# Method 8276

Technical Toxaphene and Toxaphene Co ngeners 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. Analyti cal Data .......................................................................................................... ............................. 3

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

TABLES

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

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

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

Samples

Table A1-1: Phase III Multi-laboratory Validati on 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 M ass 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 Labor atory Quality Assurance Samples

# Method	8276	U.S.	EPA	ORCR	Inter‐la boratory	Validation:		 August 2012

Analytical	Data	Report

1 

# I. Introduction

SW-846 Method 8276 is presently u nder development for the analys is of technical toxaphene

and toxaphene congeners using gas chromatogr aphy-negative ion chem ical ionization mass

spectrometry (GC-NICI/MS). Phase I and Phas e 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 th is current Phase III Inter-laboratory Validation

Study is to evaluate the use of Method 8276 fo r the analysis of te chnical toxaphene and

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

evaluated to determine reliabili ty, reproducibility, linearity, ac curacy and precision of the

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

using Method 8276. The compounds listed in Tabl e 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-Hexachlo robornane (Hx-Sed) 57981-29-0

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

2-endo,3-exo,5-endo,6-exo,8,8,10,10-Oc tachlorobornane (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-Oc tachlorobornane (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 ex traction, cleanup, concentr ation, and spiking as

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

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

extracts before shipping to participating labora tories for analysis. W ith the exception of the

referee chemist, none of the laboratory particip ants 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 Met hod 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‐la boratory	Validation:		 August 2012

Analytical	Data	Report

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# The following laboratories participated in Phase III of this study:

Ashland (formerly Hercules),

EPA National Enforcement Inve stigation Center (NEIC),

EPA Office of Research Devel opment Las Vegas, Analyst 1,

EPA Office of Research Devel opment 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 Wa ter 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 Surrogates 8



# (pg/uL) Internal

Std 9



# (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 Std 11 

# 100 250 50 150 NA 2 2 1

ORS 1 

# 50 NA NA 1 1 1

MB 2 

# 100 250 50 NA NA 2 4 1

LCS1 3 

# 100 250 50 Unk Unk 2 4 2

Source Fish Matrix 4 

# 100 250 50 NA NA 2 4 1

LCS2 5 

# 100 250 50 Unk Unk 2 4 2

MS/MSD 6 

# 100 250 50 Unk Unk 2 8 4

Terry Creek 1 7 

# 100 250 50 NA NA 2 4 2

Terry Creek 2 7 

# 100 250 50 NA NA 2 4 2

Total 48 29

1 

# ORS - Oxygen Reaction Standard – Anal yzed daily to demonstrate the absen ce 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 w ith surrogates, carried thr ough extraction and clean-up.

3 

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

congeners or technical toxaphene and car ried 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‐la boratory	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 carri ed through extraction and clean-up.

6 

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

congeners or technical toxaphene and car ried through extraction and clean-up.

7 

# Terry Creek 1 and 2 - Fish collected fr om Terry Creek from the toxaphene plan t with incurred residues spiked with

surrogates and carried thr ough 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 fina l 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 de tected 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 ge nerated for each quality control sample and

averaged for each laboratory participant. In accordance with Internati onal 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 cr iterion. Z-scores are calculat ed using the following formula:

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

where x is the individual laborato ry analytical result, X is th e “exercise assigned value,” and σ is

the established target value or cr iterion. Z-scores for this study we re calculated using an exercise

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

(i.e., MS, MSD, LCS1, LCS2 and Second Source St andard). 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 – av erage recovery) / (25% average recovery)

# Method	8276	U.S.	EPA	ORCR	Inter‐la boratory	Validation:		 August 2012

Analytical	Data	Report

4 

# 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 categor izing Z-scores includes the following (IUPAC

1993):

 |z| ≤ 2  Satisfactory

 2< |z| < 3  Questionable

 |z| ≥ 3  Unsatisfactory

# Attachment 1

Summarized Analytical Data fo r Fish Tissue Extracts and

Laboratory Quality Control Samples

# Method	8276	U.S.	EPA	ORCR	Inter‐la boratory	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

CLEANUP 1



# 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‐la boratory	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 Met hod

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

cell using activated, acidified (30% H 2 

# SO 4 

# ) silica gel per Method 3665A and Method 3630C. These extracts were

further subjected to cleanup using a Flor isil® 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‐la boratory	Validation:		 August 2012

Analytical	Data	Report	 	 Attachment	1 

# Table A1-2

PHASE III MULTI-LABORATORY VALIDATIO N DATA USING SPIKED LABORATORY

QUALITY CONTROL SAMPLES CARRIED THROUGH EXTRACTION AND CLEANUP 1



# Technical Toxaphene

ID No. of

Participants True

Value

(pg/ μ L) Grand

Mean

(pg/ μ L) %

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‐la boratory	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‐la boratory	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 Accelerate d Solvent Extractor (ASE) using a modified version

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

in the ASE extraction cell usi ng activated, acidified (30% H 2 

# SO 4 

# ) 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 TablesTableA2‐1‐TechnicalToxapheneinAlaskanCodSourceFishLaboratory Replicate ToxaphenePCB209(spikedat100)eHCH(spikedat250)PCB209 eHCH PCB209 eHCH PCB209 eHCHASHLAND1 11.2 77.4 26977.4 108 75.7 280 4.49 7.99ASHLAND2 9.50 74.0 29274.0 117EPA_NEIC1 46.3 84.8 24384.8 97.0 84.3 246 1.20 3.01EPA_NEIC2 38.2 83.8 25083.8 100EPA_R4_11 21.8 66.8 24566.8 98.1 76.0 238 10.6 2.74EPA_R4_12 14.3 80.1 23380.1 93.4EPA_R4_13 16.8 81.2 23481.2 93.7EPA_R4_21 12.1 77.3 23177.3 92.3 78.2 229 2.47 1.73EPA_R4_22 14.6 79.2 22779.2 90.7EPA_R4_31 9.18 80.0 23680.0 94.5 79.1 237 2.40 0.321EPA_R4_32 8.63 78.1 23778.1 94.8SCCWRP1 4.70 83.7 23283.7 92.8 83.3 227 2.15 1.92SCCWRP2 3.70 81.3 22481.3 89.6SCCWRP3 3.50 84.8 22584.8 90.0EPA_NERL/ORD_LV_11 ND 80.4 23380.4 93.4 79.9 227 1.25 5.37EPA_NERL/ORD_LV_12 17.5 79.4 22179.4 88.5EPA_NERL/ORD_LV_21 35.2 88.2 23388.2 93.0 88.2 234 0.0454 1.11EPA_NERL/ORD_LV_22 30.4 88.1 23588.1 94.1HighlightedcellshaveconcentrationsbelowtheLLOQof50pg/μL.Note:TheAlaskanCodSourceFishisacleanmatrix.Concentration(pg/μL)%RPDorRSD%RecoveryAvgConcentration(pg/μL)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐2‐ToxapheneCongenersinAlaskanCodSourceFishLaboratory Rep Hx‐SedHp‐Sed P26P40 P41 P44 P50P62ASHLAND 1 ND ND ND ND ND ND ND NDASHLAND 2 ND ND 0.200 ND ND ND ND NDEPA_NEIC 1 <0.0800 <0.200 <0.300 <0.0800 <0.0600 <0.200 <0.100 <3.00EPA_NEIC 2 <0.0800 <0.200 <0.300 <0.0800 <0.0600 <0.200 <0.100 <3.00EPA_R4_1 1 0.0300 0.0500 0.280 0.0300 0.0600 0.0400 0.170 0.200EPA_R4_1 2 0.0300 0.0400 0.320 0.0500 0.0700 0.0600 0.180 0.150EPA_R4_1 3 0.0400 0.0700 0.240 0.0200 0.0700 0.0900 0.220 0.330EPA_R4_2 1 ND ND ND ND ND ND ND NDEPA_R4_2 2 ND ND ND ND ND ND ND NDEPA_R4_3 1 ND ND ND ND ND ND ND NDEPA_R4_3 2 ND ND ND ND ND ND ND NDSCCWRP 1 ND ND 0.140 ND ND ND 0.160 NDSCCWRP 2 ND ND 0.280 ND ND ND 0.190 NDSCCWRP 3 ND ND 0.260 ND ND ND 0.160 NDEPA_NERL/ORD_LV_11 0.360 0.270 1.26 0.580 0.720 0.820 0.700 1.23EPA_NERL/ORD_LV_12 0.320 0.270 0.930 0.580 0.660 0.810 0.720 1.21EPA_NERL/ORD_LV_21ND ND ND ND ND 0.340 0.550 NDEPA_NERL/ORD_LV_22ND ND ND ND 0.190 ND 0.560 NDHighlightedcellshaveconcentrationsbelowtheLLOQof1pg/μLforHx‐Sed,Hp_Sed,P26,P40,P41,P44,andP50or5pg/μLforP62.Concentration(pg/μL)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐2‐ToxapheneCongenersinAlaskanCodSourceFishLaboratory RepASHLAND 1ASHLAND 2EPA_NEIC 1EPA_NEIC 2EPA_R4_1 1EPA_R4_1 2EPA_R4_1 3EPA_R4_2 1EPA_R4_2 2EPA_R4_3 1EPA_R4_3 2SCCWRP 1SCCWRP 2SCCWRP 3EPA_NERL/ORD_LV_11EPA_NERL/ORD_LV_12EPA_NERL/ORD_LV_21EPA_NERL/ORD_LV_22PCB209(spiked@100)eHCH(spiked@250)PCB209 eHCH PCB209 eHCH PCB209 eHCH71.9 262 71.9 105 71.8 266 0.279 2.8971.7 270 71.7 10885.3 247 85.3 98.7 84.9 252 0.859 4.1084.6 257 84.6 10377.9 240 77.9 96.1 75.2 240 7.04 4.0169.1 250 69.1 10078.6 231 78.6 92.476.1 236 76.1 94.4 77.1 234 2.44 1.8178.0 232 78.0 92.778.9 241 78.9 96.5 78.0 242 2.40 0.27377.0 242 77.0 96.780.1 222 80.1 88.8 82.6 228 2.87 2.6383.0 228 83.0 91.284.8 234 84.8 93.677.7 219 77.7 87.6 78.6 220 2.16 0.45679.4 220 79.4 88.080.7 229 80.7 91.6 80.8 230 0.111 0.68480.8 230 80.8 92.2%RPDorRSDConcentration(pg/μL)%Recovery AvgConc(pg/μL)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐3‐TechnicalToxapheneinTerryCreekFishSamplesLaboratory Fish ReplicateConc(pg/μL) AvgConc(pg/μL) %RPDorRSDASHLAND1 13573560.675ASHLAND1 2354ASHLAND2 13163276.31ASHLAND2 2337EPA_NEIC1 12652631.03EPA_NEIC1 2262EPA_NEIC2 13253260.685EPA_NEIC2 2327EPA_R4_11 13603683.85EPA_R4_11 2360EPA_R4_11 3384EPA_R4_12 12682634.79EPA_R4_12 2249EPA_R4_12 3273EPA_R4_21 13143121.39EPA_R4_21 2309EPA_R4_22 12382455.28EPA_R4_22 2251EPA_R4_31 13413381.70EPA_R4_31 2335EPA_R4_32 12482452.38EPA_R4_32 2242SCCWRP1 14254240.272SCCWRP1 2423SCCWRP1 3425SCCWRP2 13033143.22SCCWRP2 2315SCCWRP2 3323EPA_NERL/ORD_LV_11 12672755.90EPA_NERL/ORD_LV_11 2283EPA_NERL/ORD_LV_12 13243240.185EPA_NERL/ORD_LV_12 2324EPA_NERL/ORD_LV_21 14694752.34EPA_NERL/ORD_LV_21 2480EPA_NERL/ORD_LV_22 14894921.14EPA_NERL/ORD_LV_22 2494ToxapheneMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐3‐TechnicalToxapheneinTerryCreekFishSamplesLaboratory Fish ReplicateASHLAND 1 1ASHLAND 1 2ASHLAND 2 1ASHLAND 2 2EPA_NEIC1 1EPA_NEIC1 2EPA_NEIC2 1EPA_NEIC2 2EPA_R4_11 1EPA_R4_11 2EPA_R4_11 3EPA_R4_12 1EPA_R4_12 2EPA_R4_12 3EPA_R4_21 1EPA_R4_21 2EPA_R4_22 1EPA_R4_22 2EPA_R4_31 1EPA_R4_31 2EPA_R4_32 1EPA_R4_32 2SCCWRP1 1SCCWRP1 2SCCWRP1 3SCCWRP2 1SCCWRP2 2SCCWRP2 3EPA_NERL/ORD_LV_11 1EPA_NERL/ORD_LV_11 2EPA_NERL/ORD_LV_12 1EPA_NERL/ORD_LV_12 2EPA_NERL/ORD_LV_21 1EPA_NERL/ORD_LV_21 2EPA_NERL/ORD_LV_22 1EPA_NERL/ORD_LV_22 2Conc(pg/μL)* %Recovery* AvgConc(pg/μL) %RPDorRSD19.899.019.80.50619.798.593.493.492.81.4092.192.121.110521.10.047521.11051011011044.8810610618.693.019.17.7620.710417.989.586.686.694.77.4199.299.298.398.320.410220.31.1920.110195.995.996.30.74896.696.620.310220.40.98020.51031001001000.70099.799.720.410219.92.0419.798.519.798.41001001021.7010310310410420.310219.94.5319.497.099.799.797.83.8995.995.930.215130.20.099430.21511041041040.674104104*PCB209(Surrogate)spikedinFish1at20pg/μLandinFish2at100pg/μLPCB209Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐3‐TechnicalToxapheneinTerryCreekFishSamplesLaboratory Fish ReplicateASHLAND 1 1ASHLAND 1 2ASHLAND 2 1ASHLAND 2 2EPA_NEIC1 1EPA_NEIC1 2EPA_NEIC2 1EPA_NEIC2 2EPA_R4_11 1EPA_R4_11 2EPA_R4_11 3EPA_R4_12 1EPA_R4_12 2EPA_R4_12 3EPA_R4_21 1EPA_R4_21 2EPA_R4_22 1EPA_R4_22 2EPA_R4_31 1EPA_R4_31 2EPA_R4_32 1EPA_R4_32 2SCCWRP1 1SCCWRP1 2SCCWRP1 3SCCWRP2 1SCCWRP2 2SCCWRP2 3EPA_NERL/ORD_LV_11 1EPA_NERL/ORD_LV_11 2EPA_NERL/ORD_LV_12 1EPA_NERL/ORD_LV_12 2EPA_NERL/ORD_LV_21 1EPA_NERL/ORD_LV_21 2EPA_NERL/ORD_LV_22 1EPA_NERL/ORD_LV_22 2Conc(pg/μL)** %Recovery** AvgConc(pg/μL) %RPDorRSD55.511156.84.5858.11162981193001.2030212153.610753.31.1853.010623493.525013.126610752.310552.21.2451.510352.81062611052523.3224899.224698.448.897.548.41.3648.196.224397.32430.33424296.950.110048.56.4946.993.923694.32382.0224196.344.989.745.21.2344.989.945.991.723393.02341.2623192.523794.844.188.245.77.0047.394.623493.62266.5821987.680.916281.00.16181.116223694.42341.5423292.9**eHCH(Surrogate)spikedinFish1at50pg/μLandinFish2at250pg/μLeHCHMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2

# 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 2TableA2‐4‐ToxapheneCongenersinTerryCreekFishSamplesLaboratory Fish RepHx‐SedHp‐SedP26P40P41P44P50P62ASHLAND11 86.6 96.7 7.10 8.50 4.10 4.60 7.40 9.10ASHLAND12 86.5 98.3 7.80 10.6 4.40 4.20 8.20 8.70ASHLAND21 62.0 85.9 12.2 11.7 5.10 6.80 11.9 7.90ASHLAND22 57.9 77.1 10.3 11.5 5.00 8.30 12.8 7.90EPA_NEIC11 77.6 90.1 7.90 11.7 4.50 5.27 8.63 <3.00EPA_NEIC12 78.1 90.4 8.09 11.7 4.62 5.29 8.37 <3.00EPA_NEIC21 51.7 73.6 12.1 12.8 5.44 6.45 13.5 21.5EPA_NEIC22 51.1 72.1 11.4 12.8 5.22 6.76 13.0 18.4EPA_R4_111 86.6 98.9 8.67 11.9 4.63 5.16 9.22 10.8EPA_R4_112 88.3 99.5 8.42 12.5 4.72 5.40 9.32 10.3EPA_R4_113 88.9 101 8.65 12.1 4.79 4.91 9.43 11.1EPA_R4_121 63.0 88.0 13.0 14.1 5.78 7.21 14.4 13.6EPA_R4_122 62.8 87.8 13.1 14.0 5.78 7.21 14.7 14.5EPA_R4_123 57.9 80.0 12.2 13.1 5.42 6.71 13.7 14.3EPA_R4_211 83.3 92.8 8.00 12.2 4.57 4.46 8.86 8.12EPA_R4_212 82.5 91.3 7.67 12.0 4.48 4.94 8.72 8.81EPA_R4_221 55.2 75.4 11.3 12.7 5.29 6.21 13.3 10.9EPA_R4_222 56.0 76.0 11.7 12.9 5.30 6.42 13.3 12.8EPA_R4_311 81.1 92.9 8.04 11.8 4.51 4.68 8.81 8.08EPA_R4_312 80.5 91.5 8.14 11.8 4.50 4.62 8.64 8.43EPA_R4_321 53.4 74.8 11.0 12.7 5.14 5.95 12.9 14.7EPA_R4_322 53.8 74.2 11.7 12.9 5.13 6.37 13.2 11.5SCCWRP11 78.4 91.5 8.60 10.8 4.50 4.80 8.30 15.9SCCWRP12 81.3 94.1 8.00 10.9 4.50 5.00 8.50 17.4SCCWRP13 81.6 96.9 8.80 12.1 4.90 4.90 9.00 15.8SCCWRP21 51.2 74.1 11.6 12.4 5.30 6.30 12.6 20.3SCCWRP22 52.5 76.4 11.6 11.9 5.10 6.70 12.8 16.8SCCWRP23 53.7 78.4 12.3 12.8 5.70 7.00 13.5 23.2EPA_NERL/ORD_LV_111 72.1 87.1 8.74 10.5 4.63 4.96 6.83 11.7EPA_NERL/ORD_LV_112 73.0 79.6 7.99 8.97 4.57 4.14 7.11 10.3EPA_NERL/ORD_LV_12151.8 72.0 11.1 12.2 5.33 6.55 9.64 16.6EPA_NERL/ORD_LV_122 51.0 71.8 11.4 11.1 5.52 4.90 11.7 12.8EPA_NERL/ORD_LV_211 73.2 83.8 7.07 10.3 4.12 4.51 7.87 6.34EPA_NERL/ORD_LV_212 73.4 86.2 8.26 11.3 4.18 4.35 8.18 12.7EPA_NERL/ORD_LV_221 47.4 67.7 11.7 13.2 5.00 7.01 13.5 13.8EPA_NERL/ORD_LV_222 48.9 65.1 10.8 13.0 5.09 6.47 13.3 20.2concentration(pg/μL)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐4‐ToxapheneCongenersinTerryCreekFishSamplesLaboratory Fish RepASHLAND11ASHLAND12ASHLAND21ASHLAND22EPA_NEIC11EPA_NEIC12EPA_NEIC21EPA_NEIC22EPA_R4_111EPA_R4_112EPA_R4_113EPA_R4_121EPA_R4_122EPA_R4_123EPA_R4_211EPA_R4_212EPA_R4_221EPA_R4_222EPA_R4_311EPA_R4_312EPA_R4_321EPA_R4_322SCCWRP11SCCWRP12SCCWRP13SCCWRP21SCCWRP22SCCWRP23EPA_NERL/ORD_LV_111EPA_NERL/ORD_LV_112EPA_NERL/ORD_LV_121EPA_NERL/ORD_LV_122EPA_NERL/ORD_LV_211EPA_NERL/ORD_LV_212EPA_NERL/ORD_LV_221EPA_NERL/ORD_LV_222Hx‐SedHp‐SedP26P40P41P44P50P620.1161.649.4022.07.069.0910.34.496.8410.816.91.721.9819.97.290.000.5650.3102.380.5132.630.3793.06*1.172.046.290.0784.134.693.2415.91.351.271.622.701.704.751.133.624.705.323.874.193.674.103.843.350.8931.644.211.651.9910.21.598.151.330.8323.481.020.1893.33016.10.7431.501.240.593 0.2221.291.954.240.8400.8596.781.650.1956.822.2223.92.172.854.926.264.982.044.195.482.402.823.423.845.695.273.6415.91.249.008.3815.40.0019.84.3212.71.560.2782.679.443.7029.619.725.90.2732.8515.59.631.453.613.8666.73.053.918.291.611.788.011.4938.0Relative%Difference(RPD)orRelativeStandardDeviation(RSD)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐4‐ToxapheneCongenersinTerryCreekFishSamplesLaboratory Fish RepASHLAND11ASHLAND12ASHLAND21ASHLAND22EPA_NEIC11EPA_NEIC12EPA_NEIC21EPA_NEIC22EPA_R4_111EPA_R4_112EPA_R4_113EPA_R4_121EPA_R4_122EPA_R4_123EPA_R4_211EPA_R4_212EPA_R4_221EPA_R4_222EPA_R4_311EPA_R4_312EPA_R4_321EPA_R4_322SCCWRP11SCCWRP12SCCWRP13SCCWRP21SCCWRP22SCCWRP23EPA_NERL/ORD_LV_111EPA_NERL/ORD_LV_112EPA_NERL/ORD_LV_121EPA_NERL/ORD_LV_122EPA_NERL/ORD_LV_211EPA_NERL/ORD_LV_212EPA_NERL/ORD_LV_221EPA_NERL/ORD_LV_222Hx‐Sed Hp‐SedP26P40P41P44P50P6286.697.57.45 9.55 4.25 4.40 7.80 8.9060.081.511.3 11.6 5.05 7.55 12.4 7.9077.890.28.00 11.7 4.56 5.28 8.50 NA51.472.911.8 12.8 5.33 6.61 13.3 19.987.999.98.58 12.2 4.71 5.16 9.32 10.761.385.312.8 13.7 5.66 7.04 14.3 14.182.992.07.84 12.1 4.53 4.70 8.79 8.4755.675.711.5 12.8 5.30 6.32 13.3 11.880.892.28.09 11.8 4.51 4.65 8.73 8.2653.674.511.4 12.8 5.14 6.16 13.1 13.180.494.18.47 11.3 4.63 4.90 8.60 16.452.576.311.8 12.4 5.37 6.67 13.0 20.172.683.48.35 9.75 4.60 4.55 6.951151.471.911.3 11.7 5.40 5.75 10.7 14.773.385.07.67 10.8 4.15 4.43 8.03 9.5148.166.411.2 13.1 5.05 6.74 13.4 17.0AverageConcentration(pg/μL)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐4‐ToxapheneCongenersinTerryCreekFishSamplesLaboratory Fish RepASHLAND11ASHLAND12ASHLAND21ASHLAND22EPA_NEIC11EPA_NEIC12EPA_NEIC21EPA_NEIC22EPA_R4_111EPA_R4_112EPA_R4_113EPA_R4_121EPA_R4_122EPA_R4_123EPA_R4_211EPA_R4_212EPA_R4_221EPA_R4_222EPA_R4_311EPA_R4_312EPA_R4_321EPA_R4_322SCCWRP11SCCWRP12SCCWRP13SCCWRP21SCCWRP22SCCWRP23EPA_NERL/ORD_LV_111EPA_NERL/ORD_LV_112EPA_NERL/ORD_LV_121EPA_NERL/ORD_LV_122EPA_NERL/ORD_LV_211EPA_NERL/ORD_LV_212EPA_NERL/ORD_LV_221EPA_NERL/ORD_LV_222PCB209(spikedat100)eHCH(spikedat250)PCB209 eHCH PCB209 eHCHPCB209eHCHAvgConc(pg/μL)%RPDorRSD88.127788.1 111 90.0 275 4.221.4991.927391.9 10985.229585.2 118 88.5 274 7.3514.891.725491.7 102105240105 96.0 105 242 0.3431.49105244105 97.4108231108 92.5 108 231 1.430.130107231107 92.496.824696.8 98.5 92.6 255 4.883.3293.226393.2 10587.925687.9 10278.025278.0 101 85.8 245 12.64.8281.225281.2 10198.123198.1 92.596.624596.6 98.0 95.4 245 2.480.30794.324494.3 97.795.923095.9 91.9 95.3 230 1.190.35294.723094.7 92.295.224895.2 99.2 95.3 246 0.2311.4695.424495.4 97.795.022795.0 90.7 95.8 226 1.670.19996.622696.6 90.5100234100 93.6 100 242 0.6413.3299.824199.8 96.4101250101 100103218103 87.2 104 224 1.462.69104223104 89.2106230106 92.099.424699.4 98.4 98.6 235 1.629.3697.822497.8 89.697.923497.9 93.6 98.4 226 1.027.0898.921898.9 87.295.322895.3 91.3 95.5 229 0.2831.0495.623195.6 92.2100214100 85.7 101 218 1.553.19102221102 88.5Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐4‐1‐ToxapheneCongenersinMassUnitsinTerryCreekFishSamplesLaboratory Fish RepHx‐SedHp‐SedP26P40P41P44P50P62concentration(μg/kg)ASHLAND11 173 193 14.2 16.9 8.17 9.2 14.8 18.1ASHLAND12 172 196 15.5 21.1 8.77 8.4 16.3 17.3ASHLAND21 12 17 2.4 2.3 1.02 1.4 2.4 1.6ASHLAND22 12 15 2.1 2.3 1.00 1.66 2.6 1.6EPA_NEIC11 155 180 15.7 23.3 8.97 10.5 17.2 <5.98EPA_NEIC12 156 180 16.1 23.3 9.21 10.5 16.7 <5.98EPA_NEIC21 10 15 2.4 2.6 1.09 1.3 2.7 4.3EPA_NEIC22 10 14 2.3 2.6 1.04 1.35 2.6 3.7EPA_R4_111 173 197 17.3 23.7 9.23 10.3 18.4 21.5EPA_R4_112 176 198 16.8 24.9 9.41 10.8 18.6 20.5EPA_R4_113 177 201 17.2 24.1 9.55 9.79 18.8 22.1EPA_R4_121 12.6 17.6 2.6 2.82 1.16 1.44 2.88 2.72EPA_R4_122 12.6 17.6 2.62 2.8 1.16 1.44 2.94 2.90EPA_R4_123 11.6 16.0 2.44 2.62 1.08 1.34 2.74 2.86EPA_R4_211 166 185 15.9 24.3 9.11 8.89 17.7 16.2EPA_R4_212 164 182 15.3 23.9 8.93 9.85 17.4 17.6EPA_R4_221 11.0 15.1 2.26 2.54 1.06 1.24 2.66 2.18EPA_R4_222 11.2 15.2 2.34 2.58 1.06 1.28 2.66 2.56EPA_R4_311 162 185 16.0 23.5 8.99 9.33 17.6 16.1EPA_R4_312 160 182 16.2 23.5 8.97 9.21 17.2 16.8EPA_R4_321 10.7 15.0 2.2 2.54 1.03 1.19 2.58 2.94EPA_R4_322 10.8 14.8 2.34 2.58 1.03 1.27 2.64 2.30SCCWRP11 156 182 17.1 21.5 8.97 9.57 16.5 31.7SCCWRP12 162 188 15.9 21.7 8.97 9.97 16.9 34.7SCCWRP13 163 193 17.5 24.1 9.77 9.77 17.9 31.5SCCWRP21 10.2 14.8 2.32 2.48 1.06 1.26 2.52 4.06SCCWRP22 10.5 15.3 2.32 2.38 1.02 1.34 2.56 3.36SCCWRP23 10.7 15.7 2.46 2.56 1.14 1.40 2.70 4.64EPA_NERL/ORD_LV_111 144 174 17.4 20.9 9.23 9.89 13.6 23.3EPA_NERL/ORD_LV_112 146 159 15.9 17.9 9.11 8.25 14.2 20.5EPA_NERL/ORD_LV_12110.4 14.4 2.22 2.44 1.07 1.31 1.93 3.32EPA_NERL/ORD_LV_122 10.2 14.4 2.28 2.22 1.10 0.98 2.34 2.56EPA_NERL/ORD_LV_211 146 167 14.1 20.5 8.21 8.99 15.7 12.6EPA_NERL/ORD_LV_212 146 172 16.5 22.5 8.33 8.67 16.3 25.3EPA_NERL/ORD_LV_221 9.48 13.5 2.34 2.64 1.00 1.40 2.70 2.76EPA_NERL/ORD_LV_222 9.78 13.0 2.16 2.6 1.02 1.29 2.66 4.04Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐4‐1‐ToxapheneCongenersinMassUnitsinTerryCreekFishSamplesLaboratory Fish RepASHLAND11ASHLAND12ASHLAND21ASHLAND22EPA_NEIC11EPA_NEIC12EPA_NEIC21EPA_NEIC22EPA_R4_111EPA_R4_112EPA_R4_113EPA_R4_121EPA_R4_122EPA_R4_123EPA_R4_211EPA_R4_212EPA_R4_221EPA_R4_222EPA_R4_311EPA_R4_312EPA_R4_321EPA_R4_322SCCWRP11SCCWRP12SCCWRP13SCCWRP21SCCWRP22SCCWRP23EPA_NERL/ORD_LV_111EPA_NERL/ORD_LV_112EPA_NERL/ORD_LV_121EPA_NERL/ORD_LV_122EPA_NERL/ORD_LV_211EPA_NERL/ORD_LV_212EPA_NERL/ORD_LV_221EPA_NERL/ORD_LV_222Hx‐SedHp‐SedP26P40P41P44P50P62Relative%Difference(RPD)orRelativeStandardDeviation(RSD)0.1161.649.4022.07.069.0910.34.496.8410.816.91.721.9819.97.290.000.6430.002.520.002.640.002.95*1.172.065.960.004.134.693.7715.51.361.081.622.511.704.751.133.774.725.353.864.013.674.103.603.340.9651.634.211.651.9910.21.598.1511.115.12.302.561.061.262.662.370.7431.521.240.000.2221.291.954.240.7460.8056.171.560.1956.822.3024.42.202.874.926.424.982.044.195.482.382.823.423.655.695.273.6415.91.249.008.9715.71.3018.04.012.71.560.2782.679.443.5028.819.325.90.2732.8215.59.261.453.613.8666.83.123.928.001.531.788.011.4937.6Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐5‐TechnicalToxapheneSecondSourceStandardLaboratory ReplicateConc(pg/μL)AvgConc(pg/μL)%Recovery%RPDorRSD Conc(pg/μL)AvgConc(pg/μL) %Recovery%RPDorRSD Conc(pg/μL)AvgConc(pg/μL) %Recovery%RPDorRSDASHLAND1 152 152101109 109109251 251101EPA_NEIC1 156 1651045.29 110 1101100.368 246 26098.54.74EPA_NEIC 2174116110110267107EPA_NEIC 3166111109109268107EPA_R4_11 172 1661154.18 114 1121141.72 263 2651051.35EPA_R4_1 2168112112112264105EPA_R4_1 3159106110110269108EPA_R4_21 166 1661110.881 113 1121130.713 256 2561020.647EPA_R4_2 2165110112112257103EPA_R4_31 160 1651076.11 112 1111121.83 253 2551011.62EPA_R4_3 2170113110110257103SCCWRP1 152 1491012.80 107 1061073.40 255 2531021.14SCCWRP 214496.0102102255102SCCWRP 3150100109109250100EPA_NERL/ORD_LV_11163 14210829.7 105 1061052.64 278 2901118.34EPA_NERL/ORD_LV_1212180.4108108302121EPA_NERL/ORD_LV_21162 1661084.93 110 1091102.64 282 2781132.87EPA_NERL/ORD_LV_2 2170114107107274110TechnicalToxapheneSpikedat150pg/μLPCB209(Surrogate)Spikedat100pg/μLeHCH(Surrogate)Spikedat250pg/μLToxaphenePCB209eHCHMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐6‐TechnicalToxapheneLaboratoryQualityControlSamplesLaboratory Replicate TypeTrueValue(pg/μL) Conc(pg/μL) AvgConc(pg/μL) %Recovery %RPDorRSD Conc(pg/μL) AvgConc(pg/μL) %Recovery %RPDorRSD Conc(pg/μL) AvgConc(pg/μL)%Recovery %RPDorRSDASHLAND 1 MB ND 101 101 101 0.892 270 273 108 2.35ASHLAND 2 MB ND 100 100 276 110ASHLAND 1 LCS1 50.0 56.1 55.7 112 1.62 90.0 91.6 90.0 3.49 267 261 107 4.17ASHLAND 2 LCS1 50.0 55.2 110 93.2 93.2 256 102ASHLAND 1 LCS2 200 237 223 118 12.4 83.7 83.7 83.7 264 264 105 0.341ASHLAND 2 LCS2 20020910583.783.7265106EPA_NEIC 1 MB ND 107 106 107 1.49 254 250 102 3.16EPA_NEIC 2 MB ND 105 105 246 98.4EPA_NEIC 1 LCS1 50.0 70.6 68.2 141 6.93 94.4 96.8 94.4 5.12 282 257 113 19.9EPA_NEIC 2 LCS1 50.0 65.9 132 99.3 99.3 231 92.4EPA_NEIC 1 LCS2 200 203 204 101 0.854 94.6 95.8 94.6 2.68 267 253 107 10.9EPA_NEIC2 LCS2 20020510297.197.124095.8EPA_R4_1 1 MB 3.08 101 102 101 1.02 249 249 99.8 0.0465EPA_R4_1 2 MB 3.36 102 102 249 99.7EPA_R4_1 3 MB 4.66 103 103 249 99.8EPA_R4_1 1 LCS1 50.0 62.0 60.0 124 13.3 93.4 95.5 93.4 3.04 231 231 92.3 0.659EPA_R4_1 2 LCS1 50.0 66.8 134 94.4 94.4 230 92.1EPA_R4_1 3 LCS1 50.0 51.2 102 98.8 98.8 233 93.3EPA_R4_1 1 LCS2 200 229 221 114 5.13 77.1 80.6 77.1 4.70 257 251 103 2.34EPA_R4_1 2 LCS2 200 208 104 79.9 79.9 251 100EPA_R4_1 3LCS2 200 22511384.684.624698.2EPA_R4_2 1 MB 5.29 101 101 101 0.862 246 246 98.5 0.644EPA_R4_2 2 MB 5.06 100 100 245 97.9EPA_R4_2 1 LCS1 50.0 51.4 56.8 103 19.0 92.3 93.4 92.3 2.33 229 226 91.5 2.51EPA_R4_2 2 LCS1 50.0 62.2 124 94.5 94.5 223 89.2EPA_R4_2 1 LCS2 200 204 202 102 1.79 89.3 90.0 89.3 1.47 237 236 94.8 0.950EPA_R4_2 2 LCS2 20020110090.690.623593.9EPA_R4_3 1 MB 1.63 102 102 102 0.353 240 243 96.0 2.25EPA_R4_3 2 MB 1.82 102 102 246 98.2EPA_R4_3 1 LCS1 50.0 42.1 43.1 84.1 4.80 93.9 94.1 93.9 0.298 227 227 90.8 0.0396EPA_R4_3 2 LCS1 50.0 44.1 88.2 94.2 94.2 227 90.8EPA_R4_3 1 LCS2 200 189 181 94.3 8.43 92.5 91.8 92.5 1.51 228 234 91.3 4.91EPA_R4_3 2 LCS2 20017386.691.191.124095.9SCCWRP 1 MB 0.240 107 104 107 2.21 237 234 94.8 1.07SCCWRP 2 MB 0.240 103 103 232 92.8SCCWRP 3 MB 0.130 103 103 234 93.6SCCWRP 1 LCS1 50.0 44.5 44.9 89.0 2.07 98.5 97.3 98.5 2.50 225 224 90.0 1.03SCCWRP 2 LCS1 50.0 46.0 92.0 98.9 98.9 221 88.4SCCWRP 3 LCS1 50.0 44.3 88.6 94.5 94.5 225 90.0SCCWRP 1 LCS2 200 226 217 113 3.72 95.3 93.2 95.3 2.02 228 226 91.2 2.09SCCWRP 2 LCS2 200 210 105 91.6 91.6 221 88.4SCCWRP 3LCS2 200 21610892.892.823092.0EPA_NERL/ORD_LV_11 MB ND 105 103 105 3.78 241 237 96.5 3.97EPA_NERL/ORD_LV_12 MB ND 101 101 232 92.7EPA_NERL/ORD_LV_11 LCS1 50.0 47.6 58.9 95.2 38.2 95.7 95.2 95.7 1.16 191 194 76.3 3.20EPA_NERL/ORD_LV_12 LCS1 50.0 70.1 94.6 94.6 197 78.8EPA_NERL/ORD_LV_11 LCS2 200 207 204 103 2.15 92.1 91.6 92.1 1.20 229 217 91.4 10.3EPA_NERL/ORD_LV_12LCS2200202 91.091.020682.5EPA_NERL/ORD_LV_21 MB 19.4 107 107 107 0.871 251 249 100 1.61EPA_NERL/ORD_LV_22 MB 16.1 106 106 247 98.7EPA_NERL/ORD_LV_2 1 LCS1 50.0 66.4 70.6 133 11.9 96.6 96.5 96.6 0.270 224 224 89.7 0.187EPA_NERL/ORD_LV_22 LCS1 50.0 74.8 150 96.3 96.3 225 89.8EPA_NERL/ORD_LV_2 1 LCS2 200 205 207 103 1.64 95.1 94.9 95.1 0.464 234 234 93.5 0.312EPA_NERL/ORD_LV_22LCS220020910494.794.723593.8PCB209(Surrogate) eHCH(Surrogate)eHCH(Surrogate)SpikedinMBLCS1,andLCS2at250pg/μLToxaphenehighlightedcellshaveconcentrationsbelowtheLLOQof50pg/μLPCB209(Surrogate)SpikedinMB,LCS1,andLCS2at100pg/μLMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐7‐ToxapheneCongenersSpikedinLaboratoryQualityControlSamplesLaboratory Type Replicate Hx‐SedHp‐Sed P26P40 P41 P44 P50P62ASHLAND 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 26.3EPA_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 21.0EPA_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 23.6SCCWRP 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 22.6EPA_NERL/ORD_LV_1MB 1 0.32 0.27 0.84 0.6 0.66 0.95 0.66 1.55EPA_NERL/ORD_LV_1MB 2 0.34 0.26 0.82 0.58 0.66 0.87 0.68 1.34EPA_NERL/ORD_LV_1LCS1 1 92.4 91.6 85.0 87.1 85.4 78.2 80.7 182EPA_NERL/ORD_LV_1LCS1 2 91.3 93.2 91.2 86.3 86.0 81.1 82.9 189EPA_NERL/ORD_LV_1LCS2 1 1.55 1.48 0.95 2.07 2.34 1.15 2.09 11.9EPA_NERL/ORD_LV_1LCS2 2 2.11 2.31 1.82 1.29 2.44 2.17 1.86 12.1EPA_NERL/ORD_LV_2MB 1 ND ND ND ND 0.18 ND ND NDEPA_NERL/ORD_LV_2MB 2 ND ND ND ND ND ND ND NDEPA_NERL/ORD_LV_2LCS1 1 92.5 92.7 96 91.9 95.1 95.9 90.4 223EPA_NERL/ORD_LV_2LCS1 2 88.0 89.8 90.5 89.6 91.9 96.4 90.6 231EPA_NERL/ORD_LV_2LCS2 1 1.74 1.85 1.24 2.00 1.95 2.25 2.15 15.6EPA_NERL/ORD_LV_2LCS2 2 1.73 1.82 1.20 1.96 1.80 1.74 2.02 19.4Concentration(pg/μL)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐7‐ToxapheneCongenersSpikedinLaboratoryQualityControlSamplesLaboratory Type ReplicateASHLAND MB 1ASHLAND MB 2ASHLAND LCS1 1ASHLAND LCS1 2ASHLAND LCS2 1ASHLAND LCS2 2EPA_NEIC MB 1EPA_NEIC MB 2EPA_NEIC LCS1 1EPA_NEIC LCS1 2EPA_NEIC LCS2 1EPA_NEIC LCS2 2EPA_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 2SCCWRP MB 1SCCWRP MB 2SCCWRP MB 3SCCWRP LCS1 1SCCWRP LCS1 2SCCWRP LCS1 3SCCWRP LCS2 1SCCWRP LCS2 2SCCWRP LCS2 3EPA_NERL/ORD_LV_1MB 1EPA_NERL/ORD_LV_1MB 2EPA_NERL/ORD_LV_1LCS1 1EPA_NERL/ORD_LV_1LCS1 2EPA_NERL/ORD_LV_1LCS2 1EPA_NERL/ORD_LV_1LCS2 2EPA_NERL/ORD_LV_2MB 1EPA_NERL/ORD_LV_2MB 2EPA_NERL/ORD_LV_2LCS1 1EPA_NERL/ORD_LV_2LCS1 2EPA_NERL/ORD_LV_2LCS2 1EPA_NERL/ORD_LV_2LCS2 2Hx‐SedHp‐Sed P26P40 P41 P44 P50P62100 100 100 100 100 100 100 226100 100 100 100 100 100 100 2262.00 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 22.6100 100 100 100 100 100 100 226100 100 100 100 100 100 100 2262.00 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 22.6100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226100 100 100 100 100 100 100 2262.00 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 22.6100 100 100 100 100 100 100 226100 100 100 100 100 100 100 2262.00 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 22.6100 100 100 100 100 100 100 226100 100 100 100 100 100 100 2262.00 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 22.6100 100 100 100 100 100 100 226100 100 100 100 100 100 100 226100 100 100 100 100 100 100 2262.00 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 22.6100 100 100 100 100 100 100 226100 100 100 100 100 100 100 2262.00 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 22.6100 100 100 100 100 100 100 226100 100 100 100 100 100 100 2262.00 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 22.6TrueValue(pg/μL)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐7‐ToxapheneCongenersSpikedinLaboratoryQualityControlSamplesLaboratory Type ReplicateASHLAND MB 1ASHLAND MB 2ASHLAND LCS1 1ASHLAND LCS1 2ASHLAND LCS2 1ASHLAND LCS2 2EPA_NEIC MB 1EPA_NEIC MB 2EPA_NEIC LCS1 1EPA_NEIC LCS1 2EPA_NEIC LCS2 1EPA_NEIC LCS2 2EPA_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 2SCCWRP MB 1SCCWRP MB 2SCCWRP MB 3SCCWRP LCS1 1SCCWRP LCS1 2SCCWRP LCS1 3SCCWRP LCS2 1SCCWRP LCS2 2SCCWRP LCS2 3EPA_NERL/ORD_LV_1MB 1EPA_NERL/ORD_LV_1MB 2EPA_NERL/ORD_LV_1LCS1 1EPA_NERL/ORD_LV_1LCS1 2EPA_NERL/ORD_LV_1LCS2 1EPA_NERL/ORD_LV_1LCS2 2EPA_NERL/ORD_LV_2MB 1EPA_NERL/ORD_LV_2MB 2EPA_NERL/ORD_LV_2LCS1 1EPA_NERL/ORD_LV_2LCS1 2EPA_NERL/ORD_LV_2LCS2 1EPA_NERL/ORD_LV_2LCS2 2Hx‐SedHp‐Sed P26P40 P41 P44 P50P62107 107 100 104 102 100 97.4 2352.05 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 22.0105 106 105 105 106 110 105 2772.22 2.13 2.16 2.05 2.12 2.16 2.11 25.6101 99.0 97.6 101 101 103 101 2532.02 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 17.5AverageConc(pg/μL)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐7‐ToxapheneCongenersSpikedinLaboratoryQualityControlSamplesLaboratory Type ReplicateASHLAND MB 1ASHLAND MB 2ASHLAND LCS1 1ASHLAND LCS1 2ASHLAND LCS2 1ASHLAND LCS2 2EPA_NEIC MB 1EPA_NEIC MB 2EPA_NEIC LCS1 1EPA_NEIC LCS1 2EPA_NEIC LCS2 1EPA_NEIC LCS2 2EPA_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 2SCCWRP MB 1SCCWRP MB 2SCCWRP MB 3SCCWRP LCS1 1SCCWRP LCS1 2SCCWRP LCS1 3SCCWRP LCS2 1SCCWRP LCS2 2SCCWRP LCS2 3EPA_NERL/ORD_LV_1MB 1EPA_NERL/ORD_LV_1MB 2EPA_NERL/ORD_LV_1LCS1 1EPA_NERL/ORD_LV_1LCS1 2EPA_NERL/ORD_LV_1LCS2 1EPA_NERL/ORD_LV_1LCS2 2EPA_NERL/ORD_LV_2MB 1EPA_NERL/ORD_LV_2MB 2EPA_NERL/ORD_LV_2LCS1 1EPA_NERL/ORD_LV_2LCS1 2EPA_NERL/ORD_LV_2LCS2 1EPA_NERL/ORD_LV_2LCS2 2Hx‐SedHp‐Sed P26P40 P41 P44 P50P62108% 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%%RecoveryMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐7‐ToxapheneCongenersSpikedinLaboratoryQualityControlSamplesLaboratory Type ReplicateASHLAND MB 1ASHLAND MB 2ASHLAND LCS1 1ASHLAND LCS1 2ASHLAND LCS2 1ASHLAND LCS2 2EPA_NEIC MB 1EPA_NEIC MB 2EPA_NEIC LCS1 1EPA_NEIC LCS1 2EPA_NEIC LCS2 1EPA_NEIC LCS2 2EPA_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 2SCCWRP MB 1SCCWRP MB 2SCCWRP MB 3SCCWRP LCS1 1SCCWRP LCS1 2SCCWRP LCS1 3SCCWRP LCS2 1SCCWRP LCS2 2SCCWRP LCS2 3EPA_NERL/ORD_LV_1MB 1EPA_NERL/ORD_LV_1MB 2EPA_NERL/ORD_LV_1LCS1 1EPA_NERL/ORD_LV_1LCS1 2EPA_NERL/ORD_LV_1LCS2 1EPA_NERL/ORD_LV_1LCS2 2EPA_NERL/ORD_LV_2MB 1EPA_NERL/ORD_LV_2MB 2EPA_NERL/ORD_LV_2LCS1 1EPA_NERL/ORD_LV_2LCS1 2EPA_NERL/ORD_LV_2LCS2 1EPA_NERL/ORD_LV_2LCS2 2Hx‐SedHp‐Sed P26P40 P41 P44 P50P621.96 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 2.350.103 0.507 1.59 0.164 1.79 0.995 1.94 2.454.49 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 1.674.93 3.18 5.86 2.50 3.50 0.572 0.188 3.150.576 1.63 3.28 2.02 8.00 25.6 6.24 22.0Relative%Difference(RPD)orRelativeStandardDeviation(RSD)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐7‐ToxapheneCongenersSpikedinLaboratoryQualityControlSamplesLaboratory Type ReplicateASHLAND MB 1ASHLAND MB 2ASHLAND LCS1 1ASHLAND LCS1 2ASHLAND LCS2 1ASHLAND LCS2 2EPA_NEIC MB 1EPA_NEIC MB 2EPA_NEIC LCS1 1EPA_NEIC LCS1 2EPA_NEIC LCS2 1EPA_NEIC LCS2 2EPA_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 2SCCWRP MB 1SCCWRP MB 2SCCWRP MB 3SCCWRP LCS1 1SCCWRP LCS1 2SCCWRP LCS1 3SCCWRP LCS2 1SCCWRP LCS2 2SCCWRP LCS2 3EPA_NERL/ORD_LV_1MB 1EPA_NERL/ORD_LV_1MB 2EPA_NERL/ORD_LV_1LCS1 1EPA_NERL/ORD_LV_1LCS1 2EPA_NERL/ORD_LV_1LCS2 1EPA_NERL/ORD_LV_1LCS2 2EPA_NERL/ORD_LV_2MB 1EPA_NERL/ORD_LV_2MB 2EPA_NERL/ORD_LV_2LCS1 1EPA_NERL/ORD_LV_2LCS1 2EPA_NERL/ORD_LV_2LCS2 1EPA_NERL/ORD_LV_2LCS2 2PCB209(spikedat100)eHCH(spikedat250)PCB209 eHCH PCB209 eHCH PCB209 eHCH94.4 25994.4% 104% 94.0 256.0 1.0 2.393.5 25393.5% 101%87.2 28187.2% 112% 87.9 274.5 1.6 4.788.6 26888.6% 107%88.0 26188.0% 104% 88.6 262.5 1.4 1.189.2 26489.2% 106%107 266107% 107% 105 256.5 3.8 7.4103 247103% 98.7%99.2 25999.2% 104% 101 252.5 3.8 5.1103 246103% 98.3%103 250103% 100% 103 246.0 1.0 3.3104 242104% 97.0%96.7 25796.7% 103% 97.7 256.3 1.0 0.298.0 25698.0% 103%98.6 25698.6% 103%82.2 25082.2% 100% 87.6 245.7 7.2 3.186.1 25086.1% 100%94.6 23794.6% 94.8%81.6 26381.6% 105% 85.8 255.7 8.3 3.481.7 25881.7% 103%94.0 24694.0% 98.5%99.7 252100% 101% 99.3 251.0 0.8 0.898.9 25098.9% 100%94.7 24194.7% 96.5% 93.0 245.5 3.5 3.791.4 25091.4% 100%95.7 24595.7% 98.1% 94.6 246.0 2.4 0.893.4 24793.4% 98.6%100 245100% 98.0% 101 247.5 1.0 2.0101 250101% 100%96.7 23696.7% 94.4% 97.4 236.5 1.5 0.498.2 23798.2% 95.0%94.1 24594.1% 97.9% 95.3 243.5 2.5 1.296.5 24296.5% 96.7%101 250101% 100% 102 249.3 0.6 1.6102 245102% 98.0%102 253102% 101%94.3 23794.3% 94.8% 96.8 239.7 2.6 1.396.8 23996.8% 95.6%99.3 24399.3% 97.2%98.6 23398.6% 93.2% 98.6 238.7 2.4 2.396.3 23996.3% 95.6%101 244101% 97.6%100 224 100% 89.6%102 230.5 3.0 5.6103 237 103% 94.8%98.4 245 98.4% 98.0%100 249.5 3.6 3.6102 254 102% 102%97.2 237 97.2% 94.8%97.4 248.0 0.3 8.997.5 259 97.5% 104%98.8 23998.8% 95.7% 98.2 242.0 1.2 2.597.6 24597.6% 97.9%99.3 22999.3% 91.8% 97.1 227.5 4.4 1.395.0 22695.0% 90.3%96.5 22996.5% 91.5% 95.2 228.0 2.7 0.993.9 22793.9% 90.9%Conc(pg/μL)%RecoveryAvgConc(pg/μL)%RPDorRSDMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐8‐QualityControlSamples:MatrixSpike/MatrixSpikeDuplicates‐TechnicalToxapheneParent(pg/μL) ParentAvg(pg/μL) Conc(pg/μL)CorrectedConc(pg/μL)%Recovery AvgConc(pg/μL)RelativePercentDifference(%) AvgRPD(%)ASHLANDMS 111.2 10.4168 15879.0%ASHLANDMS 29.50197 18793.5%173ASHLANDMSD 111.2 10.4197 18693.2%16.6ASHLANDMSD 29.50174 16481.9%175 13.214.9EPA_NEICMS 146.3 42.3180 13869.1%EPA_NEICMS 238.2193 15075.2%144EPA_NEICMSD 146.3 42.3191 14974.4%7.31EPA_NEICMSD 238.2189 14773.4%148 2.394.85EPA_R4_1MS 121.8 17.6208 19195.4%EPA_R4_1MS 214.3232 214107%EPA_R4_1MS 316.8212 19497.1%200EPA_R4_1MSD 121.8 17.6221 203102%6.24EPA_R4_1MSD 214.3212 19497.0%9.86EPA_R4_1MSD 316.8215 19798.7%198 1.625.91EPA_R4_2MS 112.1 13.4197 18391.7%EPA_R4_2MS 214.6204 19195.3%187EPA_R4_2MSD 112.1 13.4192 17989.4%2.53EPA_R4_2MSD 214.6194 18190.4%180 5.263.89EPA_R4_3MS 19.18 8.91203 19597.3%EPA_R4_3MS 28.63208 19999.6%197EPA_R4_3MSD 19.18 8.91204 19597.3%0.0668EPA_R4_3MSD 28.63199 19095.2%193 4.592.33SCCWRPMS 14.70 3.97209 205103%SCCWRPMS 23.70213 209105%SCCWRPMS 33.50220 216108%210SCCWRPMSD 14.70 3.97201 19798.5%3.98SCCWRPMSD 23.70199 19597.5%6.93SCCWRPMSD 33.50207 203102%198 6.205.70EPA_NERL/ORD_LV_1MS 18.74212 203101%EPA_NERL/ORD_LV_1MS 217.5223 214107%208EPA_NERL/ORD_LV_1MSD 18.74214 205103%1.18EPA_NERL/ORD_LV_1MSD 217.5218 209105%207 2.321.75EPA_NERL/ORD_LV_2MS 135.2 32.8203 17185.3%EPA_NERL/ORD_LV_2MS 230.4194 16180.7%166EPA_NERL/ORD_LV_2MSD 135.2 32.8189 15678.1%8.88EPA_NERL/ORD_LV_2MSD 230.4188 15677.8%156 3.726.30ToxapheneLaboratory Type ReplicateTechnicalToxapheneSpikedat200pg/μLMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐8‐QualityControlSamples:MatrixSpike/MatrixSpikeDuplicates‐TechnicalToxapheneASHLANDMS 1ASHLANDMS 2ASHLANDMSD 1ASHLANDMSD 2EPA_NEICMS 1EPA_NEICMS 2EPA_NEICMSD 1EPA_NEICMSD 2EPA_R4_1MS 1EPA_R4_1MS 2EPA_R4_1MS 3EPA_R4_1MSD 1EPA_R4_1MSD 2EPA_R4_1MSD 3EPA_R4_2MS 1EPA_R4_2MS 2EPA_R4_2MSD 1EPA_R4_2MSD 2EPA_R4_3MS 1EPA_R4_3MS 2EPA_R4_3MSD 1EPA_R4_3MSD 2SCCWRPMS 1SCCWRPMS 2SCCWRPMS 3SCCWRPMSD 1SCCWRPMSD 2SCCWRPMSD 3EPA_NERL/ORD_LV_1MS 1EPA_NERL/ORD_LV_1MS 2EPA_NERL/ORD_LV_1MSD 1EPA_NERL/ORD_LV_1MSD 2EPA_NERL/ORD_LV_2MS 1EPA_NERL/ORD_LV_2MS 2EPA_NERL/ORD_LV_2MSD 1EPA_NERL/ORD_LV_2MSD 2Laboratory Type ReplicateConc(pg/μL) %RecoveryRelativePercentDifference(%)AvgRPD(%)62.962.9%62.662.6%62.462.4% 0.79859.459.4% 5.25 3.0270.970.9%74.374.3%68.868.8% 2.9970.170.1% 5.83 4.4168.668.6%68.068.0%69.569.5%67.767.7% 1.3468.368.3% 0.39667.167.1% 3.51 1.7570.170.1%67.067.0%65.965.9% 6.2665.865.8% 1.76 4.0166.666.6%68.868.8%64.264.2% 3.7063.463.4% 8.23 5.9674.574.5%70.570.5%71.171.1%66.766.7% 11.067.467.4% 4.5069.369.3% 2.56 6.0467.267.2%68.568.5%65.865.8% 2.1165.465.4% 4.63 3.3775.675.6%76.876.8%74.074.0% 2.0373.373.3% 4.60 3.31PCB209(Surrogate)Spikedat100pg/μLPCB209Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐8‐QualityControlSamples:MatrixSpike/MatrixSpikeDuplicates‐TechnicalToxapheneASHLANDMS 1ASHLANDMS 2ASHLANDMSD 1ASHLANDMSD 2EPA_NEICMS 1EPA_NEICMS 2EPA_NEICMSD 1EPA_NEICMSD 2EPA_R4_1MS 1EPA_R4_1MS 2EPA_R4_1MS 3EPA_R4_1MSD 1EPA_R4_1MSD 2EPA_R4_1MSD 3EPA_R4_2MS 1EPA_R4_2MS 2EPA_R4_2MSD 1EPA_R4_2MSD 2EPA_R4_3MS 1EPA_R4_3MS 2EPA_R4_3MSD 1EPA_R4_3MSD 2SCCWRPMS 1SCCWRPMS 2SCCWRPMS 3SCCWRPMSD 1SCCWRPMSD 2SCCWRPMSD 3EPA_NERL/ORD_LV_1MS 1EPA_NERL/ORD_LV_1MS 2EPA_NERL/ORD_LV_1MSD 1EPA_NERL/ORD_LV_1MSD 2EPA_NERL/ORD_LV_2MS 1EPA_NERL/ORD_LV_2MS 2EPA_NERL/ORD_LV_2MSD 1EPA_NERL/ORD_LV_2MSD 2Laboratory Type ReplicateConc(pg/μL) %RecoveryRelativePercentDifference(%)AvgRPD(%)22790.6%23393.0%22088.2% 2.7323393.0% 1.3619979.7%21686.5%21083.9% 5.1121083.8% 3.13 4.1220180.6%20983.4%19678.6%19979.6% 1.2420180.6% 3.4620280.6% 2.57 2.4218975.5%20280.6%19578.2% 3.4119477.6% 3.80 3.6120280.8%19879.4%19979.7% 1.4520581.8% 3.08 2.2719377.2%19176.4%19377.2%18975.6% 2.0918975.6% 1.0519176.4% 1.04 1.4018975.4%19377.0%18674.2% 1.5519075.8% 1.57 1.5620180.5%20381.4%20180.5% 0.049720582.0% 0.7840.417eHCH(Surrogate)Spikedat250pg/μLeHCHMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐9‐QualityControlSamlpesMatrixSpike/MatrixSpikeDuplicate‐CongenersHx‐Sed Hp‐Sed P26P40 P41 P44 P50P62Laboratory Type ReplicateASHLANDMS 1 101 99.1 89.8 95.2 93.3 95.3 90.2 213ASHLANDMS 2 102 100 91.6 94.7 93.4 92.6 87.6 208ASHLANDMSD 1 102 99.5 87.4 92.0 90.8 89.0 82.7 192ASHLANDMSD 2 97.4 95.8 84.4 91.1 88.8 88 81.4 189EPA_NEICMS 1 88.1 88.8 89.7 92.1 92.1 96.1 91.9 223EPA_NEICMS 2 88.5 89.4 90.7 91.6 91.6 96.4 91.7 213EPA_NEICMSD 1 86.6 86.5 85.6 88.9 89.3 92.5 87.2 210EPA_NEICMSD 2 86.1 86.0 86.6 88.8 88.9 93.2 86.6 206EPA_R4_1MS 1 98.7 96.9 91.6 96.5 96.1 102 94.7 263EPA_R4_1MS 2 103 102 95.6 100 100 106 96.3 259EPA_R4_1MS 3 105 103 98.1 101 101 107 98.4 259EPA_R4_1MSD 1 97.4 94.9 86.4 94.0 92.8 97.0 89.5 246EPA_R4_1MSD 2 95.8 93.6 85.8 92.0 92.4 96.7 88.1 245EPA_R4_1MSD 3 98.4 97.1 88.4 94.7 93.8 99.1 90.0 245EPA_R4_2MS 1 94.9 91.1 85.3 92.5 91.4 93.7 89.2 225EPA_R4_2MS 2 94.1 90.2 85.1 92.6 91.2 94.3 90.0 233EPA_R4_2MSD 1 90.7 87.1 79.2 88.7 87.9 89.8 84.7 218EPA_R4_2MSD 2 90.6 86.5 80.6 88.7 86.8 89.3 85.1 221EPA_R4_3MS 1 91.3 89.6 85.9 90.9 90.7 92.6 88.7 227EPA_R4_3MS 2 90.8 90.7 88.1 90.6 90.8 93.9 88.5 232EPA_R4_3MSD 1 90.6 90.0 85.1 88.0 88.4 90.0 85.4 216EPA_R4_3MSD 2 87.7 87.0 82.9 87.7 87.0 89.2 82.9 216SCCWRPMS 1 87.4 89.8 85.1 92.2 93.5 98.5 91.4 235SCCWRPMS 2 92.5 92.8 88.9 91.1 93.9 97.3 92.5 232SCCWRPMS 3 92.8 93.8 93.7 97.9 101 106 99.3 263SCCWRPMSD 1 87.4 87.3 81.6 88.2 88.1 90.6 86.1 213SCCWRPMSD 2 88.1 89.0 86.0 91.3 92.4 97.2 90.6 238SCCWRPMSD 3 89.9 90.7 86.2 93.9 96.4 103 93.5 246EPA_NERL/ORD_LV_1MS 1 84.5 86.9 74.2 76.6 77.2 76.9 74.9 166EPA_NERL/ORD_LV_1MS 2 84.3 84.0 83.2 79.7 76.3 77.5 77.5 155EPA_NERL/ORD_LV_1MSD 1 81.1 84.5 71.5 77.7 74.6 71.9 70.6 170EPA_NERL/ORD_LV_1MSD 2 82.5 87.0 77.0 78.8 73.5 78.6 71.9 163EPA_NERL/ORD_LV_2MS 1 87.6 86.1 92.1 92.4 93.3 104 95.2 255EPA_NERL/ORD_LV_2MS 2 89.5 88.2 91.1 94.6 96.9 107 99.5 281EPA_NERL/ORD_LV_2MSD 1 86.3 84.7 85.0 90.8 91.9 98.5 93.7 255EPA_NERL/ORD_LV_2MSD 2 84.6 83.5 84.5 90.9 90.1 100 91.0 257Hx‐Sed,Hp‐Sed,P26,P40,P41,P44,P50Spikedat100pg/μL,P62Spikedat226pg/μLConcentration(pg/μL)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐9‐QualityControlSamlpesMatrixSpike/MatrixSpikeDuplicate‐CongenersLaboratory Type ReplicateASHLANDMS 1ASHLANDMS 2ASHLANDMSD 1ASHLANDMSD 2EPA_NEICMS 1EPA_NEICMS 2EPA_NEICMSD 1EPA_NEICMSD 2EPA_R4_1MS 1EPA_R4_1MS 2EPA_R4_1MS 3EPA_R4_1MSD 1EPA_R4_1MSD 2EPA_R4_1MSD 3EPA_R4_2MS 1EPA_R4_2MS 2EPA_R4_2MSD 1EPA_R4_2MSD 2EPA_R4_3MS 1EPA_R4_3MS 2EPA_R4_3MSD 1EPA_R4_3MSD 2SCCWRPMS 1SCCWRPMS 2SCCWRPMS 3SCCWRPMSD 1SCCWRPMSD 2SCCWRPMSD 3EPA_NERL/ORD_LV_1MS 1EPA_NERL/ORD_LV_1MS 2EPA_NERL/ORD_LV_1MSD 1EPA_NERL/ORD_LV_1MSD 2EPA_NERL/ORD_LV_2MS 1EPA_NERL/ORD_LV_2MS 2EPA_NERL/ORD_LV_2MSD 1EPA_NERL/ORD_LV_2MSD 2Hx‐Sed Hp‐Sed P26P40 P41 P44 P50P6210199.1 89.8 95.2 93.3 95.3 90.2 94.2102100 91.6 94.7 93.4 92.6 87.6 91.910299.5 87.4 92.0 90.8 89.0 82.7 84.997.495.8 84.4 91.1 88.8 88.0 81.4 83.888.188.8 89.7 92.1 92.1 96.1 91.9 98.588.589.4 90.7 91.6 91.6 96.4 91.7 94.386.686.5 85.6 88.9 89.3 92.5 87.2 93.186.186.0 86.6 88.8 88.9 93.2 86.6 91.198.796.9 91.6 96.5 96.1 102 94.7 117103102 95.6 100 100 106 96.3 114105103 98.1 101 101 107 98.4 11597.494.9 86.4 94.0 92.8 97.0 89.5 10995.893.6 85.8 92.0 92.4 96.7 88.1 10998.497.1 88.4 94.7 93.8 99.1 90.0 10894.991.1 85.3 92.5 91.4 93.7 89.2 99.494.190.2 85.1 92.6 91.2 94.3 90.0 10390.787.1 79.2 88.7 87.9 89.8 84.7 96.490.686.5 80.6 88.7 86.8 89.3 85.1 97.991.389.6 85.9 90.9 90.7 92.6 88.7 10090.890.7 88.1 90.6 90.8 93.9 88.5 10390.690.0 85.1 88.0 88.4 90.0 85.4 95.487.787 82.9 87.7 87 89.2 82.9 95.587.489.8 85.1 92.2 93.5 98.5 91.4 10492.592.8 88.9 91.1 93.9 97.3 92.5 10392.893.8 93.7 97.9 101 106 99.3 11687.487.3 81.6 88.2 88.1 90.6 86.1 94.288.189.0 86.0 91.3 92.4 97.2 90.6 10589.990.7 86.2 93.9 96.4 103 93.5 10984.586.9 74.2 76.6 77.2 76.9 74.9 73.584.384.0 83.2 79.7 76.3 77.5 77.5 68.681.184.5 71.5 77.7 74.6 71.9 70.6 75.282.587.0 77.0 78.8 73.5 78.6 71.9 72.187.686.1 92.1 92.4 93.3 104 95.2 11389.588.2 91.1 94.6 96.9 107 99.5 12486.384.7 85.0 90.8 91.9 98.5 93.7 11384.683.5 84.5 90.9 90.1 100 91.0 114%RecoveryMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐9‐QualityControlSamlpesMatrixSpike/MatrixSpikeDuplicate‐CongenersLaboratory Type ReplicateASHLANDMS 1ASHLANDMS 2ASHLANDMSD 1ASHLANDMSD 2EPA_NEICMS 1EPA_NEICMS 2EPA_NEICMSD 1EPA_NEICMSD 2EPA_R4_1MS 1EPA_R4_1MS 2EPA_R4_1MS 3EPA_R4_1MSD 1EPA_R4_1MSD 2EPA_R4_1MSD 3EPA_R4_2MS 1EPA_R4_2MS 2EPA_R4_2MSD 1EPA_R4_2MSD 2EPA_R4_3MS 1EPA_R4_3MS 2EPA_R4_3MSD 1EPA_R4_3MSD 2SCCWRPMS 1SCCWRPMS 2SCCWRPMS 3SCCWRPMSD 1SCCWRPMSD 2SCCWRPMSD 3EPA_NERL/ORD_LV_1MS 1EPA_NERL/ORD_LV_1MS 2EPA_NERL/ORD_LV_1MSD 1EPA_NERL/ORD_LV_1MSD 2EPA_NERL/ORD_LV_2MS 1EPA_NERL/ORD_LV_2MS 2EPA_NERL/ORD_LV_2MSD 1EPA_NERL/ORD_LV_2MSD 2Hx‐Sed Hp‐Sed P26P40 P41 P44 P50P62101 99.8 90.7 95.0 93.4 94.0 88.9 21099.5 97.7 85.9 91.6 89.8 88.5 82.1 19188.3 89.1 90.2 91.8 91.9 96.3 91.8 21886.3 86.3 86.1 88.8 89.1 92.9 86.9 208102 101 95.1 99.3 99 105 96.5 26097.2 95.2 86.8 93.5 93.0 97.6 89.2 24694.5 90.7 85.2 92.6 91.3 94.0 89.6 22990.6 86.8 79.9 88.7 87.4 89.6 84.9 22091.1 90.2 87.0 90.7 90.7 93.2 88.6 22989.1 88.5 84.0 87.8 87.7 89.6 84.2 21690.9 92.1 89.2 93.7 96.1 101 94.4 24388.5 89 84.6 91.1 92.3 96.9 90.1 23284.4 85.5 78.7 78.2 76.8 77.2 76.2 16181.8 85.8 74.3 78.3 74.1 75.3 71.3 16788.6 87.1 91.6 93.5 95.1 105 97.4 26885.5 84.1 84.7 90.9 91.0 99.2 92.3 256AverageConcentration(pg/μL)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐9‐QualityControlSamlpesMatrixSpike/MatrixSpikeDuplicate‐CongenersLaboratory Type ReplicateASHLANDMS 1ASHLANDMS 2ASHLANDMSD 1ASHLANDMSD 2EPA_NEICMS 1EPA_NEICMS 2EPA_NEICMSD 1EPA_NEICMSD 2EPA_R4_1MS 1EPA_R4_1MS 2EPA_R4_1MS 3EPA_R4_1MSD 1EPA_R4_1MSD 2EPA_R4_1MSD 3EPA_R4_2MS 1EPA_R4_2MS 2EPA_R4_2MSD 1EPA_R4_2MSD 2EPA_R4_3MS 1EPA_R4_3MS 2EPA_R4_3MSD 1EPA_R4_3MSD 2SCCWRPMS 1SCCWRPMS 2SCCWRPMS 3SCCWRPMSD 1SCCWRPMSD 2SCCWRPMSD 3EPA_NERL/ORD_LV_1MS 1EPA_NERL/ORD_LV_1MS 2EPA_NERL/ORD_LV_1MSD 1EPA_NERL/ORD_LV_1MSD 2EPA_NERL/ORD_LV_2MS 1EPA_NERL/ORD_LV_2MS 2EPA_NERL/ORD_LV_2MSD 1EPA_NERL/ORD_LV_2MSD 2Hx‐Sed Hp‐Sed P26P40 P41 P44 P50P620.891 0.403 2.71 3.42 2.72 6.84 8.68 10.44.32 4.69 8.18 3.88 5.05 5.09 7.34 9.221.77 2.66 4.60 3.64 3.11 3.74 5.17 5.712.81 3.80 4.64 3.08 3.06 3.45 5.75 3.381.38 2.09 5.81 2.68 3.42 5.34 5.60 6.657.41 8.49 10.9 8.78 8.13 9.48 8.87 5.276.35 6.27 10.4 6.55 6.96 7.23 8.92 5.734.52 4.55 7.47 4.20 3.91 4.25 5.13 3.013.87 4.21 5.52 4.32 4.84 5.49 5.62 4.910.847 0.390 0.935 3.28 2.49 2.86 3.72 5.083.51 4.14 6.12 3.19 4.25 5.10 6.51 7.110.00 2.82 4.20 4.43 5.95 8.36 5.97 9.824.87 4.18 3.32 0.219 1.61 0.103 2.08 2.553.17 3.36 8.34 4.17 4.66 2.87 6.02 6.684.11 2.80 3.71 1.43 3.43 6.72 5.91 2.382.16 3.51 7.74 1.14 3.74 1.41 7.50 5.031.53 1.60 7.95 1.79 1.54 5.26 1.65 0.1535.63 5.37 7.60 3.96 7.28 6.71 8.96 9.01RelativePercentDifference(%RPD)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐9‐QualityControlSamlpesMatrixSpike/MatrixSpikeDuplicate‐CongenersLaboratory Type ReplicateASHLANDMS 1ASHLANDMS 2ASHLANDMSD 1ASHLANDMSD 2EPA_NEICMS 1EPA_NEICMS 2EPA_NEICMSD 1EPA_NEICMSD 2EPA_R4_1MS 1EPA_R4_1MS 2EPA_R4_1MS 3EPA_R4_1MSD 1EPA_R4_1MSD 2EPA_R4_1MSD 3EPA_R4_2MS 1EPA_R4_2MS 2EPA_R4_2MSD 1EPA_R4_2MSD 2EPA_R4_3MS 1EPA_R4_3MS 2EPA_R4_3MSD 1EPA_R4_3MSD 2SCCWRPMS 1SCCWRPMS 2SCCWRPMS 3SCCWRPMSD 1SCCWRPMSD 2SCCWRPMSD 3EPA_NERL/ORD_LV_1MS 1EPA_NERL/ORD_LV_1MS 2EPA_NERL/ORD_LV_1MSD 1EPA_NERL/ORD_LV_1MSD 2EPA_NERL/ORD_LV_2MS 1EPA_NERL/ORD_LV_2MS 2EPA_NERL/ORD_LV_2MSD 1EPA_NERL/ORD_LV_2MSD 2Hx‐Sed Hp‐Sed P26P40 P41 P44 P50P622.61 2.55 5.45 3.65 3.88 5.97 8.01 9.802.29 3.23 4.62 3.36 3.08 3.60 5.46 4.555.04 5.61 9.04 6.00 6.17 7.35 7.80 5.894.19 4.38 6.49 4.26 4.38 4.87 5.38 3.962.18 2.27 3.53 3.23 3.37 3.98 5.12 6.102.68 3.45 5.28 2.94 4.07 3.78 4.69 6.353.13 3.15 5.72 1.28 3.58 4.06 6.70 3.713.58 3.49 7.77 2.87 4.41 5.98 5.31 4.58AverageRelativePercentDifference(%RPD)Method8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐9‐QualityControlSamlpesMatrixSpike/MatrixSpikeDuplicate‐CongenersLaboratory Type ReplicateASHLANDMS 1ASHLANDMS 2ASHLANDMSD 1ASHLANDMSD 2EPA_NEICMS 1EPA_NEICMS 2EPA_NEICMSD 1EPA_NEICMSD 2EPA_R4_1MS 1EPA_R4_1MS 2EPA_R4_1MS 3EPA_R4_1MSD 1EPA_R4_1MSD 2EPA_R4_1MSD 3EPA_R4_2MS 1EPA_R4_2MS 2EPA_R4_2MSD 1EPA_R4_2MSD 2EPA_R4_3MS 1EPA_R4_3MS 2EPA_R4_3MSD 1EPA_R4_3MSD 2SCCWRPMS 1SCCWRPMS 2SCCWRPMS 3SCCWRPMSD 1SCCWRPMSD 2SCCWRPMSD 3EPA_NERL/ORD_LV_1MS 1EPA_NERL/ORD_LV_1MS 2EPA_NERL/ORD_LV_1MSD 1EPA_NERL/ORD_LV_1MSD 2EPA_NERL/ORD_LV_2MS 1EPA_NERL/ORD_LV_2MS 2EPA_NERL/ORD_LV_2MSD 1EPA_NERL/ORD_LV_2MSD 2PCB209 eHCHPCB209 eHCHPCB209 eHCHPCB209 eHCHPCB209 eHCH73.8 25373.8 10173.3 25973.3 103 73.6 25662.2 27062.2 108 17.1 6.4665.1 25265.1 101 63.7 261 11.8 2.78 14.5 4.6286.2 23486.2 93.886.8 24086.8 96.0 86.5 23775.2 22775.2 90.7 13.6 3.3472.3 22572.3 89.9 73.7 226 18.2 6.58 15.9 4.9678.0 23078.0 92.068.2 23768.2 94.966.8 24566.8 97.9 71.0 23768.0 23268.0 92.9 13.7 0.88768.4 23368.4 93.1 0.249 1.8562.0 23762.0 95.0 66.1 234 7.42 3.06 7.14 1.9374.9 22274.9 89.078.6 22078.6 88.1 76.8 22169.1 21769.1 87.0 8.07 2.2569.4 21669.4 86.6 69.3 217 12.4 1.81 10.2 2.0379.7 21979.7 87.480.1 21680.1 86.5 79.9 21768.7 22468.7 89.5 14.8 2.3868.0 21868.0 87.1 68.3 221 16.3 0.677 15.6 1.5382.1 21382.1 85.283.1 21883.1 87.288.1 22388.1 89.2 84.4 21873.3 21473.3 85.6 11.3 0.46874.8 21574.8 86.0 10.5 1.3976.2 22376.2 89.2 74.8 217 14.5 0.00 12.1 0.61881.7 21981.7 87.681.8 22281.8 88.8 81.8 22169.3 21969.3 87.6 16.4 0.0070.2 24170.2 96.4 69.8 230 15.3 8.21 15.8 4.1081.3 21781.3 86.982.5 22982.5 91.7 81.9 22371.8 22571.8 90.2 12.4 3.7671.1 22571.1 89.9 71.4 225 14.8 1.93 13.6 2.85Concentration(pg/μL)AvgConc(pg/μL) %RPDPCB209(Surrogate)Spikedat100pg/μL,eHCH(Surrogate)Spikedat250pg/μLAvg%RPD%RecoveryMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2TableA2‐10‐LaboratoryParticipantsLaboratoryDesignationASHLANDEPA_NEICEPA_NERL/ORD_LV_1 Analyst1EPA_NERL/ORD_LV_2 Analyst2EPA_R4_1RefereeEPA_R4_2Analyst1EPA_R4_3Analyst2SCCWRPMethod8276U.S.EPAORCRInter‐laboratoryValidation:AnalyticalDataReportAugust2012Attachment2

# Attachment 3

Final Phase III Toxaphene Summa ry 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

LaboratoryASHLANDEPA_ NEICEPA_R4_1EPA_R4_2EPA_R4_3SCCWRPEPA_NERL/ORD_1EPA_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 

# LaboratoryASHLANDEPA_ NEICEPA_R4_1EPA_R4_2EPA_R4_3SCCWRPEPA_NERL/ORD_1EPA_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.