). Detected results for these compounds in sample FPS- EU002-H-007-01-042808 and its duplicate were flagged “J” as estimated for this discrepancy.

In sample FPS- EU002-G-014-01-042808 and its duplicate, the RPD for the following compounds were outside the QC limit: total TCDD; 1,2,3,7,8-PeCDD; and total PeCDD. Detected results for these compounds in sample FPS- EU002-G-014-01-042808 and its duplicate were flagged “J” as estimated for this discrepancy.

12. Compound Quantitation

The individual and total Toxic Equivalents (TEQ) concentrations were calculated correctly using the appropriate toxicity equivalency factors (TEF).

All samples were diluted as necessary to bring the analyte concentrations into the calibration range of the instrument.

A second column confirmation was performed for detections of 2,3,7,8-TCDF.

The recoveries of the internal standards were within the QC limits. See Section 6 for a description of the ion abundance ratio review.

Several compounds were detected below the laboratory estimated detection limit. These results were flagged with a “J” by the laboratory to indicate that the results should be considered estimated. No further qualification is required.


13. Overall Assessment of Data

The data are acceptable use as qualified based on the information received.

ATTACHMENT

TESTAMERICA RESULTS SUMMARY

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

REGION V SUPERFUND DIVISION

DATE: SUBJECT: Review of Data Received for Review on June 4, 2008 FROM: Stephen L. Ostrodka, Chief (SRT-4J) Superfund Field Services Section TO: Data User: Weston We have reviewed the data for the following case: SITE NAME: Tittabawassee River Floodplain, MI Client Project ID: 1-04/25/08-0027 SDG NUMBER: 1072204 Number and Type of Samples: 16 Soils (Dioxin/Furans) Sample Numbers: FPS-EU002-; B-047-01-042208, B-048-01-042208, B-049-01-042308 thru B-051-01-042308, B-052-01-042208 thru B-054-01-042208, B-054-01-042208DUP, B-055-01-042308 thru B-057-01-042308, B-058-01-042208 thru B-060-01-042208, B-061-01-042408 Laboratory: Pace Analytical Hrs for Review: Following are our findings: CC: Howard Pham Region 5 TPO Mail Code: SRT-4J

Page 2 of 11 Site Name: Tittabawassee River Floodplain, MI SDG Number: 1072204 Project ID: 1-04/25/08-0027 Lab: Pace Analytical

Reviewed by: Allison C Harvey/Techlaw-ESAT Date: June 12, 2008

Below is a summary of the out-of-control audits and the possible effect on the data for this case: A total of sixteen (16) soil samples were collected April 22, 2008 through April 24, 2008. All samples were received by Pace Analytical located in Minneapolis, MN on April 26, 2008 with cooler temperatures of 1.4 °C and 4.0 °C. All samples are identified in the following table. For ease of reference within this narrative the client samples will be identified by the following shorthand: Client Sample ID Lab Sample ID Filename Narrative

Sample ID FPS-EU002-B-047-01-042208 1072204001 F80524B_07 B-047-01 FPS-EU002-B-047-01-042208 MS 1072204001-MS F80524B_08 B-047-01MS FPS-EU002-B-047-01-042208 MSD 1072204001-MSD F80524B_09 B-047-01MSD FPS-EU002-B-048-01-042208 1072204002 F80523B_12 B-048-01 FPS-EU002-B-049-01-042308 1072204003 F80523B_13 B-049-01 FPS-EU002-B-050-01-042308 1072204004 F80523B_14 B-050-01 FPS-EU002-B-051-01-042308 1072204005 F80523B_15 B-051-01 FPS-EU002-B-051-01-042308(Dup) 1072204005D F80523B_16 B-051-01Dup FPS-EU002-B-052-01-042208 1072204006 F80524A_07 B-052-01 FPS-EU002-B-053-01-042208 1072204007 F80524A_08 B-053-01 FPS-EU002-B-054-01-042208 1072204008 F80524A_09 B-054-01 FPS-EU002-B-054-01-042208D 1072204009 F80528A_17 B-054-01D FPS-EU002-B-055-01-042308 1072204010 F80524A_11 B-055-01 FPS-EU002-B-056-01-042308 1072204011 F80524A_12 B-056-01 FPS-EU002-B-057-01-042308 1072204012 F80524A_13 B-057-01 FPS-EU002-B-058-01-042208 1072204013 F80524A_14 B-058-01 FPS-EU002-B-059-01-042208 1072204014 F80524A_15 B-059-01 FPS-EU002-B-060-01-042208 1072204015 F80524A_16 B-060-01 FPS-EU002-B-061-01-042408 1072204016 F80524B_06 B-061-01

All solid samples (soil, dust and wipes) were screened in accordance with the QAPP to determine the appropriate dilutions. Samples were extracted and analyzed according to PACE SOP No. S-MN-H-002 for the Preparation and Analysis of Samples for the Determination of Dioxins and Furans by USEPA 1613B. The results are validated in general accordance with the National Functional Guidelines for Chlorinated Dibenzo-p-Dioxin (CDDs) and Chlorinated Dibenzofurans (CDFs) Data Review, the analytical SOP and the QAPP for Tittabawassee River Residential Floodplain Sampling.



The Laboratory Control Sample/Duplicate are identified as LCS-16418 and LCSD-16419. The project-specific quantitation limit laboratory spike sample is identified as ALCS-16417. The method blank is identified as BLANK-16416. The source sample for the MS/MSD analyses is sample FPS-EU002-B-047-01-042208. Sample FPS-EU002-B-054-01-042208D is a field duplicate of sample FPS-EU002-B-054-01-042208. Samples FPS-EU002-B-051-01-042308 and FPS-EU002-B-051-01-042308 (Dup) are laboratory duplicates. Samples were extracted and analyzed within 30 days of sample collection; therefore, all results are acceptable. The final data package was submitted (May 29, 2008) more than 28 days from sample receipt (April 26, 2008).



1. HOLDING TIME A total of sixteen (16) soil samples were collected April 22, 2008 through April 24, 2008. All samples were received by Pace Analytical located in Minneapolis, MN on April 26, 2008 with cooler temperatures of 1.4 °C and 4.0 °C. All samples are identified in the previous table.

All solid samples (soil, dust and wipes) were screened in accordance with the QAPP to determine the appropriate dilutions. Samples were extracted and analyzed according to PACE SOP No. S-MN-H-002 for the Preparation and Analysis of Samples for the Determination of Dioxins and Furans by USEPA 1613B. The results are validated in general accordance with the National Functional Guidelines for Chlorinated Dibenzo-p-Dioxin (CDDs) and Chlorinated Dibenzofurans (CDFs) Data Review, the analytical SOP and the QAPP for Tittabawassee River Residential Floodplain Sampling. Samples were extracted and analyzed within 30 days of sample collection; therefore all results are acceptable. 2. SYSTEM PERFORMANCE CHECK AND INSTRUMENT STABILITY

The Mass Spectrometer was tuned to a resolution of ≥ 10,000 prior to sample analyses. The CPSMs (Column Performance Check Solution) were analyzed after the perfluorokerosene (PFK) tune and before any calibration standards on the instrument at the beginning of each 12-hour period. The chromatographic peak separation between 2,3,7,8-TCDD peak and the 1,2,3,8-TCDD peak was resolved with a valley ≤ 25%.

The CS3 had an absolute RT of the first internal standard C12-1,2,3,4-TCDD within ± 15 seconds of the absolute RT of the identical compound obtained during initial calibration. Relative Retention Time (RRT) criteria of the native and labeled compounds was met. Ion abundance ratios were within their respective QC limits. All signal-to-noise (S/N) ratios were ≥ 10:1. 3. CALIBRATION

Initial calibrations were conducted on March 18, 2008 and May 27, 2008 (Instrument 10MSHR05 [F]). All %RSDs for the relative response factors (RRFs) of the labeled compounds were less than 30% and therefore acceptable. All %RSDs for the relative response factors (RRFs) of the target analytes were less than 20% and therefore acceptable. All ion abundances of all compounds for each calibration standard were within ± 15% and therefore acceptable.

Calibration verification standards were conducted at the appropriate frequencies following the CPSM (Column Performance Check Solution) and again within 12-hours following the analyses of the samples. Relative Retention Time (RRT) criteria of the native and labeled compounds was met. All signal-to-noise (S/N) ratios were ≥ 10:1.



The continuing Calibration standards and their associated samples are summarized in the following table.

Cont Cal Std Samples INITIAL CAL – 03/18/2008 CS3/CPM-5176-156 05/23/2008 @ 11:06

B-048-01, B-049-01, B-050-01, B-051-01, B-051-01Dup

CS3/CPM-5176-156 05/24/2008 @ 00:35

LCS-16418, LCSD-16419, ALCS-14617, BLANK-16416, B-052-01, B-053-01, B-054-01, B-055-01, B-056-01, B-057-01, B-058-01, B-059-01, B-060-01

CS3/CPM-5176-156 05/24/2008 @ 14:01

B-061-01, B-047-01, B-047-01MS, B-047-01MSD

INITIAL CAL – 05/27/2008 CS3/CPM-5176-157 05/28/2008 @ 14:30

B-054-01D, B-054-01

All %Ds for the relative response factors (RRFs) of the labeled compounds were

less than 30% and therefore acceptable. All %Ds for the relative response factors (RRFs) of the target analytes were less than 20% and therefore acceptable. All ion abundances of all compounds for each calibration standard were within ± 15% and therefore acceptable. 4. BLANKS The method blank is identified as BLANK-16416. The method blank contained 2,3,7,8-TCDD at 0.22 ng/Kg; 1,2,3,4,6,7,8-HpCDF at 0.16 ng/Kg and OCDD at 1.30 ng/Kg. The concentrations are all less than the lowest calibration standard concentrations; 0.5 ng/Kg for TCDD/TCDF, 2.5 ng/Kg for HpCDDs/HpCDFs and 5 ng/Kg for OCDD/OCDF. No samples required qualification for this criterion. 5. LAB CONTROL SAMPLE RECOVERY/ON-GOING PRECISION

RECOVERY The Laboratory Control Sample/Duplicate are identified as LCS-16418 and LCSD-16419. All %recoveries and RPDs were within the QC criteria; therefore, the sample results do not require qualification for this criterion.

The project-specific quantitation limit laboratory spike sample is identified as ALCS-16417. Per the Laboratory Narrative the native spike recoveries were within the target range of 60-140%. The %recoveries of the labeled compounds were within the QC limits identified in QAPP Worksheet #28B. 6. MATRIX SPIKE/ MATRIX SPIKE DUPLICATE RECOVERY The source sample for the MS/MSD analyses is sample B-047-01.



The RPDs for 1,2,3,7,8-PeCDF; 1,2,3,4,7,8-HxCDF; 1,2,3,6,7,8-HxCDD; 1,2,3,4,6,7,8-HpCDF; 1,2,3,4,7,8,9-HpCDF; 1,2,3,4,6,7,8-HpCDD; OCDF and OCDD are greater than 20%. The %recoveries for 1,2,3,7,8-PeCDF; 1,2,3,4,7,8-HxCDF; 1,2,3,4,6,7,8-HpCDD and OCDF were less than 70% and greater than 10% in sample B-047-01MS. The %recoveries for 1,2,3,4,6,7,8-HpCDF and OCDD were less than 10% in B-047-01MS. The %recoveries for 2,3,7,8-TCDF and 2,3,4,7,8-PeCDF were less than 10% in both samples B-047-01MS and sample B-047-01MSD. The %recoveries for 1,2,3,7,8-PeCDF; 1,2,3,6,7,8-HxCDD; 1,2,3,4,6,7,8,-HpCDF; 1,2,3,4,7,8,9-HpCDF; 1,2,3,4,6,7,8-HpCDD; OCDF and OCDD were greater than 130% in sample B-047-01MSD. The presence of the analytes discussed above are qualified as estimated and flagged with a “J” flag in the unspiked sample B-047-01. 7. TOXICITY EQUIVALENCY FACTOR AND ISOMER SPECIFICITY

The 2,3,7,8-TCDD TEF-adjusted concentration of a sample is used by the laboratory as an aid in determining when second column confirmation or re-extraction and re-analysis are required. When calculating the 2,3,7,8-TCDD TEF-adjusted concentration of a sample, the laboratory must include only those 2,3,7,8-substituted isomers that were detected in the sample and that met all of the qualitative identification criteria.

The laboratory should not include Estimated Maximum Possible Concentration

(EMPC) or Estimated Detection Limit (EDL) values in the TEF calculations. The TEQs were calculated properly and reported to 2 significant figures. Values are included in the Excel results spreadsheet. 8. SECOND COLUMN CONFIRMATION

In general, second column confirmation is required for any samples analyzed on a

DB-5 column in which 2,3,7,8-TCDF is reported, or where 2,3,7,8-TCDF is reported as an Estimated Maximum Possible Concentration (EMPC) at or above the Contract Required Quantitation Limit (CRQL).

The project-specific QAPP for this project (Work Assignment Number S05-0012-0802-011) indicates that no screening or confirmatory-type analyses were required for this site. 9. LABELED COMPOUND RECOVERIES

The percent recoveries were within the QC acceptance limits for all samples; therefore the sample results are acceptable.



10. FIELD QC SAMPLES Sample B-054-01 is a field duplicate of sample B-054-01D. Samples B-051-01 and B-051-01 (Dup) are laboratory duplicates. Per Worksheet #12B of the QAPP; laboratory duplicates should have RPDs ≤ 20% and field duplicates should have RPDs ≤ 25%. Copies of the calculation spreadsheets are included with the hardcopy validation package.

The %RPDs for 2,3,7,8-TCDD; 1,2,3,7,8-PeCDD; 1,2,3,7,8,9-HxCDD; 1,2,3,4,7,8-HxCDF; 1,2,3,6,7,8-HxCDF; 2,3,4,6,7,8-HxCDF; 1,2,3,7,8,9-HxCDF; 1,2,3,4,6,7,8-HpCDF; 1,2,3,4,7,8,9-HpCDF and OCDF between samples B-051-01 and B-051-01Dup were greater than 20%. All other RPDs were less than 20%.

The RPDs for all analytes except 1,2,3,6,7,8-HxCDD; 1,2,3,4,7,8,9-HpCDF; OCDF and OCDD between samples B-054-01 and B-054-01DUP were greater than 25%. 11. TARGET COMPOUND IDENTIFICATION

The following samples reported target analytes with concentrations below the pattern recognition levels identified in QAPP Worksheet #28B. The detections are considered estimates and flagged with a “J” flag.

BLANK-16416 2,3,7,8-TCDD, 1,2,3,4,6,7,8-HpCDF, OCDD B-050-01, B-052-01, B-059-01 1,2,3,4,7,8-HxCDD B-051-01 1,2,3,6,7,8-HxCDF, 2,3,4,6,7,8-HxCDF, 1,2,3,7,8,9-HxCDF, 1,2,3,6,7,8-HxCDD, 1,2,3,4,7,8,9-HpCDF B-051-01Dup 2,3,7,8-TCDD, 1,2,3,7,8-PeCDD, 1,2,3,6,7,8-HxCDF, 2,3,4,6,7,8-HxCDF, 1,2,3,7,8,9-HxCDF, 1,2,3,6,7,8-HxCDD, 1,2,3,7,8,9-HxCDD, 1,2,3,4,7,8,9-HpCDF B-060-01, B-061-01 1,2,3,7,8-PeCDD, 1,2,3,4,7,8-HxCDD The ion abundance ratios for the following target analytes were outside the

acceptance limits in the associated samples. The concentrations were below the laboratory’s detection limit; therefore these concentrations are considered unusable and flagged with a “R” flag in accordance with the NFG for CDDs and CDFs (09/2005).



2,3,7,8-TCDD B-051-01, B-053-01, B-056-01 1,2,3,7,8-PeCDD B-049-01, B-051-01, B-052-01, B-057-01, B-058-01, B-059-01 1,2,3,4,7,8-HxCDD B-051-01, B-051-01Dup, B-054-01D 1,2,3,7,8,9-HxCDD B-047-01, B-048-01, B-049-01, B-050-01, B-051-01, B-052-01, B-053-01, B-054-01, B-055-01, B-056-01, B-057-01, B-058-01, B-059-01, B-060-01 B-061-01 1,2,3,4,6,7,8-HpCDD, OCDF BLANK-16416

12. ADDITIONAL INFORMATION

Samples were prepped and analyzed according to PACE Analytical SOP S-MN-H-002. The samples were extracted May 21 - 22. The samples were analyzed May 23 - 29, 2008.

The following samples have analyte concentrations that exceeded the instrument’s

highest calibration standard. Dilutions are only performed when requested by the client. No dilutions were requested by Weston. Per Region 5 Data Validation Guidelines, these concentrations are qualified as estimated and flagged with a “J” flag. TCDF (> 200 ng/Kg): B-047-01, B-048-01, B-049-01, B-050-01,

B-052-01, B-053-01, B-054-01, B-054-01D, B-055-01, B-056-01, B-057-01, B-058-01, B-059-01, B-060-01, B-061-01

1,2,3,7,8-PeCDF (> 1000 ng/Kg): B-048-01, B-049-01, B-053-01,

B-054-01D, B-055-01, B-057-01, B-058-01, B-059-01

2,3,4,7,8-PeCDF (> 1000 ng/Kg): B-048-01, B-049-01, B-052-01, B-053-01,

B-054-01D, B-055-01, B-056-01, B-057-01, B-058-01, B-059-01

1,2,3,4,7,8-HxCDF (> 1000 ng/Kg): B-048-01, B-049-01, B-053-01,

B-054-01D, B-055-01, B-058-01, B-059-01



1,2,3,4,6,7,8-HpCDF (> 1000 ng/Kg): B-048-01, B-049-01, B-053-01, B-054-01, B-054-01D, B-055-01, B-056-01, B-057-01, B-058-01

1,2,3,4,6,7,8-HpCDD (> 1000 ng/Kg): B-048-01, B-053-01, B-054-01,

B-054-01D, B-056-01, B-058-01

OCDF (> 2000 ng/Kg): B-048-01, B-049-01, B-053-01, B-054-01, B-054-01D, B-055-01, B-056-01, B-057-01, B-058-01

OCDD (> 2000 ng/Kg): B-047-01, B-048-01, B-049-01, B-050-01,

B-052-01, B-053-01, B-054-01, B-054-01D, B-055-01, B-056-01, B-057-01, B-058-01, B-059-01

The following samples contain dioxin/furan analytes with individual analyte concentrations greater than 1000 ppt: 2,3,7,8,-TCDF: B-048-01, B-049-01, B-050-01, B-052-01,

B-053-01, B-054-01, B-054-01D, B-055-01, B-056-01, B-057-01, B-058-01, B-059-01

1,2,3,7,8-PeCDF: B-048-01, B-049-01, B-053-01, B-054-01D,

B-055-01, B-057-01, B-058-01, B-059-01

2,3,4,7,8-PeCDF: B-048-01, B-049-01, B-052-01, B-053-01, B-054-01D, B-055-01, B-056-01, B-057-01, B-058-01, B-059-01

1,2,3,4,7,8-HxCDF: B-048-01, B-049-01, B-053-01, B-054-01D,

B-055-01, B-058-01, B-059-01

1,2,3,4,6,7,8-HpCDF: B-048-01, B-049-01, B-053-01, B-054-01, B-054-01D, B-055-01, B-056-01, B-057-01, B-058-01

1,2,3,4,6,7,8-HpCDD: B-048-01, B-053-01, B-054-01, B-054-01D,

B-055-01, B-056-01, B-058-01 OCDF: B-047-01, B-048-01, B-049-01, B-053-01,

B-054-01, B-054-01D, B-055-01, B-056-01, B-057-01, B-058-01, B-059-01



OCDD: B-047-01, B-048-01, B-049-01, B-050-01,

B-052-01, B-053-01, B-054-01, B-054-01D, B-055-01, B-056-01, B-057-01, B-058-01,

B-059-01, B-060-01, B-061-01 The following samples contain dioxin/furan analytes with a total TEQ concentrations greater than 1000 ppt:

B-048-01, B-049-01, B-052-01, B-053-01, B-054-01D, B-055-01, B-057-01, B-058-01, B-059-01

Sample results are identified in the accompanying Excel spreadsheet:



Data Qualifier Definitions U The analyte was analyzed for, but was not detected at a level greater than or equal

to the level of the adjusted Contract Required Quantitation Limit (CRQL) for sample and method.

J The analyte was positively identified and the associated numerical value is the

approximated concentration of the analyte in the sample [due either to the quality of the data generated because certain Quality Control (QC) criteria were not met, or the concentration of the analyte was below the adjusted CRQL].

UJ The analyte was not detected at a level greater than or equal to the adjusted CRQL

or the reported adjusted CRQL is approximate and may be inaccurate or imprecise.

R The sample results are unusable due to the quality of the data generated because

certain criteria were not met. The analyte may or may not be present in the sample.

Sampling Date:Receipt Date:Prep/Ext Date:Anal Date:

FPS-EU002- Client ID:Lab ID:Sample Size:Sample Type:Dilution factor:% moisture:

Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results FlagUnits: ng/Kg ng/Kg ng/Kg ng/Kg ng/Kg ng/Kg ng/Kg ng/KgPRL, ng/Kg

2,3,7,8-TCDD 1 0.22 J 0.22 0.6 0.6 10.8 10.8 11 11 9.9 9.9 0.31 0.31 0.32 0.32 24Total TCDD 0.34 100 2301,2,3,7,8-PeCDD 5 U 2.4 2.4 48.7 48.7 50.2 50.2 13 13 1.09 1.09 1.13 1.13 32Total PeCDD U 70 2101,2,3,4,7,8-HxCDD 5 U 2.4 0.24 50.4 5.04 52.1 5.21 5.3 0.53 1.09 0.109 1.14 0.114 161,2,3,6,7,8,-HxCDD 5 U 2.7 0.27 56.8 5.68 55.8 5.58 27 J 2.7 1.33 0.133 2.97 0.297 931,2,3,7,8,9-HxCDD 5 U 2.4 0.24 52.8 5.28 50.5 5.05 U R 1.16 0.116 1.32 0.132 U RTotal HxCDD U 160 4701,2,3,4,6,7,8-HpCDD 5 U R 2.6 0.026 50.8 0.508 51.8 0.518 620 J 6.2 6.59 0.066 50.91 0.509 1900 JTotal HpCDD U 1000 3200OCDD 10 1.3 J 4E-04 5.9 0.002 108.5 0.033 109.9 0.033 6000 J 1.8 58.93 0.018 393.19 0.118 18000 J2,3,7,8-TCDF 1 U 0.6 0.06 10.6 1.06 10.9 1.09 890 J 89 7.88 0.788 7.21 0.721 4800 JTotal TCDF U 2100 110001,2,3,7,8-PeCDF 5 U 2.8 0.084 58.5 1.755 58.3 1.749 270 J 8.1 3.29 0.099 4.63 0.139 1200 J2,3,4,7,8-PeCDF 5 U 2.7 0.81 55.4 16.62 56 16.8 460 J 138 4.65 1.395 4.44 1.332 2400 JTotal PeCDF U 1500 68001,2,3,4,7,8-HxCDF 5 U 2.7 0.27 54.1 5.41 54.3 5.43 240 J 24 2.89 0.289 3.54 0.354 1800 J1,2,3,6,7,8-HxCDF 5 U 2.6 0.26 56.6 5.66 58 5.8 89 8.9 1.82 0.182 2.02 0.202 4702,3,4,6,7,8-HxCDF 5 U 2.7 0.27 55.1 5.51 56.3 5.63 34 3.4 1.41 0.141 1.51 0.151 1801,2,3,7,8,9-HxCDF 5 U 2.5 0.25 55.4 5.54 56.9 5.69 74 7.4 1.63 0.163 1.68 0.168 410Total HxCDF U 780 45001,2,3,4,6,7,8-HpCDF 5 0.16 J 0.002 2.6 0.026 53.8 0.538 54.1 0.541 960 J 9.6 7.36 0.074 33.64 0.336 3500 J1,2,3,4,7,8,9-HpCDF 5 U 2.8 0.028 58.1 0.581 59.3 0.593 56 J 0.56 1.65 0.017 4.1 0.041 250Total HpCDF 0.16 21000 6800OCDF 10 U R 5.1 0.002 105.3 0.032 105.1 0.032 1600 J 0.48 17.32 0.005 150.74 0.045 4800 JCalc TEQ 0.222 5.837 118.7 120.9 323.6 4.994 6.11Reported Total TEQ 0.2 320

B = analyte detected in method blankE = conc exceeds calibration curveJ = positive identification, estimated concU = Not detected at or above RL

Lab: PACE Analytical

Case: 1-04/25/08-0027SDG: 1072204Site Name: Tittabawassee FloodplainUser: Weston

1 1

5/21/20085/24/2008

1Project-Specfic LCS

LCSD-16419F80523B_18

10.1 gLCSD

LCS-16418F80524A_01

10.5 gLCSMETHOD BLANK

1

5/21/20085/24/2008

ALCS-16417F80524A_04

10.3 g

5/21/20085/24/2008

BLANK-16416F80524A_06

10.1 g 11.6 g

B-048-01-0F8052

4/24/25/25/2

11.1

5/21/20085/24/2008

B-047-01-042208MSDF80524B_09

MATRIX SPIKE DUP

11.1

B-047-01-042208MSF80524B_08

MATRIX SPIKE11.3 g

5/21/20085/24/2008

11.11

4/22/20084/26/20085/21/20085/24/2008

B-047-01-042208F80524B_07

FIELD11.4 g

5/21/20085/24/2008

Page 1 of 3



Units:PRL, ng/Kg

2,3,7,8-TCDD 1Total TCDD1,2,3,7,8-PeCDD 5Total PeCDD1,2,3,4,7,8-HxCDD 51,2,3,6,7,8,-HxCDD 51,2,3,7,8,9-HxCDD 5Total HxCDD1,2,3,4,6,7,8-HpCDD 5Total HpCDDOCDD 102,3,7,8-TCDF 1Total TCDF1,2,3,7,8-PeCDF 52,3,4,7,8-PeCDF 5Total PeCDF1,2,3,4,7,8-HxCDF 51,2,3,6,7,8-HxCDF 52,3,4,6,7,8-HxCDF 51,2,3,7,8,9-HxCDF 5Total HxCDF1,2,3,4,6,7,8-HpCDF 51,2,3,4,7,8,9-HpCDF 5Total HpCDFOCDF 10Calc TEQReported Total TEQ

B = analyte detected in method blankE = conc exceeds calibration curveJ = positive identification, estimated conU = Not detected at or above RL



TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Resultsng/Kg ng/Kg ng/Kg ng/Kg ng/Kg ng/Kg ng/Kg ng/Kg

24 9.4 9.4 5.2 5.2 U R 0.49 J 0.49 4.8 4.8 U R 6.2 6.2 13110 74 4.3 5.3 39 89 81 210

32 U R U 9.9 9.9 U R 0.71 J 0.71 U R 83 83 13 13 2292 56 1.9 3.1 21 400 87 200

1.6 11 1.1 4.3 J 0.43 U R U R 2.1 J 0.21 35 3.5 6.4 0.64 U9.3 43 4.3 19 1.9 1.4 J 0.14 1.4 J 0.14 12 1.2 190 19 230 23 200

U R U R U R 0.98 J 0.098 U R U R U R 41240 110 10 11 66 1100 620 760

19 850 8.5 360 3.6 28 0.28 27 0.27 270 2.7 2800 J 28 9200 J 92 63001400 620 52 51 460 4800 15000 11000

5.4 9900 J 2.97 3400 J 1.02 260 0.078 230 0.069 2900 J 0.87 29000 J 8.7 83000 J 24.9 95000480 8400 J 840 1800 J 180 68 6.8 64 6.4 5100 J 510 11000 J 1100 1500 J 150 4100

17000 4000 170 170 11000 24000 3600 990036 3700 J 111 540 16.2 17 0.51 17 0.51 910 27.3 1700 J 51 790 23.7 2200

720 5100 J 1530 840 252 30 9 26 7.8 1900 J 570 3000 J 900 750 225 200014000 2600 97 85 4900 8500 2900 6500

180 2600 J 260 380 38 14 1.4 10 1 510 51 1400 J 140 680 68 170047 1000 100 140 14 4.9 J 0.49 3.6 J 0.36 200 20 500 50 170 17 29018 310 31 56 5.6 3 J 0.3 2.1 J 0.21 91 9.1 160 16 59 5.9 23041 1000 100 120 12 4.2 J 0.42 3.1 J 0.31 170 17 390 39 140 14 360

6600 1100 47 35 1300 4900 1800 570035 1900 J 19 770 7.7 44 0.44 28 0.28 700 7 8800 J 88 4600 J 46 20002.5 330 3.3 58 0.58 2.6 J 0.026 1.9 J 0.019 51 0.51 390 3.9 330 3.3 370

4000 1400 81 53 1300 16000 19000 150001.44 2500 J 0.75 940 0.282 57 0.017 41 0.012 790 0.237 10000 J 3 14000 J 4.2 17000

1652 3021 548.4 19.9 18.68 1222 2533 716.81700 3000 550 20 19 1200 2500 710

11.1 g 1.26 g 12.6 g1.18 g 1.03 g 10.9 g

B-054-

FIELD

17.4

4/22/20084/26/20085/21/20085/24/2008

B-054-01-042208F80524A_09

FIELD1

20.4

B-053-01-042208F80524A_08

FIELD1

4/22/20084/26/20085/21/20085/24/2008

5.2

4/22/20084/26/20085/21/20085/24/2008

B-052-01-042208F80524A_07

FIELD1

9.2

B-051-01-042308 DupF80523B_16

Lab Duplicate1

4/23/20084/26/20085/21/20085/23/2008

17

4/23/20084/26/20085/21/20085/23/2008

B-049-01-042308F80523B_13

FIELD1

15.1

04220823B_12

FIELD1

2/20086/20081/20083/2008

4/23/20084/26/20085/21/20085/23/2008

B-050-01-042308F80523B_14

12.8 gFIELD

B-051-01-042308F80523B_15

10.6 gFIELD

4/23/20084/26/20085/21/20085/23/2008

15.2

121.6

Page 2 of 3



Units:PRL, ng/Kg

2,3,7,8-TCDD 1Total TCDD1,2,3,7,8-PeCDD 5Total PeCDD1,2,3,4,7,8-HxCDD 51,2,3,6,7,8,-HxCDD 51,2,3,7,8,9-HxCDD 5Total HxCDD1,2,3,4,6,7,8-HpCDD 5Total HpCDDOCDD 102,3,7,8-TCDF 1Total TCDF1,2,3,7,8-PeCDF 52,3,4,7,8-PeCDF 5Total PeCDF1,2,3,4,7,8-HxCDF 51,2,3,6,7,8-HxCDF 52,3,4,6,7,8-HxCDF 51,2,3,7,8,9-HxCDF 5Total HxCDF1,2,3,4,6,7,8-HpCDF 51,2,3,4,7,8,9-HpCDF 5Total HpCDFOCDF 10Calc TEQReported Total TEQ

B = analyte detected in method blankE = conc exceeds calibration curveJ = positive identification, estimated conU = Not detected at or above RL



Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQ Results Flag TEQng/Kg ng/Kg ng/Kg ng/Kg ng/Kg ng/Kg ng/Kg

13 13 13 U R 12 12 23 23 5.8 5.8 2.2 2.2 1.6 1.6170 160 130 220 70 30 25

22 29 29 32 32 U R U R U R 3.9 J 3.9 3.2 J 3.2160 200 100 180 52 25 23

R 14 1.4 17 1.7 9 0.9 19 1.9 4.2 J 0.42 2.2 J 0.22 2.2 J 0.2220 56 5.6 60 6 41 4.1 90 9 19 1.9 7.3 0.73 8.8 0.884.1 U R U R U R U R U R U R U R

300 320 240 360 110 45 52J 63 1000 10 1100 J 11 790 7.9 1500 J 15 320 3.2 130 1.3 140 1.4

1700 1800 1400 2500 560 230 260J 28.5 12000 J 3.6 11000 J 3.3 9000 J 2.7 16000 J 4.8 3500 J 1.05 1200 0.36 1500 0.45J 410 4300 J 430 2500 J 250 7000 J 700 4400 J 440 7100 J 710 460 J 46 460 J 46

9500 5400 15000 9500 14000 950 960J 66 1200 J 36 860 25.8 2100 J 63 2400 J 72 3700 J 111 350 10.5 200 6J 600 2100 J 630 1300 J 390 3200 J 960 2300 J 690 3800 J 1140 320 96 240 72

6400 3900 6600 7700 11000 1000 760J 170 1200 J 120 690 69 690 69 1400 J 140 2300 J 230 260 26 170 17

29 360 36 240 24 510 51 430 43 650 65 72 7.2 43 4.323 150 15 97 9.7 170 17 190 19 230 23 25 2.5 20 236 310 31 200 20 440 44 410 41 600 60 68 6.8 39 3.9

3100 2200 2800 3600 4600 530 460J 20 2500 J 25 3100 J 31 1700 J 17 3700 J 37 1000 10 250 2.5 360 3.6

3.7 190 1.9 130 1.3 170 1.7 280 2.8 180 1.8 29 0.29 23 0.234700 5300 3500 6900 2000 470 640

J 5.1 3100 J 0.93 3100 J 0.93 2100 J 0.63 5000 J 1.5 1100 0.33 290 0.087 390 0.1171513 1388 875.7 1951 1540 2364 206.6 162.91500 1400 870 2000 1500 2400 210 160

11.8 g11 g 0.56 g 12.9 g 12.6 g1.04 g

17.4

4/24/20084/26/20085/21/20085/24/2008

B-061-01-042408F80524B_06

FIELD1

13.9

B-060-01-042208F80524A_16

FIELD1

4/22/20084/26/20085/21/20085/24/2008

20.8

4/22/20084/26/20085/21/20085/24/2008

B-059-01-042208F80524A_15

FIELD1

22.4

B-058-01-042208F80524A_14

FIELD1

4/22/20084/26/20085/21/20085/24/2008

23.5

4/23/20084/26/20085/21/20085/24/2008

B-057-01-042308F80524A_13

FIELD1

7.7

B-056-01-042308F80524A_12

FIELD1

1.02 g

4/23/20084/26/20085/21/20085/24/2008

20.9

4/23/20084/26/20085/21/20085/24/2008

B-055-01-042308F80524A_11

FIELD1

17.4

-01-042208DF80528A_17

DUPLICATE1

1.19 g

4/22/20084/26/20085/21/20085/29/2008

Page 3 of 3

DATA VALIDATION REPORT

Tittabawassee River Residential Floodplain Sampling

SAMPLE DELIVERY GROUP: G8D300294

Prepared by

MECX, LP

12269 East Vassar Drive Aurora, CO 80014

Project: Tittabawassee

DATA VALIDATION REPORT SDG: G8D300294

1 Revision 0

I. INTRODUCTION Task Order Title: Tittabawassee River Residential Floodplain

Sampling Contract Task Order: 1303.001D.02 Sample Delivery Group: G8D300294 Project Manager: T. Balla Matrix: Soil QC Level: IV No. of Samples: 20 No. of Reanalyses/Dilutions: 0 Laboratory: Test America – West Sacramento, California

Table 1. Sample Identification

Client ID Laboratory ID Collected Method

FPS-EU002-D-018-01-042508 G8D300294-001 04/25/2008 1613B

FPS-EU002-D-019-01-042408 G8D300294-002 04/24/2008 1613B

FPS-EU002-D-020-01-042408 G8D300294-003 04/24/2008 1613B

FPS-EU002-D-021-01-042408 G8D300294-004 04/24/2008 1613B

FPS-EU002-D-022-01-042508 G8D300294-005 04/25/2008 1613B

FPS-EU002-D-023-01-042508 G8D300294-006 04/25/2008 1613B

FPS-EU002-D-023-01-042508D G8D300294-007 04/25/2008 1613B

FPS-EU002-D-024-01-042508 G8D300294-008 04/25/2008 1613B

FPS-EU002-D-025-01-042408 G8D300294-009 04/24/2008 1613B

FPS-EU002-D-026-01-042508 G8D300294-010 04/25/2008 1613B

FPS-EU002-D-027-01-042508 G8D300294-011 04/25/2008 1613B

FPS-EU002-D-028-01-042508 G8D300294-012 04/25/2008 1613B

FPS-EU002-D-029-01-042508 G8D300294-013 04/25/2008 1613B

FPS-EU002-D-030-01-042408 G8D300294-014 04/24/2008 1613B



2 Revision 0

Client ID Laboratory ID Collected Method

FPS-EU002-D-031-01-042508 G8D300294-015 04/25/2008 1613B

FPS-EU002-D-032-01-042508 G8D300294-016 04/25/2008 1613B

FPS-EU002-D-033-01-042508 G8D300294-017 04/25/2008 1613B

FPS-EU002-D-033-01-042508D G8D300294-018 04/25/2008 1613B

FPS-EU002-D-034-01-042508 G8D300294-019 04/25/2008 1613B

FPS-EU002-D-035-01-042508 G8D300294-020 04/25/2008 1613B

II. Sample Management

No anomalies were observed regarding sample management. The samples in this SDG were

received at TestAmerica – West Sacramento below the temperature limits of 4°C ±2°C; however,

as the temperature was above 0 the data was not qualified. According to the sample receipt

checklist and case narrative for this SDG, one sample was received with a cracked lid. As no

notation was made of the sample leaking from the container, no qualification of the sample was

deemed necessary. All other samples were received intact at the laboratory. All COCs were

appropriately signed and dated by field and/or laboratory personnel. Custody seals were intact

upon arrival at Test America.



3 Revision 0

Data Qualifier Reference Table

Qualifier Organics Inorganics

U The analyte was analyzed for, but was

not detected above the reported sample quantitation limit. The associated value is the quantitation limit or the estimated detection limit for dioxins.

The material was analyzed for, but was not detected above the level of the associated value. The associated value is either the sample quantitation limit or the sample detection limit. The associated value is the sample detection limit or the quantitation limit for perchlorate only.

J The analyte was positively identified; the associated numerical value is the approximate concentration of the analyte in the sample.

The associated value is an estimated quantity.

N The analysis indicates the presence of an analyte for which there is presumptive evidence to make a "tentative identification."

Not applicable.

NJ The analysis indicates the presence of an analyte that has been "tentatively identified" and the associated numerical value represents its approximate concentration.

Not applicable.

UJ The analyte was not deemed above the reported sample quantitation limit. However, the reported quantitation limit is approximate and may or may not represent the actual limit of quantitation necessary to accurately and precisely measure the analyte in the sample.

The material was analyzed for, but was not detected. The associated value is an estimate and may be inaccurate or imprecise.

R The data are unusable. The sample results are rejected due to serious deficiencies in the ability to analyze the sample and to meet quality control criteria. The presence or absence of the analyte cannot be verified.

The data are unusable. The sample results are rejected due to serious deficiencies in the ability to analyze the sample and to meet quality control criteria. The presence or absence of the analyte cannot be verified.



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III. Method Analyses

A. EPA METHOD 1613—Dioxin/Furans

Reviewed By: E. Wessling

Date Reviewed: June 16, 2008

The samples listed in Table 1 for this analysis were validated based on the guidelines outlined in

the MECX Data Validation Procedure for Dioxins and Furans (DVP-19, Rev. 0), USEPA Method

1613, and the National Functional Guidelines Chlorinated Dioxin/Furan Data Review (9/05).

• Holding Times: Extraction and analytical holding times were met. The samples were

stored in the dark at 4°C ±2°C and extracted and analyzed within one year of collection.

• Instrument Performance: Instrument performance criteria were met. Following are

findings associated with instrument performance:

o GC Column Performance: A Windows Defining Mix (WDM) containing the first

and last eluting congeners of each descriptor and isomer specificity compounds

was not analyzed prior to the initial calibration sequence or at the beginning of

each analytical sequence. The GC column performance in the calibrations was

acceptable, with the height of the valley between the closely eluting isomers and

2,3,7,8-TCDD reported as less than 25%.

o Mass Spectrometer Performance: The mass spectrometer performance was

acceptable with the static resolving power greater than 10,000.

• Calibration: Calibration criteria were met.

o Initial Calibration: Initial calibration criteria were met. The initial calibration was

acceptable with %RSDs ≤20% for the 15 native compounds (calibration by isotope

dilution) and ≤35% for the two native and all labeled compounds (calibration by

internal standard). The relative retention times and ion abundance ratios were

within the Method 1613 QC limits for all standards.

o Continuing Calibration: Calibration verification (VER) consisted of a mid-level

standard (CS3) and window defining mixture (WDM) DB-5 CPSM analyzed at the

beginning of each analytical sequence. The VERs were acceptable with the

concentrations within the acceptance criteria listed in Table 6 of EPA Method 1613.

The ion abundance ratios and relative retention times were within the method QC

limits.

• Blanks: Method blanks, “KWMR1AA and KMWMR1AG” were free from target compound

detects and no qualifications of the site samples were required. Two method blanks were



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generated as the site samples were processed through the clean-up at different times.

The site samples were associated with the method blank which accompanied them during

the clean-up.

• Blank Spikes and Laboratory Control Samples: Two sets of LCS/LCSD samples and two

low-level blank spike were extracted and analyzed with the samples of this SDG. All LCS

recoveries and RPDs were within were within the acceptance criteria listed in Table 6 of

Method 1613 and laboratory-established control limits. The sensitivity checks, low-level

blank spikes showed recoveries with ±40% for all compounds. The site samples were

associated with the LCS/LCSD and sensitivity check which accompanied the site samples

during the clean-up.

• Matrix Spike/Matrix Spike Duplicate: An MS/MSD pair was analyzed in association with

this SDG. Sample FPS-EU002-D-022-01-042408 contained 4 target compounds where

the recoveries and/or RPDs exceeded the laboratory-established acceptance criteria.

These target compounds; 1,2,3,4,7,8,-HxCDD, 1,2,3,4,6,7,8-HpCDD, 1,2,3,4,6,7,8-

HpCDF and OCDF; were qualified as estimated, “J,” for detects and “UJ,” for nondetects

in the parent sample. For several additional compounds, the amount of target compound

in the native samples was greater than 4 times the amount spiked and recovery was not

evaluated. No further qualifications were required.

• Duplicate Analyses: Following are the findings associated with Duplicate analyses:

o Laboratory Duplicates: The laboratory analyzed sample FPS-EU002-D-020-01-

042408 as a laboratory duplicate analyses. The RPDs exceeded the laboratory-

established limits of 25% for and Total PeCDD, Total HxCDD, 1,2,3,7,8,9-HxCDF.

These target compounds in the parent sample were qualified as estimated, “J,” for

the exceedance. The laboratory duplicate pairs also contained occurrences of low-

level detects which were nondetect in the one of the pair. Since the detects were

near the detection limits, no qualifications were deemed necessary.

o Field Duplicates: There were two field duplicate pairs analyzed in this SDG, FPS-

EU002-D-023-01-042508/FPS-EU002-D-023-01-042508D and FPS-EU002-D-033-

01-042508/FPS-EU002-D-033-01-042508D. The RPDs in duplicate pair FPS-

EU002-D-023-01-042508/FPS-EU002-D-023-01-042508D exceeded the QC limits

established in the QAPP of 50% for Total PeCDD, 2,3,4,6,7,8-HxCDD, both

HpCDF isomers, Total HpCDF, and OCDF. The RPDs in duplicate pair FPS-

EU002-D-033-01-042508/FPS-EU002-D-033-01-042508D exceeded the QC limits

established in the QAPP of 50% for Total PeCDD, 2,3,7,8-TCDF, Total TCDF,

1,2,3,7,8-PeCDF, Total PeCDF and 1,2,3,7,8,9-HxCDF. These target compounds

in the respective site sample and duplicate were qualified as estimated, “J,” for the

exceedance. The field duplicate pairs also contained occurrences of low-level

detects which were nondetect in one of the pair. Since the detects were near the

detection limits, no qualifications were deemed necessary.

• Internal Standards Performance: The labeled standard recoveries were within the



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acceptance criteria listed in Table 7 of Method 1613B with the exception of 13C-1,2,3,

4,7,8-HxCDD in sample FPS-EU002-D-019-01-042408, 8 labeled internal standards in

FPS-EU002-D-022-01-042408, 13C-1,2,3,4,7,8-HxCDD in FPS-EU002-D-023-01-042408

and 13C-1,2,3,4,7,8-HxCDF in FPS-EU002-D-026-01-042508. The associated native

isomer in the site sample was qualified as estimated, “J,” in the aforementioned samples.

13C-1,2,3,6,7,8-HxCDF in sample FPS-EU002-D-029-01-042508 did not meet the ion

abundance criteria. The laboratory calculated the target compound concentrations

using an area response consistent with a theoretical ion abundance for the labeled

isomer. The reviewer qualified the associated target compounds in the site samples as

estimated, “J.”

• Compound Identification: Compound identification was verified. The RRTs for the

2,3,7,8-substituted compounds were within the windows. The SICPs maximized within 2

seconds for the quantitation ions. The S/N ratio was greater than 2.5 to 1. The ion

abundance ratios were within the criteria specified in Table 9 of Method 1613B. The

laboratory analyzed for polychlorinated dioxins/furans by EPA Method 1613B. Target

compound 2,3,7,8-TCDD in sample FPS-EU002-D-018-01-042408 did not meet ion

abundance criteria for identification. The laboratory reported this isomer as an EMPC with

the designation on the sample result form of “JA.” The reviewer qualified the 2,3,7,8-

TCDD as an estimated nondetect, “UJ,” in the site sample. No further qualifications were

noted.

• Compound Quantification and Reported Detection Limits: Compound quantitation was

verified by recalculating a representative number of sample detects and blank spike

concentrations. Manual integrations were deemed appropriate by the reviewer.

Confirmation was performed for 2,3,7,8-TCDF detects as the primary column did not

meet the resolution criteria. The laboratory calculated and reported compound-specific

detection limits, EDLs. Any detects below the laboratory lower calibration level were

qualified as estimated, “J.” Nondetects are valid to the detection limit calculated by the

laboratory. This detection limit is not based upon overall signal to noise within the

retention time widow but rather a peak within the window; therefore, it is not a true

estimated detection limit, (EDL) as defined by the method.

2,3,7,8-TCDF in samples FPS-EU002-D-019-01-042408, FPS-EU002-D-020-01-042408,

FPS-EU002-D-022-01-042408, FPS-EU002-D-023-01-042508, FPS-EU002-D-023-01-

042508D, FPS-EU002-D-025-01-042408, FPS-EU002-D-026-01-042508, FPS-EU002-D-

029-01-042508 and FPS-EU002-D-032-01-042508 were reported above the linear range

of the confirmation instrument. This compound was qualified as estimated, “J,” in the

aforementioned site samples.

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