Method 8276 

Technical Toxaphene and Toxaphene Congeners by Gas Chromatography – 

Negative Ion Chemical Ionization/Mass Spectroscopy (GC-NICI/MS) 

U.S. EPA Office of Resource Conservation and Recovery 

Inter-laboratory Validation Study for Fish Tissue 

ANALYTICAL DATA REPORT 

August 2012 

Submitted to: 

U. S. Environmental Protection Agency 

Office of Resource Conservation and Recovery 

1200 Pennsylvania Avenue, NW 

Washington, DC 20460 

Submitted by: 

TechLaw, Inc. 

14500 Avion Parkway, Suite 300 

Chantilly, VA 20151 

EPA Contract No. GS-10F-0168J 
TABLE OF CONTENTS 

I. Introduction ............................................................................................................................................ 1 . 

II. Phase III Study Design ........................................................................................................................... 2 

III. Analytical Data ....................................................................................................................................... 3 

IV. Z-Scores.................................................................................................................................................. 3 

TABLES 

Table 1: Analytes of Interest ........................................................................................................... 1 

Table 2: Inter-laboratory Validation Study Design for Method 8276 for Fish Tissue .................... 2 

Attachment 1 – Summarized Analytical Data for Fish Tissue Extracts and Laboratory Quality Control 

Samples 

Table A1-1: Phase III Multi-laboratory Validation Data for Fish Samples at Terry Creek 

Table A1-2: Phase III Multi-laboratory Validation Data Using Spiked Laboratory Quality Control 

Samples Carried through Extraction and Clean-up 

Attachment 2 – Final Phase III Toxaphene Data Tables 

Table A2-1: Technical Toxaphene in Alaskan Cod Fish 

Table A2-2: Toxaphene Congeners in Alaskan Cod Source Fish 

Table A2-3: Technical Toxaphene in Terry Creek Fish Samples 

Table A2-3-1: Technical Toxaphene in Mass Units in Terry Creek Fish Samples 

Table A2-4: Toxaphene Congeners in Terry Creek Fish Samples 

Table A2-4-1: Toxaphene Congeners in Mass Units in Terry Creek Fish Samples 

Table A2-5: Technical Toxaphene Second Source Standard

Table A2-6: Technical Toxaphene in Laboratory Quality Control Samples 

Table A2-7: Toxaphene Congeners in Laboratory Quality Control Samples

Table A2-8: Quality Control Samples: Matrix Spike/Matrix Spike Duplicate for Technical 

Toxaphene

Table A2-9: Quality Control Samples: Matrix Spike/Matrix Spike Duplicate for Toxaphene 

Congeners

Table A2-10: Laboratory Participants 
TABLE OF CONTENTS (cont) 

Attachment 3 – Final Phase III Toxaphene Summary Results with Z Values 

Table A3-1: Z-Scores for Laboratory Quality Assurance Samples
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		 August	2012	

Analytical	Data	Report	    

1

I. Introduction

SW-846 Method 8276 is presently under development for the analysis of technical toxaphene 

and toxaphene congeners using gas chromatography-negative ion chemical ionization mass 

spectrometry (GC-NICI/MS). Phase I and Phase II of the Method 8276 validation studies were 

conducted in 2008 and 2009. The first performance studies were completed using analytical 

standards only. Subsequent studies were conducted to evaluate the method for analysis of water, 

soil, and sediment matrices. The purpose of this current Phase III Inter-laboratory Validation 

Study is to evaluate the use of Method 8276 for the analysis of technical toxaphene and 

toxaphene congeners in fish tissue extracts. Data produced by the laboratory participants were 

evaluated to determine reliability, reproducibility, linearity, accuracy and precision of the 

method. This information was then used to establish method precision and bias for fish tissue 

using Method 8276. The compounds listed in Table 1 were included in the Phase III study. 

Table 2 provides information regarding the study design. 

Table 1. Analytes of Interest 

COMPOUND CAS Registry No

technical toxaphene 8001-35-2 

toxaphene congeners 

2-exo,3-endo,6-exo,8,9,10-Hexachlorobornane (Hx-Sed) 57981-29-0 

2-endo,3-exo,5-endo,6-exo,8,9,10-Heptachlorobornane (Hp-Sed) 70649-42-2 

2-endo,3-exo,5-endo,6-exo,8,8,10,10-Octachlorobornane (P26) 142534-71-2 

2-endo,3-exo,5-endo,6-exo,8,9,10,10-Octachlorobornane (P40) 166021-27-8 

2-exo,3-endo,5-exo,8,9,9,10,10-Octachlorobornane (P41) 165820-16-6 

2-exo,5,5,8,9,9,10,10-Octachlorobornane (P44) 165820-17-7 

2-endo,3-exo,5-endo,6-exo,8,8,9,10,10-Nonachlorobornane (P50) 6680-80-8 

2,2,5,5,8,9,9,10,10-Nonachlorobornane (P62) 154159-06-5 

The EPA Region 4 Laboratory completed all extraction, cleanup, concentration, and spiking as 

necessary for sample matrices. An EPA Region 4 laboratory chemist served as referee and 

conducted confirmation testing for all spiked laboratory quality control (QC) samples and fish 

extracts before shipping to participating laboratories for analysis. With the exception of the 

referee chemist, none of the laboratory participants knew the concentrations of the prepared 

laboratory QC samples and fish extracts. Each laboratory was responsible for conforming to 

study instructions and the QC parameters recommended in Method 8276 (March 2010, Revision 

0). Participating laboratories were also asked to complete a questionnaire and provide comments 

that would be helpful for further development of Method 8276. 
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		 August	2012	

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The following laboratories participated in Phase III of this study: 

Ashland (formerly Hercules), 

EPA National Enforcement Investigation Center (NEIC), 

EPA Office of Research Development Las Vegas, Analyst 1, 

EPA Office of Research Development Las Vegas, Analyst 2, 

EPA Region 4 Lab, Analyst 1*, 

EPA Region 4 Lab, Analyst 2, 

EPA Region 4 Lab, Analyst 3, and 

Southern California Coastal Water Research Project (SCCWRP) 

*Referee 

II. Phase III Study Design 

Table 2. Inter-laboratory Validation Study Design for Method 8276 for Fish Tissue 

Method 8276 Phase III Study Design 

Sample Matrices Surrogates8

(pg/uL) 

 Internal 

Std9 

(pg/uL) 

Technical 

Toxaphene 

Spike 

Conc.10 

(pg/uL) 

Congener 

Spike 

Conc.10 

(pg/uL) 

Min No. of 

both 

Analyses 

Total Min 

No. of 

Analyses 

Total 

No. of 

Vials 

PCB 209 

ε-HCH

PCB 204 

Calibration Stds 20-160 50-400 50 50-400 1-500 1 13 13 

Second-source Std11 100 250 50 150 NA 2 2 1 

ORS1 50 NA NA 1 1 1 

MB2 100 250 50 NA NA 2 4 1 

LCS13 100 250 50 Unk Unk 2 4 2 

Source Fish Matrix4 100 250 50 NA NA 2 4 1 

LCS2 5 100 250 50 Unk Unk 2 4 2 

MS/MSD6 100 250 50 Unk Unk 2 8 4 

Terry Creek 17 100 250 50 NA NA 2 4 2 

Terry Creek 27 100 250 50 NA NA 2 4 2 

Total 48 29 

1

ORS - Oxygen Reaction Standard – Analyzed daily to demonstrate the absence of oxygen so that PCBs do not 

constitute an interference concern for toxaphene ions. See Method 8276 for details. 

2

MB - Method Blank: Hydromatrix® and sand spiked with surrogates, carried through extraction and clean-up. 

3

LCS1 - Laboratory Control Sample – Hydromatrix® and sand spiked with surrogates and either toxaphene 

congeners or technical toxaphene and carried through extraction and clean-up. 

4

Source fish matrix – Alaskan cod purchased at a local grocery store and determined to be free from toxaphene 

congener contamination prior to its use. The fish was spiked with surrogates and carried through extraction and 

clean-up. 
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		 August	2012	

Analytical	Data	Report	    

3

5

LCS2 - LCS spiked with surrogates and either toxaphene congeners or technical toxaphene at a different 

concentration than the LCS1 and carried through extraction and clean-up. 

6

MS/MSD - Matrix Spike/Matrix Spike Duplicate: Source fish matrix spiked with surrogates and either toxaphene 

congeners or technical toxaphene and carried through extraction and clean-up. 

7

Terry Creek 1 and 2 - Fish collected from Terry Creek from the toxaphene plant with incurred residues spiked with 

surrogates and carried through extraction and clean-up. 

8 Surrogate compounds were spiked prior to extraction to evaluate overall efficiency. 

9 Internal standard (PCB 204) was spiked into the final extract at the conclusion of extraction and cleanup. 

10 Technical toxaphene and the toxaphene congeners were spiked separately into the calibration standards, 

LCS1/LCS2, and MS/MSD samples. 

11 The second-source standard contains technical toxaphene only. 

Technical toxaphene calibration range: 50 - 400 pg/uL 

Toxaphene congener calibration range: 1.0 - 500 pg/uL, except for Parlar 62: 5.0 – 500 pg/uL. 

III. Analytical Data 

The technical toxaphene and toxaphene congeners detected in fish extracts from the Phase III 

Study are summarized in Attachment 1 and Attachment 2. 

IV. Z-Scores

Z-scores, provided in Attachment 3, were generated for each quality control sample and 

averaged for each laboratory participant. In accordance with International Union of Pure and 

Applied Chemistry (IUPAC) 1993 guidance, Z-scores can be used as indicators of accuracy in 

laboratory inter-comparison studies and reflect the difference between a laboratory result and a 

target value or performance criterion. Z-scores are calculated using the following formula: 

Z-score = (laboratory estimate)/(performance criterion) = (x - X)/σ

where x is the individual laboratory analytical result, X is the “exercise assigned value,” and σ is 

the established target value or criterion. Z-scores for this study were calculated using an exercise 

assigned value equal to the average recovery (for each replicate) for each quality control sample 

(i.e., MS, MSD, LCS1, LCS2 and Second Source Standard). A fixed performance criterion for 

each analyte for each laboratory was calculated using 25% of the exercise assigned value (σ = 

0.25 * X), yielding the following: 

Z-score = (laboratory analytical result – average recovery) / (25% average recovery) 
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		 August	2012	

Analytical	Data	Report	    

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Z-scores that have been calculated for this study can be interpreted in the following way: 

 A value of +1 indicates the laboratory result is 25% higher than the exercise assigned 

value. 

 A value of -1 indicates the laboratory result is 25% lower than the exercise assigned 

value. 

 A value of +2 indicates the laboratory result is 50% higher than the exercise assigned 

value. 

 A value of -2 indicates the laboratory result if 50% lower than the exercise assigned 

value. 

An accepted approach to classifying and categorizing Z-scores includes the following (IUPAC 

1993): 

 |z| ≤ 2  Satisfactory 

 2< |z| < 3  Questionable 

 |z| ≥ 3  Unsatisfactory 
Attachment 1 

Summarized Analytical Data for Fish Tissue Extracts and 

Laboratory Quality Control Samples 
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		 August	2012	

Analytical	Data	Report	 	 Attachment	1	

			

	 	

Table A1-1 

PHASE III MULTI-LABORATORY VALIDATION DATA USING FISH SAMPLES COLLECTED 

FROM TERRY CREEK IN BRUNSWICK, GEORGIA WITH EXTRACTS SUBJECTED TO 

CLEANUP1

Toxaphene 

ID No. of 

Participants 

Grand Mean 

(ug/kg) 

Std. 

Deviation 

Reproducibility 

% RSD 

TC 1 8 7030 1170 16.7 

TC 2 8 650 112 17.2 

Hp-Sed 

ID No. of 

Participants 

Grand Mean 

(ug/kg ) 

Std. 

Deviation 

Reproducibility 

% RSD 

TC1 8 184 10.3 5.59 

TC2 8 15.1 0.963 6.37 

P26

ID No. of 

Participants 

Grand Mean 

(ug/kg ) 

Std. 

Deviation 

Reproducibility 

% RSD 

TC1 8 16.0 0.738 4.62 

TC2 8 2.32 0.063 2.71 

Hx-Sed 

ID No. of 

Participants 

Grand Mean 

(ug/kg ) 

Std. 

Deviation 

Reproducibility 

% RSD 

TC1 8 160 10.7 6.65 

TC2 8 10.8 0.84 7.75 
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		 August	2012	

Analytical	Data	Report	 	 Attachment	1	

			

	 	

Table A1-1 (cont.) 

P40 

ID No. of 

Participants 

Grand Mean 

(ug/kg) 

Std. 

Deviation 

Reproducibility 

% RSD 

TC1 8 21.8 2.05 9.37 

TC2 8 2.49 0.114 4.57 

 

P41

ID No. of 

Participants 

Grand Mean 

(ug/kg ) 

Std. 

Deviation 

Reproducibility 

% RSD 

TC1 8 8.93 0.322 3.60 

TC2 8 1.05 0.027 2.53 

P44

ID No. of 

Participants 

Grand Mean 

(ug/kg ) 

Std. 

Deviation 

Reproducibility 

% RSD 

TC1 8 9.53 0.693 7.28 

TC2 8 1.34 0.099 7.40 

P50

ID No. of 

Participants 

Grand Mean 

(ug/kg ) 

Std. 

Deviation 

Reproducibility 

% RSD 

TC1 8 16.5 1.20 7.25 

TC2 8 2.57 0.125 4.87 

P62 

ID No. of Participants Grand Mean 

(ug/kg) 

Std. 

Deviation 

Reproducibility 

% RSD 

TC1 8 22.3 7.01 31.5 

TC2 8 3.07 1.02 33.3 

1

Samples were extracted in hexane in an Accelerated Solvent Extractor (ASE) using a modified version of Method 

3545A with a sample mass of 10 g of solid material (Ottawa sand). In-cell cleanup was done in the ASE extraction 

cell using activated, acidified (30% H2SO4) silica gel per Method 3665A and Method 3630C. These extracts were 

further subjected to cleanup using a Florisil® cartridge (1% deactivated with DI water) approach according to Method 

3620C. The sample was in hexane throughout the process and was concentrated to a final extract volume of 1 mL. 
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		 August	2012	

Analytical	Data	Report	 	 Attachment	1	

			

	 	

Table A1-2 

PHASE III MULTI-LABORATORY VALIDATION DATA USING SPIKED LABORATORY 

QUALITY CONTROL SAMPLES CARRIED THROUGH EXTRACTION AND CLEANUP1

Technical Toxaphene 

ID No. of 

Participants 

True 

Value 

(pg/μL) 

Grand 

Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

(% RSD) 

Second Source 

Standard 8 150 159 106 9.90 6.20 

LCS 1 8 50 57.3 115 9.74 16.9 

LCS 2 8 200 207 104 13.5 6.50 

PCB 209 LCS1 8 100 95.0 95.0 1.93 2.03 

ε-HCH LCS 1 8 250 231 92.2 21.0 9.10 

PCB 209 LCS2 8 100 90.2 90.2 5.36 5.95 

ε-HCH LCS2 8 250 240 95.8 15.5 6.46 

Hx-Sed 

ID No. of 

Participants 

True Value 

(pg/μL) 

Grand Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

(% RSD) 

LCS1 8 100 98.4 98.4 5.84 5.94 

LCS2 8 2 1.95 97.4 0.16 8.00 

Hp-Sed 

ID No. of 

Participants 

True Value 

(pg/μL) 

Grand Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

 (% RSD) 

LCS1 8 100 98.9 98.9 5.77 5.84 

LCS2 8 2 1.99 99.3 0.13 6.30 

P26 

ID No. of 

Participants 

True Value 

(pg/μL) 

Grand Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

(% RSD) 

LCS1 8 100 97.9 97.9 5.27 5.39 

LCS2 8 2 1.83 91.4 0.36 19.7 
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		 August	2012	

Analytical	Data	Report	 	 Attachment	1	

			

	 	

Table A1-2 (cont.) 

P40 

ID No. of 

Participants 

True Value 

(pg/μL) 

Grand Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

(% RSD) 

LCS1 8 100 98.1 98.1 6.33 6.45 

LCS2 8 2 1.94 97.2 0.15 7.46 

P41 

ID No. of 

Participants 

True Value 

(pg/μL) 

Grand Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

 (% RSD) 

LCS1 8 100 98.6 98.6 6.31 6.40 

LCS2 8 2 2.03 102 0.17 8.32 

P44 

ID No. of 

Participants 

True Value 

(pg/μL) 

Grand Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

(RSD) 

LCS1 8 100 99.4 99.4 8.85 8.91 

LCS2 8 2 1.99 99.7 0.16 8.09 

P50 

ID No. of 

Participants 

True Value 

(pg/μL) 

Grand Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

(% RSD) 

LCS1 8 100 96.9 96.9 7.47 7.71 

LCS2 8 2 2.01 101 0.07 3.55 

P62 

ID No. of 

Participants 

True Value 

(pg/μL) 

Grand Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

(% RSD) 

LCS1 8 226 237 105 26.0 11.0 

LCS2 8 22.6 21.0 92.9 4.51 21.5 
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		 August	2012	

Analytical	Data	Report	 	 Attachment	1	

			

	 	

Table A1-2 (cont.) 

Congeners - PCB 209

ID No. of 

Participants 

True Value 

(pg/μL) 

Grand Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

(% RSD) 

LCS1 8 100 95.1 95.1 5.13 5.39 

LCS2 8 100 94.9 94.9 5.55 5.85 

Congeners – ε-HCH

ID No. of 

Participants 

True Value 

(pg/μL) 

Grand Mean 

(pg/μL) 

% 

Recovery 

Std. 

Deviation 

Reproducibility 

(% RSD) 

LCS1 8 250 248 99.0 11.7 4.72 

LCS2 8 250 247 98.9 7.84 3.17 

1

Samples were extracted in hexane in an Accelerated Solvent Extractor (ASE) using a modified version 

of Method 3545A with a sample mass of 10 g of solid material (Ottawa sand). In-cell cleanup was done 

in the ASE extraction cell using activated, acidified (30% H2SO4) silica gel per Method 3665A and 

Method 3630C. These extracts were further subjected to cleanup using a Florisil® cartridge (1% 

deactivated with DI water) approach according to Method 3620C. The sample was in hexane throughout 

the process and was concentrated to a final extract volume of 1 mL. 
Attachment 2 

Final Phase III Toxaphene Data Tables 
Table A2‐1  ‐ Technical Toxaphene in Alaskan Cod Source Fish

Laboratory Replicate Toxaphene

PCB 209

(spiked at 100)

eHCH

(spiked at 250) PCB 209 eHCH PCB 209 eHCH 

ASHLAND 1 11.2 77.4 269 77.4 108 75.7 280 

ASHLAND 2 9.50 74.0 292 74.0 117

EPA_ NEIC 1 46.3 84.8 243 84.8 97.0 84.3 246 EPA_ NEIC 2 38.2 83.8 250 83.8 100

EPA_R4_1 1 21.8 66.8 245 66.8 98.1 76.0 238 EPA_R4_1 2 14.3 80.1 233 80.1 93.4EPA_R4_1 3 16.8 81.2 234 81.2 93.7EPA_R4_2 1 12.1 77.3 231 77.3 92.3 78.2 229 EPA_R4_2 2 14.6 79.2 227 79.2 90.7EPA_R4_3 1 9.18 80.0 236 80.0 94.5 79.1 237 EPA_R4_3 2 8.63 78.1 237 78.1 94.8

SCCWRP 1 4.70 83.7 232 83.7 92.8 83.3 227 SCCWRP 2 3.70 81.3 224 81.3 89.6SCCWRP 3 3.50 84.8 225 84.8 90.0

EPA_NERL/ORD_LV_1 1 ND 80.4 233 80.4 93.4 79.9 227 EPA_NERL/ORD_LV_1 2 17.5 79.4 221 79.4 88.5EPA_NERL/ORD_LV_2 1 35.2 88.2 233 88.2 93.0 88.2 234 EPA_NERL/ORD_LV_2 2 30.4 88.1 235 88.1 94.1

Highlighted cells have concentrations below the LLOQ of 50 pg/μL.

Note: The Alaskan Cod Source Fish is a clean matrix.

Concentration (pg/μL) % Recovery Avg Concentration (pg/μL

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐2 ‐ Toxaphene Congeners in Alaskan Cod Source Fish

Laboratory Rep Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 

ASHLAND 1 ND ND ND ND ND ND ND ASHLAND 2 ND ND 0.200 ND ND ND ND 

EPA_ NEIC 1 <0.0800 <0.200 <0.300 <0.0800 <0.0600 <0.200 <0.100 

EPA_ NEIC 2 <0.0800 <0.200 <0.300 <0.0800 <0.0600 <0.200 <0.100 

EPA_R4_1 1 0.0300 0.0500 0.280 0.0300 0.0600 0.0400 0.170 EPA_R4_1 2 0.0300 0.0400 0.320 0.0500 0.0700 0.0600 0.180 EPA_R4_1 3 0.0400 0.0700 0.240 0.0200 0.0700 0.0900 0.220 EPA_R4_2 1 ND ND ND ND ND ND ND EPA_R4_2 2 ND ND ND ND ND ND ND EPA_R4_3 1 ND ND ND ND ND ND ND EPA_R4_3 2 ND ND ND ND ND ND ND 

SCCWRP 1 ND ND 0.140 ND ND ND 0.160 SCCWRP 2 ND ND 0.280 ND ND ND 0.190 SCCWRP 3 ND ND 0.260 ND ND ND 0.160 

EPA_NERL/ORD_LV_1 1 0.360 0.270 1.26 0.580 0.720 0.820 0.700 

EPA_NERL/ORD_LV_1 2 0.320 0.270 0.930 0.580 0.660 0.810 0.720 

EPA_NERL/ORD_LV_2 1 ND ND ND ND ND 0.340 0.550 

EPA_NERL/ORD_LV_2 2 ND ND ND ND 0.190 ND 0.560 

Highlighted cells have concentrations below the LLOQ of

1 pg/μL for Hx‐Sed, Hp_Sed, P26, P40, P41, P44, and P50

or 5 pg/μL for P62.

Concentration (pg/μL)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐2 ‐ Toxaphene Congeners in Alaskan Cod Source Fish

Laboratory Rep

ASHLAND 1ASHLAND 2

EPA_ NEIC 1

EPA_ NEIC 2

EPA_R4_1 1EPA_R4_1 2EPA_R4_1 3EPA_R4_2 1EPA_R4_2 2EPA_R4_3 1EPA_R4_3 2

SCCWRP 1SCCWRP 2SCCWRP 3

EPA_NERL/ORD_LV_1 1

EPA_NERL/ORD_LV_1 2

EPA_NERL/ORD_LV_2 1EPA_NERL/ORD_LV_2 2

PCB 209 (spiked @ 100) eHCH (spiked @ 250) PCB 209 eHCH PCB 209 eHC

71.9 262 71.9 105 71.8 2671.7 270 71.7 10885.3 247 85.3 98.7 84.9 2584.6 257 84.6 10377.9 240 77.9 96.1 75.2 2469.1 250 69.1 10078.6 231 78.6 92.476.1 236 76.1 94.4 77.1 2378.0 232 78.0 92.778.9 241 78.9 96.5 78.0 2477.0 242 77.0 96.780.1 222 80.1 88.8 82.6 2283.0 228 83.0 91.284.8 234 84.8 93.677.7 219 77.7 87.6 78.6 2279.4 220 79.4 88.080.7 229 80.7 91.6 80.8 2380.8 230 80.8 92.2

Concentration (pg/μL) % Recovery Avg Conc (pg/μ

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐3 ‐ Technical Toxaphene in Terry Creek Fish Samples

Laboratory Fish Replicate

Conc (pg/μL) Avg Conc (pg/μL) % RPD or RSD

ASHLAND 1 1 357 356 0.675

ASHLAND 1 2 354

ASHLAND 2 1 316 327 6.31ASHLAND 2 2 337

EPA_ NEIC 1 1 265 263 1.03

EPA_ NEIC 1 2 262

EPA_ NEIC 2 1 325 326 0.685

EPA_ NEIC 2 2 327

EPA_R4_1 1 1 360 368 3.85EPA_R4_1 1 2 360

EPA_R4_1 1 3 384

EPA_R4_1 2 1 268 263 4.79EPA_R4_1 2 2 249

EPA_R4_1 2 3 273

EPA_R4_2 1 1 314 312 1.39EPA_R4_2 1 2 309

EPA_R4_2 2 1 238 245 5.28EPA_R4_2 2 2 251

EPA_R4_3 1 1 341 338 1.70EPA_R4_3 1 2 335

EPA_R4_3 2 1 248 245 2.38EPA_R4_3 2 2 242

SCCWRP 1 1 425 424 0.272SCCWRP 1 2 423

SCCWRP 1 3 425SCCWRP 2 1 303 314 3.22

SCCWRP 2 2 315

SCCWRP 2 3 323

EPA_NERL/ORD_LV_1 1 1 267 275 5.90EPA_NERL/ORD_LV_1 1 2 283

EPA_NERL/ORD_LV_1 2 1 324 324 0.185

EPA_NERL/ORD_LV_1 2 2 324

EPA_NERL/ORD_LV_2 1 1 469 475 2.34EPA_NERL/ORD_LV_2 1 2 480

EPA_NERL/ORD_LV_2 2 1 489 492 1.14EPA_NERL/ORD_LV_2 2 2 494

Toxaphene

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐3 ‐ Technical Toxaphene in Terry Creek Fish Samples

Laboratory Fish Replicate

ASHLAND 1 1ASHLAND 1 2ASHLAND 2 1ASHLAND 2 2

EPA_ NEIC 1 1

EPA_ NEIC 1 2

EPA_ NEIC 2 1

EPA_ NEIC 2 2

EPA_R4_1 1 1EPA_R4_1 1 2EPA_R4_1 1 3EPA_R4_1 2 1EPA_R4_1 2 2EPA_R4_1 2 3EPA_R4_2 1 1EPA_R4_2 1 2EPA_R4_2 2 1EPA_R4_2 2 2EPA_R4_3 1 1EPA_R4_3 1 2EPA_R4_3 2 1EPA_R4_3 2 2

SCCWRP 1 1SCCWRP 1 2SCCWRP 1 3SCCWRP 2 1SCCWRP 2 2SCCWRP 2 3

EPA_NERL/ORD_LV_1 1 1EPA_NERL/ORD_LV_1 1 2EPA_NERL/ORD_LV_1 2 1EPA_NERL/ORD_LV_1 2 2EPA_NERL/ORD_LV_2 1 1EPA_NERL/ORD_LV_2 1 2EPA_NERL/ORD_LV_2 2 1EPA_NERL/ORD_LV_2 2 2

Conc (pg/μL)* % Recovery* Avg Conc (pg/μL) % RPD or RS

19.8 99.0 19.8 0.50619.7 98.593.4 93.4 92.8 1.40

92.1 92.121.1 105 21.1 0.0475

21.1 105

101 101 104 4.88106 106

18.6 93.0 19.1 7.7620.7 10417.9 89.586.6 86.6 94.7 7.41

99.2 99.298.3 98.320.4 102 20.3 1.19

20.1 10195.9 95.9 96.3 0.74896.6 96.620.3 102 20.4 0.98020.5 103

100 100 100 0.700

99.7 99.720.4 102 19.9 2.04

19.7 98.519.7 98.4

100 100 102 1.70103 103104 104

20.3 102 19.9 4.53

19.4 97.099.7 99.7 97.8 3.8995.9 95.930.2 151 30.2 0.0994

30.2 151

104 104 104 0.674104 104

* PCB 209 (Surrogate) spiked in Fish 1 at 20 pg/μL and

in Fish 2 at 100 pg/μL

PCB 209

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐3 ‐ Technical Toxaphene in Terry Creek Fish Samples

Laboratory Fish Replicate

ASHLAND 1 1ASHLAND 1 2ASHLAND 2 1ASHLAND 2 2

EPA_ NEIC 1 1

EPA_ NEIC 1 2

EPA_ NEIC 2 1

EPA_ NEIC 2 2

EPA_R4_1 1 1EPA_R4_1 1 2EPA_R4_1 1 3EPA_R4_1 2 1EPA_R4_1 2 2EPA_R4_1 2 3EPA_R4_2 1 1EPA_R4_2 1 2EPA_R4_2 2 1EPA_R4_2 2 2EPA_R4_3 1 1EPA_R4_3 1 2EPA_R4_3 2 1EPA_R4_3 2 2

SCCWRP 1 1SCCWRP 1 2SCCWRP 1 3SCCWRP 2 1SCCWRP 2 2SCCWRP 2 3

EPA_NERL/ORD_LV_1 1 1EPA_NERL/ORD_LV_1 1 2EPA_NERL/ORD_LV_1 2 1EPA_NERL/ORD_LV_1 2 2EPA_NERL/ORD_LV_2 1 1EPA_NERL/ORD_LV_2 1 2EPA_NERL/ORD_LV_2 2 1EPA_NERL/ORD_LV_2 2 2

Conc (pg/μL)** % Recovery** Avg Conc (pg/μL) % RPD or 

55.5 111 56.8 4.58

58.1 116

298 119 300 1.20302 121

53.6 107 53.3 1.18

53.0 106

234 93.5 250 13.1

266 107

52.3 105 52.2 1.24

51.5 10352.8 106

261 105 252 3.32248 99.2246 98.4

48.8 97.5 48.4 1.3648.1 96.2

243 97.3 243 0.334242 96.9

50.1 100 48.5 6.49

46.9 93.9

236 94.3 238 2.02

241 96.3

44.9 89.7 45.2 1.2344.9 89.945.9 91.7

233 93.0 234 1.26

231 92.5237 94.8

44.1 88.2 45.7 7.0047.3 94.6

234 93.6 226 6.58

219 87.6

80.9 162 81.0 0.161

81.1 162

236 94.4 234 1.54

232 92.9

** eHCH (Surrogate) spiked in Fish 1 at 50 pg/μL and in

Fish 2 at 250 pg/μL

eHCH

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐3‐1 ‐ Technical Toxaphene in Mass Units in Terry Creek Fish Samples

Laboratory Fish Replicate Toxaphene

Conc (μg/kg) Avg Conc (μg/kg) % RPD or RSD

ASHLAND 1 1 7140 7110 0.844

ASHLAND 1 2 7080

ASHLAND 2 1 632.0 653 6.43

ASHLAND 2 2 674

EPA_ NEIC 1 1 5300 5270 1.14

EPA_ NEIC 1 2 5240

EPA_ NEIC 2 1 650 652 0.613

EPA_ NEIC 2 2 654

EPA_R4_1 1 1 7200 7360 3.77

EPA_R4_1 1 2 7200

EPA_R4_1 1 3 7680

EPA_R4_1 2 1 536.0 526.7 4.81

EPA_R4_1 2 2 498

EPA_R4_1 2 3 546

EPA_R4_2 1 1 6280 6230 1.61

EPA_R4_2 1 2 6180

EPA_R4_2 2 1 476 489 5.32

EPA_R4_2 2 2 502.0

EPA_R4_3 1 1 6820 6760 1.78

EPA_R4_3 1 2 6700

EPA_R4_3 2 1 496 490 2.45

EPA_R4_3 2 2 484

SCCWRP 1 1 8500 8490 0.272

SCCWRP 1 2 8460

SCCWRP 1 3 8500

SCCWRP 2 1 606 627 3.21

SCCWRP 2 2 630

SCCWRP 2 3 646

EPA_NERL/ORD_LV_1 1 1 5340 5500 5.82

EPA_NERL/ORD_LV_1 1 2 5660.0

EPA_NERL/ORD_LV_1 2 1 648 648.0 0

EPA_NERL/ORD_LV_1 2 2 648.0

EPA_NERL/ORD_LV_2 1 1 9380 9490 2.32

EPA_NERL/ORD_LV_2 1 2 9600

EPA_NERL/ORD_LV_2 2 1 978 983 1.02

EPA_NERL/ORD_LV_2 2 2 988

* PCB 209 (Surrogate) spiked in Fish 1  at 20 pg/μL and in Fish 2 at 100 pg/μL

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report

August 2012

Attachment 2
Table A2‐4 ‐ Toxaphene Congeners in Terry Creek Fish Samples

Laboratory Fish Rep Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 

ASHLAND 1 1 86.6 96.7 7.10 8.50 4.10 4.60 7.40 ASHLAND 1 2 86.5 98.3 7.80 10.6 4.40 4.20 8.20 ASHLAND 2 1 62.0 85.9 12.2 11.7 5.10 6.80 11.9 ASHLAND 2 2 57.9 77.1 10.3 11.5 5.00 8.30 12.8 

EPA_ NEIC 1 1 77.6 90.1 7.90 11.7 4.50 5.27 8.63 

EPA_ NEIC 1 2 78.1 90.4 8.09 11.7 4.62 5.29 8.37 

EPA_ NEIC 2 1 51.7 73.6 12.1 12.8 5.44 6.45 13.5 

EPA_ NEIC 2 2 51.1 72.1 11.4 12.8 5.22 6.76 13.0 

EPA_R4_1 1 1 86.6 98.9 8.67 11.9 4.63 5.16 9.22 EPA_R4_1 1 2 88.3 99.5 8.42 12.5 4.72 5.40 9.32 EPA_R4_1 1 3 88.9 101 8.65 12.1 4.79 4.91 9.43 EPA_R4_1 2 1 63.0 88.0 13.0 14.1 5.78 7.21 14.4 EPA_R4_1 2 2 62.8 87.8 13.1 14.0 5.78 7.21 14.7 EPA_R4_1 2 3 57.9 80.0 12.2 13.1 5.42 6.71 13.7 EPA_R4_2 1 1 83.3 92.8 8.00 12.2 4.57 4.46 8.86 EPA_R4_2 1 2 82.5 91.3 7.67 12.0 4.48 4.94 8.72 EPA_R4_2 2 1 55.2 75.4 11.3 12.7 5.29 6.21 13.3 EPA_R4_2 2 2 56.0 76.0 11.7 12.9 5.30 6.42 13.3 EPA_R4_3 1 1 81.1 92.9 8.04 11.8 4.51 4.68 8.81 EPA_R4_3 1 2 80.5 91.5 8.14 11.8 4.50 4.62 8.64 EPA_R4_3 2 1 53.4 74.8 11.0 12.7 5.14 5.95 12.9 EPA_R4_3 2 2 53.8 74.2 11.7 12.9 5.13 6.37 13.2 

SCCWRP 1 1 78.4 91.5 8.60 10.8 4.50 4.80 8.30 

SCCWRP 1 2 81.3 94.1 8.00 10.9 4.50 5.00 8.50 

SCCWRP 1 3 81.6 96.9 8.80 12.1 4.90 4.90 9.00 

SCCWRP 2 1 51.2 74.1 11.6 12.4 5.30 6.30 12.6 

SCCWRP 2 2 52.5 76.4 11.6 11.9 5.10 6.70 12.8 

SCCWRP 2 3 53.7 78.4 12.3 12.8 5.70 7.00 13.5 

EPA_NERL/ORD_LV_1 1 1 72.1 87.1 8.74 10.5 4.63 4.96 6.83 

EPA_NERL/ORD_LV_1 1 2 73.0 79.6 7.99 8.97 4.57 4.14 7.11 

EPA_NERL/ORD_LV_1 2 1 51.8 72.0 11.1 12.2 5.33 6.55 9.64 

EPA_NERL/ORD_LV_1 2 2 51.0 71.8 11.4 11.1 5.52 4.90 11.7 

EPA_NERL/ORD_LV_2 1 1 73.2 83.8 7.07 10.3 4.12 4.51 7.87 

EPA_NERL/ORD_LV_2 1 2 73.4 86.2 8.26 11.3 4.18 4.35 8.18 

EPA_NERL/ORD_LV_2 2 1 47.4 67.7 11.7 13.2 5.00 7.01 13.5 EPA_NERL/ORD_LV_2 2 2 48.9 65.1 10.8 13.0 5.09 6.47 13.3 

concentration (pg/μL)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐4 ‐ Toxaphene Congeners in Terry Creek Fish Samples

Laboratory Fish Rep

ASHLAND 1 1ASHLAND 1 2ASHLAND 2 1ASHLAND 2 2

EPA_ NEIC 1 1

EPA_ NEIC 1 2

EPA_ NEIC 2 1

EPA_ NEIC 2 2

EPA_R4_1 1 1EPA_R4_1 1 2EPA_R4_1 1 3EPA_R4_1 2 1EPA_R4_1 2 2EPA_R4_1 2 3EPA_R4_2 1 1EPA_R4_2 1 2EPA_R4_2 2 1EPA_R4_2 2 2EPA_R4_3 1 1EPA_R4_3 1 2EPA_R4_3 2 1EPA_R4_3 2 2

SCCWRP 1 1

SCCWRP 1 2

SCCWRP 1 3

SCCWRP 2 1

SCCWRP 2 2

SCCWRP 2 3

EPA_NERL/ORD_LV_1 1 1

EPA_NERL/ORD_LV_1 1 2

EPA_NERL/ORD_LV_1 2 1

EPA_NERL/ORD_LV_1 2 2

EPA_NERL/ORD_LV_2 1 1

EPA_NERL/ORD_LV_2 1 2

EPA_NERL/ORD_LV_2 2 1

EPA_NERL/ORD_LV_2 2 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 

0.116 1.64 9.40 22.0 7.06 9.09 

6.84 10.8 16.9 1.72 1.98 19.9 

0.565 0.310 2.38 0.513 2.63 0.379 

1.17 2.04 6.29 0.078 4.13 4.69 

1.35 1.27 1.62 2.70 1.70 4.75 

4.70 5.32 3.87 4.19 3.67 4.10 

0.893 1.64 4.21 1.65 1.99 10.2 

1.33 0.832 3.48 1.02 0.189 3.33 

0.743 1.50 1.24 0.593 0.222 1.29 

0.840 0.859 6.78 1.65 0.195 6.82 

2.17 2.85 4.92 6.26 4.98 2.04 

2.40 2.82 3.42 3.84 5.69 5.27 

1.24 9.00 8.38 15.4 0.00 19.8 

1.56 0.278 2.67 9.44 3.70 29.6 

0.273 2.85 15.5 9.63 1.45 3.61 

3.05 3.91 8.29 1.61 1.78 8.01 

Relative % Difference (RPD) or Relative Standard Deviation (RSD)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐4 ‐ Toxaphene Congeners in Terry Creek Fish Samples

Laboratory Fish Rep

ASHLAND 1 1ASHLAND 1 2ASHLAND 2 1ASHLAND 2 2

EPA_ NEIC 1 1

EPA_ NEIC 1 2

EPA_ NEIC 2 1

EPA_ NEIC 2 2

EPA_R4_1 1 1EPA_R4_1 1 2EPA_R4_1 1 3EPA_R4_1 2 1EPA_R4_1 2 2EPA_R4_1 2 3EPA_R4_2 1 1EPA_R4_2 1 2EPA_R4_2 2 1EPA_R4_2 2 2EPA_R4_3 1 1EPA_R4_3 1 2EPA_R4_3 2 1EPA_R4_3 2 2

SCCWRP 1 1

SCCWRP 1 2

SCCWRP 1 3

SCCWRP 2 1

SCCWRP 2 2

SCCWRP 2 3

EPA_NERL/ORD_LV_1 1 1

EPA_NERL/ORD_LV_1 1 2

EPA_NERL/ORD_LV_1 2 1

EPA_NERL/ORD_LV_1 2 2

EPA_NERL/ORD_LV_2 1 1

EPA_NERL/ORD_LV_2 1 2

EPA_NERL/ORD_LV_2 2 1

EPA_NERL/ORD_LV_2 2 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 

86.6 97.5 7.45 9.55 4.25 4.40 

60.0 81.5 11.3 11.6 5.05 7.55 

77.8 90.2 8.00 11.7 4.56 5.28 

51.4 72.9 11.8 12.8 5.33 6.61 

87.9 99.9 8.58 12.2 4.71 5.16 

61.3 85.3 12.8 13.7 5.66 7.04 

82.9 92.0 7.84 12.1 4.53 4.70 

55.6 75.7 11.5 12.8 5.30 6.32 

80.8 92.2 8.09 11.8 4.51 4.65 

53.6 74.5 11.4 12.8 5.14 6.16 

80.4 94.1 8.47 11.3 4.63 4.90 

52.5 76.3 11.8 12.4 5.37 6.67 

72.6 83.4 8.35 9.75 4.60 4.55 51.4 71.9 11.3 11.7 5.40 5.75 

73.3 85.0 7.67 10.8 4.15 4.43 

48.1 66.4 11.2 13.1 5.05 6.74 

Average Concentration (pg/μL)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐4 ‐ Toxaphene Congeners in Terry Creek Fish Samples

Laboratory Fish Rep

ASHLAND 1 1

ASHLAND 1 2

ASHLAND 2 1

ASHLAND 2 2

EPA_ NEIC 1 1

EPA_ NEIC 1 2

EPA_ NEIC 2 1

EPA_ NEIC 2 2

EPA_R4_1 1 1EPA_R4_1 1 2EPA_R4_1 1 3EPA_R4_1 2 1EPA_R4_1 2 2EPA_R4_1 2 3EPA_R4_2 1 1EPA_R4_2 1 2EPA_R4_2 2 1EPA_R4_2 2 2EPA_R4_3 1 1EPA_R4_3 1 2EPA_R4_3 2 1EPA_R4_3 2 2

SCCWRP 1 1SCCWRP 1 2SCCWRP 1 3SCCWRP 2 1SCCWRP 2 2SCCWRP 2 3

EPA_NERL/ORD_LV_1 1 1

EPA_NERL/ORD_LV_1 1 2

EPA_NERL/ORD_LV_1 2 1

EPA_NERL/ORD_LV_1 2 2

EPA_NERL/ORD_LV_2 1 1

EPA_NERL/ORD_LV_2 1 2

EPA_NERL/ORD_LV_2 2 1

EPA_NERL/ORD_LV_2 2 2

PCB 209 (spiked

at 100)

eHCH (spiked at

250) PCB 209 eHCH PCB 209 eHCH P

Avg Conc (pg/μL) % R

88.1 277 88.1 111 90.0 275 

91.9 273 91.9 109

85.2 295 85.2 118 88.5 274 91.7 254 91.7 102

105 240 105 96.0 105 242 105 244 105 97.4

108 231 108 92.5 108 231 

107 231 107 92.4

96.8 246 96.8 98.5 92.6 255 93.2 263 93.2 105

87.9 256 87.9 10278.0 252 78.0 101 85.8 245 

81.2 252 81.2 10198.1 231 98.1 92.596.6 245 96.6 98.0 95.4 245 94.3 244 94.3 97.795.9 230 95.9 91.9 95.3 230 94.7 230 94.7 92.295.2 248 95.2 99.2 95.3 246 

95.4 244 95.4 97.795.0 227 95.0 90.7 95.8 226 

96.6 226 96.6 90.5

100 234 100 93.6 100 242 

99.8 241 99.8 96.4

101 250 101 100

103 218 103 87.2 104 224 104 223 104 89.2

106 230 106 92.0

99.4 246 99.4 98.4 98.6 235 

97.8 224 97.8 89.697.9 234 97.9 93.6 98.4 226 

98.9 218 98.9 87.2

95.3 228 95.3 91.3 95.5 229 95.6 231 95.6 92.2

100 214 100 85.7 101 218 102 221 102 88.5

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐4‐1 ‐ Toxaphene Congeners in Mass Units in Terry Creek Fish Samples

Laboratory Fish Rep Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 

concentration (μg/kg)

ASHLAND 1 1 173 193 14.2 16.9 8.17 9.2 14.8 

ASHLAND 1 2 172 196 15.5 21.1 8.77 8.4 16.3 ASHLAND 2 1 12 17 2.4 2.3 1.02 1.4 2.4 

ASHLAND 2 2 12 15 2.1 2.3 1.00 1.66 2.6 

EPA_ NEIC 1 1 155 180 15.7 23.3 8.97 10.5 17.2 EPA_ NEIC 1 2 156 180 16.1 23.3 9.21 10.5 16.7 EPA_ NEIC 2 1 10 15 2.4 2.6 1.09 1.3 2.7 EPA_ NEIC 2 2 10 14 2.3 2.6 1.04 1.35 2.6 

EPA_R4_1 1 1 173 197 17.3 23.7 9.23 10.3 18.4 EPA_R4_1 1 2 176 198 16.8 24.9 9.41 10.8 18.6 EPA_R4_1 1 3 177 201 17.2 24.1 9.55 9.79 18.8 EPA_R4_1 2 1 12.6 17.6 2.6 2.82 1.16 1.44 2.88 EPA_R4_1 2 2 12.6 17.6 2.62 2.8 1.16 1.44 2.94 EPA_R4_1 2 3 11.6 16.0 2.44 2.62 1.08 1.34 2.74 EPA_R4_2 1 1 166 185 15.9 24.3 9.11 8.89 17.7 EPA_R4_2 1 2 164 182 15.3 23.9 8.93 9.85 17.4 EPA_R4_2 2 1 11.0 15.1 2.26 2.54 1.06 1.24 2.66 EPA_R4_2 2 2 11.2 15.2 2.34 2.58 1.06 1.28 2.66 EPA_R4_3 1 1 162 185 16.0 23.5 8.99 9.33 17.6 EPA_R4_3 1 2 160 182 16.2 23.5 8.97 9.21 17.2 EPA_R4_3 2 1 10.7 15.0 2.2 2.54 1.03 1.19 2.58 EPA_R4_3 2 2 10.8 14.8 2.34 2.58 1.03 1.27 2.64 

SCCWRP 1 1 156 182 17.1 21.5 8.97 9.57 16.5 SCCWRP 1 2 162 188 15.9 21.7 8.97 9.97 16.9 SCCWRP 1 3 163 193 17.5 24.1 9.77 9.77 17.9 SCCWRP 2 1 10.2 14.8 2.32 2.48 1.06 1.26 2.52 SCCWRP 2 2 10.5 15.3 2.32 2.38 1.02 1.34 2.56 SCCWRP 2 3 10.7 15.7 2.46 2.56 1.14 1.40 2.70 

EPA_NERL/ORD_LV_1 1 1 144 174 17.4 20.9 9.23 9.89 13.6 

EPA_NERL/ORD_LV_1 1 2 146 159 15.9 17.9 9.11 8.25 14.2 

EPA_NERL/ORD_LV_1 2 1 10.4 14.4 2.22 2.44 1.07 1.31 1.93 

EPA_NERL/ORD_LV_1 2 2 10.2 14.4 2.28 2.22 1.10 0.98 2.34 EPA_NERL/ORD_LV_2 1 1 146 167 14.1 20.5 8.21 8.99 15.7 

EPA_NERL/ORD_LV_2 1 2 146 172 16.5 22.5 8.33 8.67 16.3 

EPA_NERL/ORD_LV_2 2 1 9.48 13.5 2.34 2.64 1.00 1.40 2.70 EPA_NERL/ORD_LV_2 2 2 9.78 13.0 2.16 2.6 1.02 1.29 2.66 

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐4‐1 ‐ Toxaphene Congeners in Mass Units in Terry Creek Fish Samples

Laboratory Fish Rep

ASHLAND 1 1

ASHLAND 1 2

ASHLAND 2 1

ASHLAND 2 2

EPA_ NEIC 1 1EPA_ NEIC 1 2EPA_ NEIC 2 1EPA_ NEIC 2 2

EPA_R4_1 1 1EPA_R4_1 1 2EPA_R4_1 1 3EPA_R4_1 2 1EPA_R4_1 2 2EPA_R4_1 2 3EPA_R4_2 1 1EPA_R4_2 1 2EPA_R4_2 2 1EPA_R4_2 2 2EPA_R4_3 1 1EPA_R4_3 1 2EPA_R4_3 2 1EPA_R4_3 2 2

SCCWRP 1 1

SCCWRP 1 2

SCCWRP 1 3

SCCWRP 2 1

SCCWRP 2 2

SCCWRP 2 3

EPA_NERL/ORD_LV_1 1 1

EPA_NERL/ORD_LV_1 1 2

EPA_NERL/ORD_LV_1 2 1EPA_NERL/ORD_LV_1 2 2

EPA_NERL/ORD_LV_2 1 1

EPA_NERL/ORD_LV_2 1 2

EPA_NERL/ORD_LV_2 2 1EPA_NERL/ORD_LV_2 2 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 

Relative % Difference (RPD) or Relative Standard Devi

0.116 1.64 9.40 22.0 7.06 9.09 

6.84 10.8 16.9 1.72 1.98 19.9 

0.643 0.00 2.52 0.00 2.64 0.00 

1.17 2.06 5.96 0.00 4.13 4.69 1.36 1.08 1.62 2.51 1.70 4.75 4.72 5.35 3.86 4.01 3.67 4.10 

0.965 1.63 4.21 1.65 1.99 10.2 

11.1 15.1 2.30 2.56 1.06 1.26 

0.743 1.52 1.24 0.00 0.222 1.29 

0.746 0.805 6.17 1.56 0.195 6.82 

2.20 2.87 4.92 6.42 4.98 2.04 2.38 2.82 3.42 3.65 5.69 5.27 1.24 9.00 8.97 15.7 1.30 18.0 

1.56 0.278 2.67 9.44 3.50 28.8 

0.273 2.82 15.5 9.26 1.45 3.61 

3.12 3.92 8.00 1.53 1.78 8.01 

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:Analytical Data Report
Table A2‐5 ‐ Technical Toxaphene Second Source Standard

Laboratory Replicate Conc (pg/μL)

Avg Conc

(pg/μL) % Recovery % RPD or RSD Conc (pg/μL)

Avg Conc

(pg/μL) % Recovery % RPD or RSD Conc (pg/μL)

Avg Conc

(pg/μL) % Reco

ASHLAND 1 152 152 101 109 109 109 251 251 10

EPA_ NEIC 1 156 165 104 5.29 110 110 110 0.368 246 260 98.EPA_ NEIC 2 174 116 110 110 267 107EPA_ NEIC 3 166 111 109 109 268 107

EPA_R4_1 1 172 166 115 4.18 114 112 114 1.72 263 265 105 EPA_R4_1 2 168 112 112 112 264 105

EPA_R4_1 3 159 106 110 110 269 108EPA_R4_2 1 166 166 111 0.881 113 112 113 0.713 256 256 102 

EPA_R4_2 2 165 110 112 112 257 103EPA_R4_3 1 160 165 107 6.11 112 111 112 1.83 253 255 10

EPA_R4_3 2 170 113 110 110 257 103

SCCWRP 1 152 149 101 2.80 107 106 107 3.40 255 253 102 SCCWRP 2 144 96.0 102 102 255 102

SCCWRP 3 150 100 109 109 250 100

EPA_NERL/ORD_LV_1 1 163 142 108 29.7 105 106 105 2.64 278 290 11EPA_NERL/ORD_LV_1 2 121 80.4 108 108 302 12

EPA_NERL/ORD_LV_2 1 162 166 108 4.93 110 109 110 2.64 282 278 113 

EPA_NERL/ORD_LV_2 2 170 114 107 107 274 110

Technical Toxaphene Spiked

at 150 pg/μL

PCB 209 (Surrogate) Spiked

at 100 pg/μL

eHCH (Surrogate) Spik

250 pg/μL

Toxaphene PCB 209 eHCH

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐6 ‐ Technical Toxaphene Laboratory Quality Control Samples

Laboratory Replicate Type True Value (pg/μL) Conc (pg/μL) Avg Conc (pg/μL) % Recovery % RPD or RSD Conc (pg/μL) Avg Conc (pg/μL) % Recovery % RPD or RSD Conc (pg/μL) Avg 

ASHLAND 1 MB ND 101 101 101 0.892 270 ASHLAND 2 MB ND 100 100 276 ASHLAND 1 LCS1 50.0 56.1 55.7 112 1.62 90.0 91.6 90.0 3.49 267 ASHLAND 2 LCS1 50.0 55.2 110 93.2 93.2 256 ASHLAND 1 LCS2 200 237 223 118 12.4 83.7 83.7 83.7 264 ASHLAND 2 LCS2 200 209 105 83.7 83.7 265 

EPA_ NEIC 1 MB ND 107 106 107 1.49 254 EPA_ NEIC 2 MB ND 105 105 246 EPA_ NEIC 1 LCS1 50.0 70.6 68.2 141 6.93 94.4 96.8 94.4 5.12 282 EPA_ NEIC 2 LCS1 50.0 65.9 132 99.3 99.3 231 EPA_ NEIC 1 LCS2 200 203 204 101 0.854 94.6 95.8 94.6 2.68 267 EPA_ NEIC 2 LCS2 200 205 102 97.1 97.1 240 

EPA_R4_1 1 MB 3.08 101 102 101 1.02 249 EPA_R4_1 2 MB 3.36 102 102 249 EPA_R4_1 3 MB 4.66 103 103 249 EPA_R4_1 1 LCS1 50.0 62.0 60.0 124 13.3 93.4 95.5 93.4 3.04 231 EPA_R4_1 2 LCS1 50.0 66.8 134 94.4 94.4 230 EPA_R4_1 3 LCS1 50.0 51.2 102 98.8 98.8 233 EPA_R4_1 1 LCS2 200 229 221 114 5.13 77.1 80.6 77.1 4.70 257 EPA_R4_1 2 LCS2 200 208 104 79.9 79.9 251 EPA_R4_1 3 LCS2 200 225 113 84.6 84.6 246 EPA_R4_2 1 MB 5.29 101 101 101 0.862 246 EPA_R4_2 2 MB 5.06 100 100 245 EPA_R4_2 1 LCS1 50.0 51.4 56.8 103 19.0 92.3 93.4 92.3 2.33 229 EPA_R4_2 2 LCS1 50.0 62.2 124 94.5 94.5 223 EPA_R4_2 1 LCS2 200 204 202 102 1.79 89.3 90.0 89.3 1.47 237 EPA_R4_2 2 LCS2 200 201 100 90.6 90.6 235 

EPA_R4_3 1 MB 1.63 102 102 102 0.353 240 EPA_R4_3 2 MB 1.82 102 102 246 EPA_R4_3 1 LCS1 50.0 42.1 43.1 84.1 4.80 93.9 94.1 93.9 0.298 227 EPA_R4_3 2 LCS1 50.0 44.1 88.2 94.2 94.2 227 EPA_R4_3 1 LCS2 200 189 181 94.3 8.43 92.5 91.8 92.5 1.51 228 EPA_R4_3 2 LCS2 200 173 86.6 91.1 91.1 240 

SCCWRP 1 MB 0.240 107 104 107 2.21 237 SCCWRP 2 MB 0.240 103 103 232 SCCWRP 3 MB 0.130 103 103 234 SCCWRP 1 LCS1 50.0 44.5 44.9 89.0 2.07 98.5 97.3 98.5 2.50 225 SCCWRP 2 LCS1 50.0 46.0 92.0 98.9 98.9 221 SCCWRP 3 LCS1 50.0 44.3 88.6 94.5 94.5 225 SCCWRP 1 LCS2 200 226 217 113 3.72 95.3 93.2 95.3 2.02 228 SCCWRP 2 LCS2 200 210 105 91.6 91.6 221 SCCWRP 3 LCS2 200 216 108 92.8 92.8 230 

EPA_NERL/ORD_LV_1 1 MB ND 105 103 105 3.78 241 

EPA_NERL/ORD_LV_1 2 MB ND 101 101 232 

EPA_NERL/ORD_LV_1 1 LCS1 50.0 47.6 58.9 95.2 38.2 95.7 95.2 95.7 1.16 191 

EPA_NERL/ORD_LV_1 2 LCS1 50.0 70.1 94.6 94.6 197 

EPA_NERL/ORD_LV_1 1 LCS2 200 207 204 103 2.15 92.1 91.6 92.1 1.20 229 

EPA_NERL/ORD_LV_1 2 LCS2 200 202 91.0 91.0 206 

EPA_NERL/ORD_LV_2 1 MB 19.4 107 107 107 0.871 251 

EPA_NERL/ORD_LV_2 2 MB 16.1 106 106 247 

EPA_NERL/ORD_LV_2 1 LCS1 50.0 66.4 70.6 133 11.9 96.6 96.5 96.6 0.270 224 

EPA_NERL/ORD_LV_2 2 LCS1 50.0 74.8 150 96.3 96.3 225 

EPA_NERL/ORD_LV_2 1 LCS2 200 205 207 103 1.64 95.1 94.9 95.1 0.464 234 

EPA_NERL/ORD_LV_2 2 LCS2 200 209 104 94.7 94.7 235 

PCB 209 (Surrogate) 

eHCH (Surrogat

Toxaphene

highlighted cells have concentrations below the LLOQ of

50 pg/μL PCB 209 (Surrogate) Spiked in MB, LCS 1, and LCS 2 at 100 pg/μL

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐7 ‐ Toxaphene Congeners Spiked in Laboratory Quality Control Samples

Laboratory Type Replicate Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 P62

ASHLAND MB 1 0.100 0.100 ND ND ND ND ND NDASHLAND MB 2 ND ND ND ND ND ND ND NDASHLAND LCS1 1 108 108 101 104 102 101 97.9 246ASHLAND LCS1 2 106 107 99.3 104 102 100 96.8 224ASHLAND LCS2 1 2.00 2.30 2.00 2.30 2.20 2.40 1.90 23.0ASHLAND LCS2 2 2.10 2.10 1.80 2.00 2.00 2.00 2.10 26.3

EPA_ NEIC MB 1 <0.0800 <0.200 <0.300 <0.0800 <0.0600 <0.200 <0.100 <3.00EPA_ NEIC MB 2 <0.0800 <0.200 <0.300 <0.0800 <0.0600 <0.200 <0.100 <3.00EPA_ NEIC LCS1 1 98.7 99.6 103 99.1 99.9 101 99.9 225EPA_ NEIC LCS1 2 95.7 96.0 101 98.8 99.7 103 101 240EPA_ NEIC LCS2 1 1.91 1.90 2.31 2.04 1.88 1.96 2.23 23.1EPA_ NEIC LCS2 2 1.94 1.93 2.14 2.04 2.05 2.05 1.94 21.0

EPA_R4_1 MB 1 ND ND ND ND ND ND ND NDEPA_R4_1 MB 2 ND ND ND ND ND ND ND NDEPA_R4_1 MB 3 ND ND ND ND ND ND ND NDEPA_R4_1 LCS1 1 107 109 108 106 107 111 106 274EPA_R4_1 LCS1 2 106 107 105 106 107 111 106 276EPA_R4_1 LCS1 3 101 102 101 103 104 108 104 281EPA_R4_1 LCS2 1 2.26 2.18 2.3 2.07 2.11 2.11 2.09 24.7EPA_R4_1 LCS2 2 2.24 2.17 2.26 2.04 2.12 2.25 2.17 25.9EPA_R4_1 LCS2 3 2.15 2.04 1.93 2.04 2.13 2.11 2.08 26.0EPA_R4_2 MB 1 ND ND ND ND ND ND ND NDEPA_R4_2 MB 2 ND ND ND ND ND ND ND NDEPA_R4_2 LCS1 1 99.6 97.8 97.0 101 99.7 102 99.8 253EPA_R4_2 LCS1 2 102 100 98.1 101 102 104 102 253EPA_R4_2 LCS2 1 2.04 2.01 1.91 1.90 1.87 1.95 1.88 23.7EPA_R4_2 LCS2 2 1.99 2.00 1.85 1.93 2.00 1.96 1.99 23.2EPA_R4_3 MB 1 ND ND ND ND ND ND ND NDEPA_R4_3 MB 2 ND ND ND ND ND ND ND NDEPA_R4_3 LCS1 1 96.6 96.4 97.5 97.8 97.5 100 96.9 243EPA_R4_3 LCS1 2 96.7 96.9 95.9 97.9 99.3 101 98.8 249EPA_R4_3 LCS2 1 2.05 1.97 2.15 1.83 1.97 2.03 2.01 23.1EPA_R4_3 LCS2 2 1.96 2.02 2.00 1.85 1.88 1.98 1.93 23.6

SCCWRP MB 1 ND ND ND ND ND ND ND NDSCCWRP MB 2 ND ND ND ND ND ND ND NDSCCWRP MB 3 ND ND ND ND ND ND ND NDSCCWRP LCS1 1 97.1 98.8 96.2 96.1 96.5 94.9 95.7 211SCCWRP LCS1 2 99.2 101 102 102 104 106 103 249SCCWRP LCS1 3 99.0 103 103 104 107 109 105 261SCCWRP LCS2 1 1.76 1.90 1.65 1.86 1.87 1.91 1.89 18.1SCCWRP LCS2 2 1.78 1.93 1.76 1.90 1.91 1.91 1.95 17.6SCCWRP LCS2 3 1.88 1.89 1.93 1.95 2.03 2.12 1.97 22.6

EPA_NERL/ORD_LV_1 MB 1 0.32 0.27 0.84 0.6 0.66 0.95 0.66 1.55EPA_NERL/ORD_LV_1 MB 2 0.34 0.26 0.82 0.58 0.66 0.87 0.68 1.34EPA_NERL/ORD_LV_1 LCS1 1 92.4 91.6 85.0 87.1 85.4 78.2 80.7 182

EPA_NERL/ORD_LV_1 LCS1 2 91.3 93.2 91.2 86.3 86.0 81.1 82.9 189

EPA_NERL/ORD_LV_1 LCS2 1 1.55 1.48 0.95 2.07 2.34 1.15 2.09 11.9

EPA_NERL/ORD_LV_1 LCS2 2 2.11 2.31 1.82 1.29 2.44 2.17 1.86 12.1

EPA_NERL/ORD_LV_2 MB 1 ND ND ND ND 0.18 ND ND NDEPA_NERL/ORD_LV_2 MB 2 ND ND ND ND ND ND ND NDEPA_NERL/ORD_LV_2 LCS1 1 92.5 92.7 96 91.9 95.1 95.9 90.4 223

EPA_NERL/ORD_LV_2 LCS1 2 88.0 89.8 90.5 89.6 91.9 96.4 90.6 231

EPA_NERL/ORD_LV_2 LCS2 1 1.74 1.85 1.24 2.00 1.95 2.25 2.15 15.6

EPA_NERL/ORD_LV_2 LCS2 2 1.73 1.82 1.20 1.96 1.80 1.74 2.02 19.4

Concentration (pg/μL)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐7 ‐ Toxaphene Congeners Spiked in Laboratory Quality Control Samples

Laboratory Type Replicate

ASHLAND MB 1ASHLAND MB 2ASHLAND LCS1 1ASHLAND LCS1 2ASHLAND LCS2 1ASHLAND LCS2 2

EPA_ NEIC MB 1EPA_ NEIC MB 2EPA_ NEIC LCS1 1EPA_ NEIC LCS1 2EPA_ NEIC LCS2 1EPA_ NEIC LCS2 2

EPA_R4_1 MB 1EPA_R4_1 MB 2EPA_R4_1 MB 3EPA_R4_1 LCS1 1EPA_R4_1 LCS1 2EPA_R4_1 LCS1 3EPA_R4_1 LCS2 1EPA_R4_1 LCS2 2EPA_R4_1 LCS2 3EPA_R4_2 MB 1EPA_R4_2 MB 2EPA_R4_2 LCS1 1EPA_R4_2 LCS1 2EPA_R4_2 LCS2 1EPA_R4_2 LCS2 2EPA_R4_3 MB 1EPA_R4_3 MB 2EPA_R4_3 LCS1 1EPA_R4_3 LCS1 2EPA_R4_3 LCS2 1EPA_R4_3 LCS2 2

SCCWRP MB 1SCCWRP MB 2SCCWRP MB 3SCCWRP LCS1 1SCCWRP LCS1 2SCCWRP LCS1 3SCCWRP LCS2 1SCCWRP LCS2 2SCCWRP LCS2 3

EPA_NERL/ORD_LV_1 MB 1EPA_NERL/ORD_LV_1 MB 2EPA_NERL/ORD_LV_1 LCS1 1

EPA_NERL/ORD_LV_1 LCS1 2

EPA_NERL/ORD_LV_1 LCS2 1

EPA_NERL/ORD_LV_1 LCS2 2

EPA_NERL/ORD_LV_2 MB 1EPA_NERL/ORD_LV_2 MB 2EPA_NERL/ORD_LV_2 LCS1 1

EPA_NERL/ORD_LV_2 LCS1 2

EPA_NERL/ORD_LV_2 LCS2 1

EPA_NERL/ORD_LV_2 LCS2 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 P62

100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226

2.00 2.00 2.00 2.00 2.00 2.00 2.00 22.62.00 2.00 2.00 2.00 2.00 2.00 2.00 22.6

100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226

2.00 2.00 2.00 2.00 2.00 2.00 2.00 22.62.00 2.00 2.00 2.00 2.00 2.00 2.00 22.6

100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226

2.00 2.00 2.00 2.00 2.00 2.00 2.00 22.62.00 2.00 2.00 2.00 2.00 2.00 2.00 22.62.00 2.00 2.00 2.00 2.00 2.00 2.00 22.6

100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226

2.00 2.00 2.00 2.00 2.00 2.00 2.00 22.62.00 2.00 2.00 2.00 2.00 2.00 2.00 22.6

100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226

2.00 2.00 2.00 2.00 2.00 2.00 2.00 22.62.00 2.00 2.00 2.00 2.00 2.00 2.00 22.6

100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226

2.00 2.00 2.00 2.00 2.00 2.00 2.00 22.62.00 2.00 2.00 2.00 2.00 2.00 2.00 22.62.00 2.00 2.00 2.00 2.00 2.00 2.00 22.6

100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226

2.00 2.00 2.00 2.00 2.00 2.00 2.00 22.62.00 2.00 2.00 2.00 2.00 2.00 2.00 22.6

100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226

2.00 2.00 2.00 2.00 2.00 2.00 2.00 22.62.00 2.00 2.00 2.00 2.00 2.00 2.00 22.6

True Value (pg/μL)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐7 ‐ Toxaphene Congeners Spiked in Laboratory Quality Control Samples

Laboratory Type Replicate

ASHLAND MB 1ASHLAND MB 2ASHLAND LCS1 1ASHLAND LCS1 2ASHLAND LCS2 1ASHLAND LCS2 2

EPA_ NEIC MB 1EPA_ NEIC MB 2EPA_ NEIC LCS1 1EPA_ NEIC LCS1 2EPA_ NEIC LCS2 1EPA_ NEIC LCS2 2

EPA_R4_1 MB 1EPA_R4_1 MB 2EPA_R4_1 MB 3EPA_R4_1 LCS1 1EPA_R4_1 LCS1 2EPA_R4_1 LCS1 3EPA_R4_1 LCS2 1EPA_R4_1 LCS2 2EPA_R4_1 LCS2 3EPA_R4_2 MB 1EPA_R4_2 MB 2EPA_R4_2 LCS1 1EPA_R4_2 LCS1 2EPA_R4_2 LCS2 1EPA_R4_2 LCS2 2EPA_R4_3 MB 1EPA_R4_3 MB 2EPA_R4_3 LCS1 1EPA_R4_3 LCS1 2EPA_R4_3 LCS2 1EPA_R4_3 LCS2 2

SCCWRP MB 1SCCWRP MB 2SCCWRP MB 3SCCWRP LCS1 1SCCWRP LCS1 2SCCWRP LCS1 3SCCWRP LCS2 1SCCWRP LCS2 2SCCWRP LCS2 3

EPA_NERL/ORD_LV_1 MB 1EPA_NERL/ORD_LV_1 MB 2EPA_NERL/ORD_LV_1 LCS1 1

EPA_NERL/ORD_LV_1 LCS1 2

EPA_NERL/ORD_LV_1 LCS2 1

EPA_NERL/ORD_LV_1 LCS2 2

EPA_NERL/ORD_LV_2 MB 1EPA_NERL/ORD_LV_2 MB 2EPA_NERL/ORD_LV_2 LCS1 1

EPA_NERL/ORD_LV_2 LCS1 2

EPA_NERL/ORD_LV_2 LCS2 1

EPA_NERL/ORD_LV_2 LCS2 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 P62

107 107 100 104 102 100 97.4 235

2.05 2.20 1.90 2.15 2.10 2.20 2.00 24.797.2 97.8 102 98.9 99.8 102 100 2321.93 1.92 2.23 2.04 1.97 2.01 2.09 22.0

105 106 105 105 106 110 105 277

2.22 2.13 2.16 2.05 2.12 2.16 2.11 25.6

101 99.0 97.6 101 101 103 101 253

2.02 2.01 1.88 1.92 1.94 1.96 1.94 23.496.7 96.6 96.7 97.8 98.4 100 97.9 2462.01 2.00 2.08 1.84 1.93 2.01 1.97 23.398.4 101 101 101 103 103 101 2401.81 1.91 1.78 1.9 1.94 1.98 1.94 19.491.9 92.4 88.1 86.7 85.7 79.7 81.8 1861.83 1.9 1.39 1.68 2.39 1.66 1.98 12.090.2 91.3 93.2 90.8 93.5 96.1 90.5 2271.74 1.84 1.22 1.98 1.88 2.00 2.09 17.5

Average Conc (pg/μL)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐7 ‐ Toxaphene Congeners Spiked in Laboratory Quality Control Samples

Laboratory Type Replicate

ASHLAND MB 1ASHLAND MB 2ASHLAND LCS1 1ASHLAND LCS1 2ASHLAND LCS2 1ASHLAND LCS2 2

EPA_ NEIC MB 1EPA_ NEIC MB 2EPA_ NEIC LCS1 1EPA_ NEIC LCS1 2EPA_ NEIC LCS2 1EPA_ NEIC LCS2 2

EPA_R4_1 MB 1EPA_R4_1 MB 2EPA_R4_1 MB 3EPA_R4_1 LCS1 1EPA_R4_1 LCS1 2EPA_R4_1 LCS1 3EPA_R4_1 LCS2 1EPA_R4_1 LCS2 2EPA_R4_1 LCS2 3EPA_R4_2 MB 1EPA_R4_2 MB 2EPA_R4_2 LCS1 1EPA_R4_2 LCS1 2EPA_R4_2 LCS2 1EPA_R4_2 LCS2 2EPA_R4_3 MB 1EPA_R4_3 MB 2EPA_R4_3 LCS1 1EPA_R4_3 LCS1 2EPA_R4_3 LCS2 1EPA_R4_3 LCS2 2

SCCWRP MB 1SCCWRP MB 2SCCWRP MB 3SCCWRP LCS1 1SCCWRP LCS1 2SCCWRP LCS1 3SCCWRP LCS2 1SCCWRP LCS2 2SCCWRP LCS2 3

EPA_NERL/ORD_LV_1 MB 1EPA_NERL/ORD_LV_1 MB 2EPA_NERL/ORD_LV_1 LCS1 1

EPA_NERL/ORD_LV_1 LCS1 2

EPA_NERL/ORD_LV_1 LCS2 1

EPA_NERL/ORD_LV_1 LCS2 2

EPA_NERL/ORD_LV_2 MB 1EPA_NERL/ORD_LV_2 MB 2EPA_NERL/ORD_LV_2 LCS1 1

EPA_NERL/ORD_LV_2 LCS1 2

EPA_NERL/ORD_LV_2 LCS2 1

EPA_NERL/ORD_LV_2 LCS2 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 P62

108% 108% 101% 104% 102% 101% 97.9% 109%106% 107% 99.3% 104% 102% 100% 96.8% 98.9%100% 115% 100% 115% 110% 120% 95.0% 102%105% 105% 90% 100% 100% 100% 105% 116%

98.7% 100% 103% 99.1% 100% 101% 100% 100%95.7% 96.0% 101% 98.8% 100% 103% 101% 106%95.5% 95.0% 116% 102% 94.0% 98.0% 112% 102%97.0% 96.5% 107% 102% 103% 103% 97.0% 93.0%

107% 109% 108% 106% 107% 111% 106% 121%106% 107% 105% 106% 107% 111% 106% 122%101% 102% 101% 103% 104% 108% 104% 125%113% 109% 115% 104% 106% 106% 105% 95.1%112% 109% 113% 102% 106% 113% 109% 100%108% 102% 96.5% 102% 107% 106% 104% 100%100% 97.8% 97.0% 101% 100% 102% 100% 112%102% 100% 98.1% 101% 102% 104% 102% 112%102% 101% 95.5% 95.0% 93.5% 97.5% 94.0% 91.2%100% 100% 92.5% 96.5% 100% 98% 100% 89.1%

96.6% 96.4% 97.5% 97.8% 97.5% 100% 97% 107%96.7% 96.9% 95.9% 97.9% 99.3% 101% 98.8% 110%

103% 98.5% 108% 91.5% 98.5% 102% 101% 88.7%

98.0% 101% 100% 92.5% 94.0% 99.0% 96.5% 90.9%97.1% 98.8% 96.2% 96.1% 96.5% 94.9% 95.7% 93.4%99.2% 101% 102% 102% 104% 106% 103% 110%99.0% 103% 103% 104% 107% 109% 105% 115%88.0% 95.0% 82.5% 93.0% 93.5% 95.5% 94.5% 79.9%89.0% 96.5% 88.0% 95.0% 95.5% 95.5% 97.5% 78.0%94.0% 94.5% 96.5% 97.5% 102% 106% 98.5% 100%92.4% 91.6% 85.0% 87.1% 85.4% 78.2% 80.7% 80.5%91.3% 93.2% 91.2% 86.3% 86.0% 81.1% 82.9% 83.6%77.5% 74.0% 47.5% 104% 117% 57.5% 105% 45.8%

106% 116% 91.0% 64.5% 122% 109% 93.0% 46.5%

92.5% 92.7% 96.0% 91.9% 95.1% 95.9% 90.4% 98.9%88.0% 89.8% 90.5% 89.6% 91.9% 96.4% 90.6% 102%87.0% 92.5% 62.0% 100% 97.5% 113% 108% 59.8%86.5% 91.0% 60.0% 98.0% 90.0% 87.0% 101% 74.6%

% Recovery

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐7 ‐ Toxaphene Congeners Spiked in Laboratory Quality Control Samples

Laboratory Type Replicate

ASHLAND MB 1ASHLAND MB 2ASHLAND LCS1 1ASHLAND LCS1 2ASHLAND LCS2 1ASHLAND LCS2 2

EPA_ NEIC MB 1EPA_ NEIC MB 2EPA_ NEIC LCS1 1EPA_ NEIC LCS1 2EPA_ NEIC LCS2 1EPA_ NEIC LCS2 2

EPA_R4_1 MB 1EPA_R4_1 MB 2EPA_R4_1 MB 3EPA_R4_1 LCS1 1EPA_R4_1 LCS1 2EPA_R4_1 LCS1 3EPA_R4_1 LCS2 1EPA_R4_1 LCS2 2EPA_R4_1 LCS2 3EPA_R4_2 MB 1EPA_R4_2 MB 2EPA_R4_2 LCS1 1EPA_R4_2 LCS1 2EPA_R4_2 LCS2 1EPA_R4_2 LCS2 2EPA_R4_3 MB 1EPA_R4_3 MB 2EPA_R4_3 LCS1 1EPA_R4_3 LCS1 2EPA_R4_3 LCS2 1EPA_R4_3 LCS2 2

SCCWRP MB 1SCCWRP MB 2SCCWRP MB 3SCCWRP LCS1 1SCCWRP LCS1 2SCCWRP LCS1 3SCCWRP LCS2 1SCCWRP LCS2 2SCCWRP LCS2 3

EPA_NERL/ORD_LV_1 MB 1EPA_NERL/ORD_LV_1 MB 2EPA_NERL/ORD_LV_1 LCS1 1

EPA_NERL/ORD_LV_1 LCS1 2

EPA_NERL/ORD_LV_1 LCS2 1

EPA_NERL/ORD_LV_1 LCS2 2

EPA_NERL/ORD_LV_2 MB 1EPA_NERL/ORD_LV_2 MB 2EPA_NERL/ORD_LV_2 LCS1 1

EPA_NERL/ORD_LV_2 LCS1 2

EPA_NERL/ORD_LV_2 LCS2 1

EPA_NERL/ORD_LV_2 LCS2 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 P62

1.96 1.03 2.09 0.0966 0.00 0.0996 1.13 9.544.88 9.09 10.5 14.0 9.52 18.2 10.0 13.43.05 3.68 2.37 0.364 0.230 1.21 0.857 6.371.56 1.57 7.64 0.00 8.65 4.49 13.9 9.303.05 3.26 3.29 1.66 1.70 1.56 1.20 1.452.64 3.67 9.39 0.845 0.472 3.75 2.33 2.792.37 2.33 1.19 0.257 1.84 1.78 1.83 0.1072.48 0.499 3.19 1.57 6.72 0.512 5.68 2.35

0.103 0.507 1.59 0.164 1.79 0.995 1.94 2.45

4.49 2.51 7.23 1.09 4.68 2.49 4.06 2.531.18 2.29 3.82 4.06 5.45 7.17 5.04 10.83.56 1.09 7.93 2.37 4.30 6.12 2.15 14.31.20 1.73 7.04 0.923 0.700 3.64 2.69 3.7730.6 43.8 62.8 46.4 4.18 61.4 11.6 1.67

4.93 3.18 5.86 2.50 3.50 0.572 0.188 3.15

0.576 1.63 3.28 2.02 8.00 25.6 6.24 22.0

Relative % Difference (RPD) or Relative Standard Deviation (RSD)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐7 ‐ Toxaphene Congeners Spiked in Laboratory Quality Control Samples

Laboratory Type Replicate

ASHLAND MB 1ASHLAND MB 2ASHLAND LCS1 1ASHLAND LCS1 2ASHLAND LCS2 1ASHLAND LCS2 2

EPA_ NEIC MB 1EPA_ NEIC MB 2EPA_ NEIC LCS1 1EPA_ NEIC LCS1 2EPA_ NEIC LCS2 1EPA_ NEIC LCS2 2

EPA_R4_1 MB 1EPA_R4_1 MB 2EPA_R4_1 MB 3EPA_R4_1 LCS1 1EPA_R4_1 LCS1 2EPA_R4_1 LCS1 3EPA_R4_1 LCS2 1EPA_R4_1 LCS2 2EPA_R4_1 LCS2 3EPA_R4_2 MB 1EPA_R4_2 MB 2EPA_R4_2 LCS1 1EPA_R4_2 LCS1 2EPA_R4_2 LCS2 1EPA_R4_2 LCS2 2EPA_R4_3 MB 1EPA_R4_3 MB 2EPA_R4_3 LCS1 1EPA_R4_3 LCS1 2EPA_R4_3 LCS2 1EPA_R4_3 LCS2 2

SCCWRP MB 1SCCWRP MB 2SCCWRP MB 3SCCWRP LCS1 1SCCWRP LCS1 2SCCWRP LCS1 3SCCWRP LCS2 1SCCWRP LCS2 2SCCWRP LCS2 3

EPA_NERL/ORD_LV_1 MB 1EPA_NERL/ORD_LV_1 MB 2EPA_NERL/ORD_LV_1 LCS1 1

EPA_NERL/ORD_LV_1 LCS1 2

EPA_NERL/ORD_LV_1 LCS2 1

EPA_NERL/ORD_LV_1 LCS2 2

EPA_NERL/ORD_LV_2 MB 1EPA_NERL/ORD_LV_2 MB 2EPA_NERL/ORD_LV_2 LCS1 1

EPA_NERL/ORD_LV_2 LCS1 2

EPA_NERL/ORD_LV_2 LCS2 1

EPA_NERL/ORD_LV_2 LCS2 2

PCB 209 (spiked at

100)

eHCH (spiked at

250) PCB 209 eHCH PCB 209 eHCH PCB 209 eHC

94.4 259 94.4% 104% 94.0 256.0 1.0 2.93.5 253 93.5% 101%87.2 281 87.2% 112% 87.9 274.5 1.6 4.88.6 268 88.6% 107%88.0 261 88.0% 104% 88.6 262.5 1.4 1.89.2 264 89.2% 106%

107 266 107% 107% 105 256.5 3.8 7.103 247 103% 98.7%

99.2 259 99.2% 104% 101 252.5 3.8 5.

103 246 103% 98.3%103 250 103% 100% 103 246.0 1.0 3.104 242 104% 97.0%

96.7 257 96.7% 103% 97.7 256.3 1.0 0.98.0 256 98.0% 103%98.6 256 98.6% 103%82.2 250 82.2% 100% 87.6 245.7 7.2 3.86.1 250 86.1% 100%94.6 237 94.6% 94.8%81.6 263 81.6% 105% 85.8 255.7 8.3 3.81.7 258 81.7% 103%94.0 246 94.0% 98.5%99.7 252 100% 101% 99.3 251.0 0.8 0.98.9 250 98.9% 100%94.7 241 94.7% 96.5% 93.0 245.5 3.5 3.91.4 250 91.4% 100%95.7 245 95.7% 98.1% 94.6 246.0 2.4 0.93.4 247 93.4% 98.6%

100 245 100% 98.0% 101 247.5 1.0 2.101 250 101% 100%

96.7 236 96.7% 94.4% 97.4 236.5 1.5 0.98.2 237 98.2% 95.0%94.1 245 94.1% 97.9% 95.3 243.5 2.5 1.96.5 242 96.5% 96.7%

101 250 101% 100% 102 249.3 0.6 1.102 245 102% 98.0%102 253 102% 101%

94.3 237 94.3% 94.8% 96.8 239.7 2.6 1.96.8 239 96.8% 95.6%99.3 243 99.3% 97.2%

98.6 233 98.6% 93.2% 98.6 238.7 2.4 2.96.3 239 96.3% 95.6%

101 244 101% 97.6%100 224 100% 89.6% 102 230.5 3.0 5.103 237 103% 94.8%

98.4 245 98.4% 98.0% 100 249.5 3.6 3.

102 254 102% 102%

97.2 237 97.2% 94.8% 97.4 248.0 0.3 8.97.5 259 97.5% 104%98.8 239 98.8% 95.7% 98.2 242.0 1.2 2.97.6 245 97.6% 97.9%99.3 229 99.3% 91.8% 97.1 227.5 4.4 1.95.0 226 95.0% 90.3%96.5 229 96.5% 91.5% 95.2 228.0 2.7 0.93.9 227 93.9% 90.9%

Conc (pg/μL) % Recovery Avg Conc (pg/μL) % RPD or RSD

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐8 ‐ Quality Control Samples:

Matrix Spike/Matrix Spike Duplicates ‐ Technical Toxaphene

Parent (pg/μL) Parent Avg (pg/μL) Conc (pg/μL)

Corrected Conc

(pg/μL) % Recovery Avg Conc (pg/μL)

Rela

Dif

ASHLAND MS 1 11.2 10.4 168 158 79.0%ASHLAND MS 2 9.50 197 187 93.5% 173

ASHLAND MSD 1 11.2 10.4 197 186 93.2% 

ASHLAND MSD 2 9.50 174 164 81.9% 175 

EPA_ NEIC MS 1 46.3 42.3 180 138 69.1%EPA_ NEIC MS 2 38.2 193 150 75.2% 144

EPA_ NEIC MSD 1 46.3 42.3 191 149 74.4% 

EPA_ NEIC MSD 2 38.2 189 147 73.4% 148 

EPA_R4_1 MS 1 21.8 17.6 208 191 95.4%EPA_R4_1 MS 2 14.3 232 214 107%EPA_R4_1 MS 3 16.8 212 194 97.1% 200

EPA_R4_1 MSD 1 21.8 17.6 221 203 102% EPA_R4_1 MSD 2 14.3 212 194 97.0% 

EPA_R4_1 MSD 3 16.8 215 197 98.7% 198 

EPA_R4_2 MS 1 12.1 13.4 197 183 91.7%EPA_R4_2 MS 2 14.6 204 191 95.3% 187

EPA_R4_2 MSD 1 12.1 13.4 192 179 89.4% 

EPA_R4_2 MSD 2 14.6 194 181 90.4% 180 

EPA_R4_3 MS 1 9.18 8.91 203 195 97.3%EPA_R4_3 MS 2 8.63 208 199 99.6% 197

EPA_R4_3 MSD 1 9.18 8.91 204 195 97.3% 

EPA_R4_3 MSD 2 8.63 199 190 95.2% 193 

SCCWRP MS 1 4.70 3.97 209 205 103%SCCWRP MS 2 3.70 213 209 105%SCCWRP MS 3 3.50 220 216 108% 210SCCWRP MSD 1 4.70 3.97 201 197 98.5% 

SCCWRP MSD 2 3.70 199 195 97.5% 

SCCWRP MSD 3 3.50 207 203 102% 198 

EPA_NERL/ORD_LV_1 MS 1 8.74 212 203 101%EPA_NERL/ORD_LV_1 MS 2 17.5 223 214 107% 208

EPA_NERL/ORD_LV_1 MSD 1 8.74 214 205 103% EPA_NERL/ORD_LV_1 MSD 2 17.5 218 209 105% 207 EPA_NERL/ORD_LV_2 MS 1 35.2 32.8 203 171 85.3%EPA_NERL/ORD_LV_2 MS 2 30.4 194 161 80.7% 166

EPA_NERL/ORD_LV_2 MSD 1 35.2 32.8 189 156 78.1% 

EPA_NERL/ORD_LV_2 MSD 2 30.4 188 156 77.8% 156 

Toxaphene

Laboratory Type Replicate

Technical Toxaphene Spiked at 200 pg/μL

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐8 ‐ Quality Control Samples:

Matrix Spike/Matrix Spike Duplicates ‐ Technical Toxaphene

ASHLAND MS 1ASHLAND MS 2ASHLAND MSD 1ASHLAND MSD 2

EPA_ NEIC MS 1EPA_ NEIC MS 2EPA_ NEIC MSD 1EPA_ NEIC MSD 2

EPA_R4_1 MS 1EPA_R4_1 MS 2EPA_R4_1 MS 3EPA_R4_1 MSD 1EPA_R4_1 MSD 2EPA_R4_1 MSD 3EPA_R4_2 MS 1EPA_R4_2 MS 2EPA_R4_2 MSD 1EPA_R4_2 MSD 2EPA_R4_3 MS 1EPA_R4_3 MS 2EPA_R4_3 MSD 1EPA_R4_3 MSD 2

SCCWRP MS 1SCCWRP MS 2SCCWRP MS 3SCCWRP MSD 1SCCWRP MSD 2SCCWRP MSD 3

EPA_NERL/ORD_LV_1 MS 1EPA_NERL/ORD_LV_1 MS 2

EPA_NERL/ORD_LV_1 MSD 1EPA_NERL/ORD_LV_1 MSD 2

EPA_NERL/ORD_LV_2 MS 1EPA_NERL/ORD_LV_2 MS 2

EPA_NERL/ORD_LV_2 MSD 1EPA_NERL/ORD_LV_2 MSD 2

Laboratory Type Replicate Conc (pg/μL) % Recovery

Relative Percent

Difference (%) Avg RPD (%)

62.9 62.9%62.6 62.6%62.4 62.4% 0.79859.4 59.4% 5.25 3.0270.9 70.9%74.3 74.3%68.8 68.8% 2.9970.1 70.1% 5.83 4.4168.6 68.6%68.0 68.0%69.5 69.5%67.7 67.7% 1.3468.3 68.3% 0.39667.1 67.1% 3.51 1.7570.1 70.1%67.0 67.0%65.9 65.9% 6.2665.8 65.8% 1.76 4.0166.6 66.6%68.8 68.8%64.2 64.2% 3.7063.4 63.4% 8.23 5.9674.5 74.5%70.5 70.5%71.1 71.1%66.7 66.7% 11.067.4 67.4% 4.5069.3 69.3% 2.56 6.0467.2 67.2%68.5 68.5%65.8 65.8% 2.1165.4 65.4% 4.63 3.3775.6 75.6%76.8 76.8%74.0 74.0% 2.0373.3 73.3% 4.60 3.31

PCB 209 (Surrogate) Spiked at 100

pg/μL

PCB 209

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐8 ‐ Quality Control Samples:

Matrix Spike/Matrix Spike Duplicates ‐ Technical Toxaphene

ASHLAND MS 1ASHLAND MS 2ASHLAND MSD 1ASHLAND MSD 2

EPA_ NEIC MS 1EPA_ NEIC MS 2EPA_ NEIC MSD 1EPA_ NEIC MSD 2

EPA_R4_1 MS 1EPA_R4_1 MS 2EPA_R4_1 MS 3EPA_R4_1 MSD 1EPA_R4_1 MSD 2EPA_R4_1 MSD 3EPA_R4_2 MS 1EPA_R4_2 MS 2EPA_R4_2 MSD 1EPA_R4_2 MSD 2EPA_R4_3 MS 1EPA_R4_3 MS 2EPA_R4_3 MSD 1EPA_R4_3 MSD 2

SCCWRP MS 1SCCWRP MS 2SCCWRP MS 3SCCWRP MSD 1SCCWRP MSD 2SCCWRP MSD 3

EPA_NERL/ORD_LV_1 MS 1EPA_NERL/ORD_LV_1 MS 2

EPA_NERL/ORD_LV_1 MSD 1EPA_NERL/ORD_LV_1 MSD 2

EPA_NERL/ORD_LV_2 MS 1EPA_NERL/ORD_LV_2 MS 2

EPA_NERL/ORD_LV_2 MSD 1EPA_NERL/ORD_LV_2 MSD 2

Laboratory Type Replicate Conc (pg/μL) % Recovery

Relative Percent

Difference (%) Avg RPD (%)

227 90.6%233 93.0%220 88.2% 2.73233 93.0% 1.36199 79.7%216 86.5%210 83.9% 5.11210 83.8% 3.13 4.12201 80.6%209 83.4%196 78.6%199 79.6% 1.24201 80.6% 3.46202 80.6% 2.57 2.42189 75.5%202 80.6%195 78.2% 3.41194 77.6% 3.80 3.61202 80.8%198 79.4%199 79.7% 1.45205 81.8% 3.08 2.27193 77.2%191 76.4%193 77.2%189 75.6% 2.09189 75.6% 1.05191 76.4% 1.04 1.40189 75.4%193 77.0%186 74.2% 1.55190 75.8% 1.57 1.56201 80.5%203 81.4%201 80.5% 0.0497205 82.0% 0.784 0.417

eHCH (Surrogate) Spiked at 250 pg/μL

eHCH

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐9 ‐ Quality Control Samlpes Matrix Spike/Matrix Spike Duplicate ‐ Congeners

Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 P

Laboratory Type ReplicateASHLAND MS 1 101 99.1 89.8 95.2 93.3 95.3 90.2 2ASHLAND MS 2 102 100 91.6 94.7 93.4 92.6 87.6 2ASHLAND MSD 1 102 99.5 87.4 92.0 90.8 89.0 82.7 1ASHLAND MSD 2 97.4 95.8 84.4 91.1 88.8 88 81.4 1EPA_ NEIC MS 1 88.1 88.8 89.7 92.1 92.1 96.1 91.9 2EPA_ NEIC MS 2 88.5 89.4 90.7 91.6 91.6 96.4 91.7 2EPA_ NEIC MSD 1 86.6 86.5 85.6 88.9 89.3 92.5 87.2 2

EPA_ NEIC MSD 2 86.1 86.0 86.6 88.8 88.9 93.2 86.6 2

EPA_R4_1 MS 1 98.7 96.9 91.6 96.5 96.1 102 94.7 2EPA_R4_1 MS 2 103 102 95.6 100 100 106 96.3 2EPA_R4_1 MS 3 105 103 98.1 101 101 107 98.4 2EPA_R4_1 MSD 1 97.4 94.9 86.4 94.0 92.8 97.0 89.5 2EPA_R4_1 MSD 2 95.8 93.6 85.8 92.0 92.4 96.7 88.1 2EPA_R4_1 MSD 3 98.4 97.1 88.4 94.7 93.8 99.1 90.0 2EPA_R4_2 MS 1 94.9 91.1 85.3 92.5 91.4 93.7 89.2 2EPA_R4_2 MS 2 94.1 90.2 85.1 92.6 91.2 94.3 90.0 2EPA_R4_2 MSD 1 90.7 87.1 79.2 88.7 87.9 89.8 84.7 2EPA_R4_2 MSD 2 90.6 86.5 80.6 88.7 86.8 89.3 85.1 2EPA_R4_3 MS 1 91.3 89.6 85.9 90.9 90.7 92.6 88.7 2EPA_R4_3 MS 2 90.8 90.7 88.1 90.6 90.8 93.9 88.5 2EPA_R4_3 MSD 1 90.6 90.0 85.1 88.0 88.4 90.0 85.4 2EPA_R4_3 MSD 2 87.7 87.0 82.9 87.7 87.0 89.2 82.9 2SCCWRP MS 1 87.4 89.8 85.1 92.2 93.5 98.5 91.4 2SCCWRP MS 2 92.5 92.8 88.9 91.1 93.9 97.3 92.5 2SCCWRP MS 3 92.8 93.8 93.7 97.9 101 106 99.3 2SCCWRP MSD 1 87.4 87.3 81.6 88.2 88.1 90.6 86.1 2SCCWRP MSD 2 88.1 89.0 86.0 91.3 92.4 97.2 90.6 2SCCWRP MSD 3 89.9 90.7 86.2 93.9 96.4 103 93.5 2EPA_NERL/ORD_LV_1 MS 1 84.5 86.9 74.2 76.6 77.2 76.9 74.9 1EPA_NERL/ORD_LV_1 MS 2 84.3 84.0 83.2 79.7 76.3 77.5 77.5 1EPA_NERL/ORD_LV_1 MSD 1 81.1 84.5 71.5 77.7 74.6 71.9 70.6 1EPA_NERL/ORD_LV_1 MSD 2 82.5 87.0 77.0 78.8 73.5 78.6 71.9 1EPA_NERL/ORD_LV_2 MS 1 87.6 86.1 92.1 92.4 93.3 104 95.2 2EPA_NERL/ORD_LV_2 MS 2 89.5 88.2 91.1 94.6 96.9 107 99.5 2EPA_NERL/ORD_LV_2 MSD 1 86.3 84.7 85.0 90.8 91.9 98.5 93.7 2EPA_NERL/ORD_LV_2 MSD 2 84.6 83.5 84.5 90.9 90.1 100 91.0 2

Hx‐Sed, Hp‐Sed, P26, P40, P41, P44, P50 Spiked at 100 pg/μL, P62 Spiked at 226 pg

Concentration (pg/μL)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐9 ‐ Quality Control Samlpes Matrix Spike/Matrix Spike Duplicate ‐ Congeners

Laboratory Type ReplicateASHLAND MS 1ASHLAND MS 2ASHLAND MSD 1ASHLAND MSD 2EPA_ NEIC MS 1EPA_ NEIC MS 2EPA_ NEIC MSD 1

EPA_ NEIC MSD 2

EPA_R4_1 MS 1EPA_R4_1 MS 2EPA_R4_1 MS 3EPA_R4_1 MSD 1EPA_R4_1 MSD 2EPA_R4_1 MSD 3EPA_R4_2 MS 1EPA_R4_2 MS 2EPA_R4_2 MSD 1EPA_R4_2 MSD 2EPA_R4_3 MS 1EPA_R4_3 MS 2EPA_R4_3 MSD 1EPA_R4_3 MSD 2SCCWRP MS 1SCCWRP MS 2SCCWRP MS 3SCCWRP MSD 1SCCWRP MSD 2SCCWRP MSD 3EPA_NERL/ORD_LV_1 MS 1EPA_NERL/ORD_LV_1 MS 2EPA_NERL/ORD_LV_1 MSD 1EPA_NERL/ORD_LV_1 MSD 2EPA_NERL/ORD_LV_2 MS 1EPA_NERL/ORD_LV_2 MS 2EPA_NERL/ORD_LV_2 MSD 1EPA_NERL/ORD_LV_2 MSD 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 P

101 99.1 89.8 95.2 93.3 95.3 90.2 9102 100 91.6 94.7 93.4 92.6 87.6 9102 99.5 87.4 92.0 90.8 89.0 82.7 8

97.4 95.8 84.4 91.1 88.8 88.0 81.4 888.1 88.8 89.7 92.1 92.1 96.1 91.9 988.5 89.4 90.7 91.6 91.6 96.4 91.7 986.6 86.5 85.6 88.9 89.3 92.5 87.2 986.1 86.0 86.6 88.8 88.9 93.2 86.6 998.7 96.9 91.6 96.5 96.1 102 94.7 1

103 102 95.6 100 100 106 96.3 1105 103 98.1 101 101 107 98.4 1

97.4 94.9 86.4 94.0 92.8 97.0 89.5 195.8 93.6 85.8 92.0 92.4 96.7 88.1 198.4 97.1 88.4 94.7 93.8 99.1 90.0 194.9 91.1 85.3 92.5 91.4 93.7 89.2 994.1 90.2 85.1 92.6 91.2 94.3 90.0 190.7 87.1 79.2 88.7 87.9 89.8 84.7 990.6 86.5 80.6 88.7 86.8 89.3 85.1 991.3 89.6 85.9 90.9 90.7 92.6 88.7 190.8 90.7 88.1 90.6 90.8 93.9 88.5 190.6 90.0 85.1 88.0 88.4 90.0 85.4 987.7 87 82.9 87.7 87 89.2 82.9 987.4 89.8 85.1 92.2 93.5 98.5 91.4 192.5 92.8 88.9 91.1 93.9 97.3 92.5 192.8 93.8 93.7 97.9 101 106 99.3 187.4 87.3 81.6 88.2 88.1 90.6 86.1 988.1 89.0 86.0 91.3 92.4 97.2 90.6 189.9 90.7 86.2 93.9 96.4 103 93.5 184.5 86.9 74.2 76.6 77.2 76.9 74.9 784.3 84.0 83.2 79.7 76.3 77.5 77.5 681.1 84.5 71.5 77.7 74.6 71.9 70.6 782.5 87.0 77.0 78.8 73.5 78.6 71.9 787.6 86.1 92.1 92.4 93.3 104 95.2 189.5 88.2 91.1 94.6 96.9 107 99.5 186.3 84.7 85.0 90.8 91.9 98.5 93.7 184.6 83.5 84.5 90.9 90.1 100 91.0 1

% Recovery

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐9 ‐ Quality Control Samlpes Matrix Spike/Matrix Spike Duplicate ‐ Congeners

Laboratory Type ReplicateASHLAND MS 1ASHLAND MS 2ASHLAND MSD 1ASHLAND MSD 2EPA_ NEIC MS 1EPA_ NEIC MS 2EPA_ NEIC MSD 1

EPA_ NEIC MSD 2

EPA_R4_1 MS 1EPA_R4_1 MS 2EPA_R4_1 MS 3EPA_R4_1 MSD 1EPA_R4_1 MSD 2EPA_R4_1 MSD 3EPA_R4_2 MS 1EPA_R4_2 MS 2EPA_R4_2 MSD 1EPA_R4_2 MSD 2EPA_R4_3 MS 1EPA_R4_3 MS 2EPA_R4_3 MSD 1EPA_R4_3 MSD 2SCCWRP MS 1SCCWRP MS 2SCCWRP MS 3SCCWRP MSD 1SCCWRP MSD 2SCCWRP MSD 3EPA_NERL/ORD_LV_1 MS 1EPA_NERL/ORD_LV_1 MS 2EPA_NERL/ORD_LV_1 MSD 1EPA_NERL/ORD_LV_1 MSD 2EPA_NERL/ORD_LV_2 MS 1EPA_NERL/ORD_LV_2 MS 2EPA_NERL/ORD_LV_2 MSD 1EPA_NERL/ORD_LV_2 MSD 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 P

101 99.8 90.7 95.0 93.4 94.0 88.9 2

99.5 97.7 85.9 91.6 89.8 88.5 82.1 188.3 89.1 90.2 91.8 91.9 96.3 91.8 286.3 86.3 86.1 88.8 89.1 92.9 86.9 2

102 101 95.1 99.3 99 105 96.5 2

97.2 95.2 86.8 93.5 93.0 97.6 89.2 294.5 90.7 85.2 92.6 91.3 94.0 89.6 290.6 86.8 79.9 88.7 87.4 89.6 84.9 291.1 90.2 87.0 90.7 90.7 93.2 88.6 289.1 88.5 84.0 87.8 87.7 89.6 84.2 290.9 92.1 89.2 93.7 96.1 101 94.4 288.5 89 84.6 91.1 92.3 96.9 90.1 284.4 85.5 78.7 78.2 76.8 77.2 76.2 181.8 85.8 74.3 78.3 74.1 75.3 71.3 188.6 87.1 91.6 93.5 95.1 105 97.4 285.5 84.1 84.7 90.9 91.0 99.2 92.3 2

Average Concentration (pg/μL)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐9 ‐ Quality Control Samlpes Matrix Spike/Matrix Spike Duplicate ‐ Congeners

Laboratory Type ReplicateASHLAND MS 1ASHLAND MS 2ASHLAND MSD 1ASHLAND MSD 2EPA_ NEIC MS 1EPA_ NEIC MS 2EPA_ NEIC MSD 1

EPA_ NEIC MSD 2

EPA_R4_1 MS 1EPA_R4_1 MS 2EPA_R4_1 MS 3EPA_R4_1 MSD 1EPA_R4_1 MSD 2EPA_R4_1 MSD 3EPA_R4_2 MS 1EPA_R4_2 MS 2EPA_R4_2 MSD 1EPA_R4_2 MSD 2EPA_R4_3 MS 1EPA_R4_3 MS 2EPA_R4_3 MSD 1EPA_R4_3 MSD 2SCCWRP MS 1SCCWRP MS 2SCCWRP MS 3SCCWRP MSD 1SCCWRP MSD 2SCCWRP MSD 3EPA_NERL/ORD_LV_1 MS 1EPA_NERL/ORD_LV_1 MS 2EPA_NERL/ORD_LV_1 MSD 1EPA_NERL/ORD_LV_1 MSD 2EPA_NERL/ORD_LV_2 MS 1EPA_NERL/ORD_LV_2 MS 2EPA_NERL/ORD_LV_2 MSD 1EPA_NERL/ORD_LV_2 MSD 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 P

0.891 0.403 2.71 3.42 2.72 6.84 8.68 1

4.32 4.69 8.18 3.88 5.05 5.09 7.34 91.77 2.66 4.60 3.64 3.11 3.74 5.17 52.81 3.80 4.64 3.08 3.06 3.45 5.75 31.38 2.09 5.81 2.68 3.42 5.34 5.60 67.41 8.49 10.9 8.78 8.13 9.48 8.87 56.35 6.27 10.4 6.55 6.96 7.23 8.92 54.52 4.55 7.47 4.20 3.91 4.25 5.13 33.87 4.21 5.52 4.32 4.84 5.49 5.62 4

0.847 0.390 0.935 3.28 2.49 2.86 3.72 5

3.51 4.14 6.12 3.19 4.25 5.10 6.51 70.00 2.82 4.20 4.43 5.95 8.36 5.97 94.87 4.18 3.32 0.219 1.61 0.103 2.08 23.17 3.36 8.34 4.17 4.66 2.87 6.02 64.11 2.80 3.71 1.43 3.43 6.72 5.91 22.16 3.51 7.74 1.14 3.74 1.41 7.50 51.53 1.60 7.95 1.79 1.54 5.26 1.65 05.63 5.37 7.60 3.96 7.28 6.71 8.96 9

Relative Percent Difference (% RPD)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐9 ‐ Quality Control Samlpes Matrix Spike/Matrix Spike Duplicate ‐ Congeners

Laboratory Type ReplicateASHLAND MS 1ASHLAND MS 2ASHLAND MSD 1ASHLAND MSD 2EPA_ NEIC MS 1EPA_ NEIC MS 2EPA_ NEIC MSD 1

EPA_ NEIC MSD 2

EPA_R4_1 MS 1EPA_R4_1 MS 2EPA_R4_1 MS 3EPA_R4_1 MSD 1EPA_R4_1 MSD 2EPA_R4_1 MSD 3EPA_R4_2 MS 1EPA_R4_2 MS 2EPA_R4_2 MSD 1EPA_R4_2 MSD 2EPA_R4_3 MS 1EPA_R4_3 MS 2EPA_R4_3 MSD 1EPA_R4_3 MSD 2SCCWRP MS 1SCCWRP MS 2SCCWRP MS 3SCCWRP MSD 1SCCWRP MSD 2SCCWRP MSD 3EPA_NERL/ORD_LV_1 MS 1EPA_NERL/ORD_LV_1 MS 2EPA_NERL/ORD_LV_1 MSD 1EPA_NERL/ORD_LV_1 MSD 2EPA_NERL/ORD_LV_2 MS 1EPA_NERL/ORD_LV_2 MS 2EPA_NERL/ORD_LV_2 MSD 1EPA_NERL/ORD_LV_2 MSD 2

Hx‐Sed Hp‐Sed P26 P40 P41 P44 P50 P

2.61 2.55 5.45 3.65 3.88 5.97 8.01 92.29 3.23 4.62 3.36 3.08 3.60 5.46 45.04 5.61 9.04 6.00 6.17 7.35 7.80 54.19 4.38 6.49 4.26 4.38 4.87 5.38 32.18 2.27 3.53 3.23 3.37 3.98 5.12 62.68 3.45 5.28 2.94 4.07 3.78 4.69 63.13 3.15 5.72 1.28 3.58 4.06 6.70 33.58 3.49 7.77 2.87 4.41 5.98 5.31 4

Average Relative Percent Difference (% RPD)

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐9 ‐ Quality Control Samlpes Matrix Spike/Matrix Spike Duplicate ‐ Congeners

Laboratory Type ReplicateASHLAND MS 1ASHLAND MS 2ASHLAND MSD 1ASHLAND MSD 2EPA_ NEIC MS 1EPA_ NEIC MS 2EPA_ NEIC MSD 1

EPA_ NEIC MSD 2

EPA_R4_1 MS 1EPA_R4_1 MS 2EPA_R4_1 MS 3EPA_R4_1 MSD 1EPA_R4_1 MSD 2EPA_R4_1 MSD 3EPA_R4_2 MS 1EPA_R4_2 MS 2EPA_R4_2 MSD 1EPA_R4_2 MSD 2EPA_R4_3 MS 1EPA_R4_3 MS 2EPA_R4_3 MSD 1EPA_R4_3 MSD 2SCCWRP MS 1SCCWRP MS 2SCCWRP MS 3SCCWRP MSD 1SCCWRP MSD 2SCCWRP MSD 3EPA_NERL/ORD_LV_1 MS 1EPA_NERL/ORD_LV_1 MS 2EPA_NERL/ORD_LV_1 MSD 1EPA_NERL/ORD_LV_1 MSD 2EPA_NERL/ORD_LV_2 MS 1EPA_NERL/ORD_LV_2 MS 2EPA_NERL/ORD_LV_2 MSD 1EPA_NERL/ORD_LV_2 MSD 2

PCB 209 eHCH PCB 209 eHCH PCB 209 eHCH PCB 209 eHCH 

73.8 253 73.8 10173.3 259 73.3 103 73.6 25662.2 270 62.2 108 17.1 6.4665.1 252 65.1 101 63.7 261 11.8 2.78 86.2 234 86.2 93.886.8 240 86.8 96.0 86.5 23775.2 227 75.2 90.7 13.6 3.3472.3 225 72.3 89.9 73.7 226 18.2 6.58 78.0 230 78.0 92.068.2 237 68.2 94.966.8 245 66.8 97.9 71.0 23768.0 232 68.0 92.9 13.7 0.88768.4 233 68.4 93.1 0.249 1.8562.0 237 62.0 95.0 66.1 234 7.42 3.06 74.9 222 74.9 89.078.6 220 78.6 88.1 76.8 22169.1 217 69.1 87.0 8.07 2.2569.4 216 69.4 86.6 69.3 217 12.4 1.81 79.7 219 79.7 87.480.1 216 80.1 86.5 79.9 21768.7 224 68.7 89.5 14.8 2.3868.0 218 68.0 87.1 68.3 221 16.3 0.677 82.1 213 82.1 85.283.1 218 83.1 87.288.1 223 88.1 89.2 84.4 21873.3 214 73.3 85.6 11.3 0.46874.8 215 74.8 86.0 10.5 1.3976.2 223 76.2 89.2 74.8 217 14.5 0.00 81.7 219 81.7 87.681.8 222 81.8 88.8 81.8 22169.3 219 69.3 87.6 16.4 0.0070.2 241 70.2 96.4 69.8 230 15.3 8.21 81.3 217 81.3 86.982.5 229 82.5 91.7 81.9 22371.8 225 71.8 90.2 12.4 3.7671.1 225 71.1 89.9 71.4 225 14.8 1.93 

Concentration (pg/μL) Avg Conc (pg/μL) % RPD

PCB 209 (Surrogate) Spiked at 100 pg/μL, eHCH (Surrogate) Spiked at 250 pg/μ

% Recovery 

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Table A2‐10 ‐ Laboratory Participants

Laboratory DesignationASHLANDEPA_ NEICEPA_NERL/ORD_LV_1 Analyst 1EPA_NERL/ORD_LV_2 Analyst 2EPA_R4_1 RefereeEPA_R4_2 Analyst 1EPA_R4_3 Analyst 2SCCWRP

Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:

Analytical Data Report
Attachment 3 

Final Phase III Toxaphene Summary Results with Z values 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:August 2012   

Analytical Data Report    Attachment 3

   

Table A3-1 

Z-Scores for Laboratory Quality Assurance Samples 

Laboratory 

ASHLAND 

EPA_ NEIC 

EPA_R4_1 EPA_R4_2 EPA_R4_3 

SCCWRP 

EPA_NERL/ORD_1 EPA_NERL/ORD_2 

 Analyte 

Second 

Source 

Standard 

Toxaphene -0.18 0.15 0.17 0.16 0.13 -0.27 -0.45 0.17 

PCB 209 -0.02 0.02 0.09 0.10 0.07 -0.12 -0.12 -0.03 

eHCH -0.19 -0.05 0.02 -0.11 -0.13 -0.16 0.40 0.21 

LCS1 

Toxaphene -0.04 0.50 0.23 0.01 -0.96 -0.83 0.15 0.98 

PCB 209 -0.22 0.02 0.01 -0.07 -0.05 0.09 0.00 0.05 

eHCH 0.63 0.45 0.02 -0.08 -0.05 -0.11 -0.63 -0.10 

Hx-Sed 0.38 0.06 0.25 0.08 -0.08 -0.01 -0.28 -0.35 

Hp-Sed 0.34 0.05 0.27 -0.02 -0.11 0.07 -0.28 -0.33 

P26 0.12 0.10 0.26 -0.03 -0.07 0.09 -0.42 -0.21 

P40 0.20 0.07 0.26 0.10 -0.03 0.09 -0.48 -0.32 

P41 0.12 0.06 0.27 0.06 -0.03 0.14 -0.54 -0.23 

P44 0.01 0.05 0.39 0.11 0.01 0.12 -0.82 -0.16 

P50 0.01 0.06 0.32 0.12 0.01 0.16 -0.65 -0.29 

P62 0.11 -0.17 0.63 0.23 0.11 0.01 -0.90 -0.21 

LCS2 

Toxaphene 0.54 -0.06 0.23 -0.12 -0.53 0.17 -0.08 -0.04 

PCB 209 -0.27 0.09 -0.41 0.01 0.09 0.15 0.08 0.23 

eHCH 0.40 0.29 0.20 -0.06 -0.09 -0.22 -0.37 -0.09 

Hx-Sed 0.09 0.06 0.54 0.12 0.10 -0.30 -0.26 -0.45 

Hp-Sed 0.63 -0.02 0.28 0.03 0.01 -0.17 -0.19 -0.31 

P26 0.34 0.52 0.69 0.08 0.50 -0.14 -1.00 -1.35 

P40 0.72 0.16 0.21 -0.07 -0.22 -0.09 -0.55 0.07 

P41 0.33 -0.11 0.18 -0.19 -0.21 -0.18 0.71 -0.31 

P44 0.79 0.00 0.31 -0.10 0.00 -0.05 -0.68 -0.02 

P50 -0.23 0.15 0.20 -0.16 -0.09 -0.15 -0.08 0.14 

P62 0.35 0.43 0.83 0.43 0.41 -0.33 -1.73 -0.70 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation:August 2012   

Analytical Data Report    Attachment 3

   

Laboratory 

ASHLAND 

EPA_ NEIC 

EPA_R4_1 EPA_R4_2 EPA_R4_3 

SCCWRP 

EPA_NERL/ORD_1 EPA_NERL/ORD_2 

 Analyte 

MS 

Toxaphene -0.63 -0.62 0.25 -0.02 0.20 0.47 0.44 -0.46 

PCB 209 -0.39 -0.02 -0.05 -0.06 -0.11 0.14 -0.10 0.37 

eHCH 0.49 0.28 0.00 -0.13 -0.03 -0.19 -0.23 0.01 

Hx-Sed 0.32 -0.01 0.39 0.06 -0.09 -0.09 -0.37 -0.19 

Hp-Sed 0.29 0.02 0.36 -0.07 -0.10 -0.01 -0.30 -0.23 

P26 0.04 0.08 0.28 -0.16 -0.08 0.02 -0.46 0.12 

P40 0.12 0.02 0.30 0.01 -0.07 0.06 -0.62 0.05 

P41 0.04 0.00 0.28 -0.05 -0.07 0.16 -0.68 0.12 

P44 -0.05 -0.06 0.35 -0.10 -0.14 0.17 -0.80 0.37 

P50 -0.03 -0.02 0.24 -0.06 -0.10 0.15 -0.65 0.28 

P62 -0.30 -0.27 0.53 -0.03 -0.01 0.23 -1.21 0.66 

MSD 

Toxaphene 0.06 -0.66 0.32 -0.08 0.19 0.32 0.51 -0.61 

PCB 209 -0.27 -0.05 0.04 -0.07 -0.19 0.05 -0.08 0.40 

eHCH 0.39 0.32 -0.01 -0.12 0.02 -0.23 -0.27 0.04 

Hx-Sed 0.50 -0.01 0.31 0.02 -0.04 -0.07 -0.37 -0.21 

Hp-Sed 0.45 0.00 0.26 -0.12 -0.04 -0.02 -0.17 -0.24 

P26 0.18 0.09 0.16 -0.18 0.02 0.05 -0.45 0.06 

P40 0.12 0.02 0.19 -0.02 -0.06 0.09 -0.49 0.07 

P41 0.10 0.02 0.20 -0.05 -0.04 0.17 -0.66 0.11 

P44 -0.12 -0.03 0.25 -0.10 -0.10 0.22 -0.72 0.32 

P50 -0.14 -0.02 0.17 -0.03 -0.07 0.21 -0.67 0.31 

P62 -0.50 -0.32 0.48 0.01 -0.06 0.24 -0.96 0.67 

 

Z-scores for each participant and analyte all fell into the satisfactory category (|z| ≤ 2), with all 

scores falling between -1.73 and 0.98. These results indicate that there is an acceptable level of 

consistency between laboratories within the confines of this study.