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 for Fish Tissue 

STATISTICAL ANALYSIS 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 

Task Order No. EP-G11S-00001 

Work Order No. B-008 
TABLE OF CONTENTS 

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

II. Inter-Laboratory Comparisons ...................................................................................................3 

III. Intra-Laboratory Comparisons ...................................................................................................9 

IV. Statistical Tests ........................................................................................................................11 

V. References ................................................................................................................................32 

Appendix A – Normality Testing of Technical Toxaphene and Toxaphene Congener Data 

Appendix B – Results and 3-Sigma Control Limits for Terry Creek Fish Tissue Samples 

Appendix C – Results and 3-Sigma Control Charts for Quality Control Samples 

TABLES 

Table II-1: Terry Creek 1 Fish Sample Results ........................................................................4 

Table II-2: Terry Creek 2 Fish Sample Results ........................................................................4 

Table II-3: Technical Toxaphene 2nd Source Standard and LCS Recoveries ...........................5 

Table II-4: Toxaphene Congeners LCS Recoveries .................................................................6 

Table II-5: Technical Toxaphene Matrix Spike Recoveries .....................................................7 

Table II-6: Toxaphene Congeners Matrix Spike Recoveries ...................................................8 

Table III-1: Intra-Laboratory Comparison for Terry Creek Samples ........................................9 

Table III-2: Intra-Laboratory Comparison for Laboratory 

 Control Samples (LCS) ........................................................................................10 

Table III-3: Intra-Laboratory Comparison for Matrix Spikes/Matrix 

 Spike Duplicates (MS/MSD) ................................................................................10 

Table IV-1: Individual Values Outside of 3-Sigma Control Limits ........................................13 

Table IV-2: Laboratory Observations Within and Outside of Control Limits .........................14 

Table IV-3: Method Blanks – Detections and Associated Laboratories ..................................15 

Table IV-4: Source Fish – Detections and Associated Laboratories .......................................16 
TABLE OF CONTENTS (continued) 

TABLES (continued) 

Table IV-5: Second Source Standard – Toxaphene and Surrogates ........................................17 

Table IV-6: Low-Level LCS Results – Toxaphene and Congeners ........................................17 

Table IV-7: Mid-Level LCS Results – Toxaphene and Congeners .........................................18 

Table IV-8: Spiked Surrogates ................................................................................................18 

Table IV-9: MS/MSD Results – Toxaphene, Surrogates and Congeners ...............................19 

Table IV-10: Means and Standard Deviations Comparing Toxaphene Results 

 Between Analysts – Fish 1 ...................................................................................20 

Table IV-11: Means and Standard Deviations Comparing Toxaphene Results 

 Between Analysts – Fish 2 ...................................................................................20 

Table IV-12: Means and Standard Deviations Comparing Hx-Sed Results 

 Between Analysts – Fish 1 ...................................................................................21 

Table IV-13: Means and Standard Deviations Comparing Hx-Sed Results 

 Between Analysts – Fish 2 ...................................................................................21 

Table IV-14: Means and Standard Deviations Comparing Hp-Sed Results 

 Between Analysts – Fish 1 ...................................................................................22 

Table IV-15: Means and Standard Deviations Comparing Hp-Sed Results 

 Between Analysts – Fish 2 ...................................................................................22 

Table IV-16: Means and Standard Deviations Comparing P26 Results 

 Between Analysts – Fish 1 ...................................................................................23 

Table IV-17: Means and Standard Deviations Comparing P26 Results 

 Between Analysts – Fish 2 ...................................................................................23 

Table IV-18: Means and Standard Deviations Comparing P40 Results 

 Between Analysts – Fish 1 ...................................................................................24 

Table IV-19: Means and Standard Deviations Comparing P40 Results 

 Between Analysts – Fish 2 ...................................................................................24 

Table IV-20: Means and Standard Deviations Comparing P41 Results 

 Between Analysts – Fish 1 ...................................................................................25 

Table IV-21: Means and Standard Deviations Comparing P41 Results 

 Between Analysts – Fish 2 ...................................................................................25 
TABLE OF CONTENTS (continued) 

TABLES (continued) 

Table IV-22: Means and Standard Deviations Comparing P44 Results 

 Between Analysts – Fish 1 ...................................................................................26 

Table IV-23: Means and Standard Deviations Comparing P44 Results 

 Between Analysts – Fish 2 ...................................................................................26 

Table IV-24: Means and Standard Deviations Comparing P50 Results 

 Between Analysts – Fish 1 ...................................................................................27 

Table IV-25: Means and Standard Deviations Comparing P50 Results 

 Between Analysts – Fish 2 ...................................................................................27 

Table IV-26: Means and Standard Deviations Comparing P62 Results 

 Between Analysts – Fish 1 ...................................................................................28 

Table IV-27: Means and Standard Deviations Comparing P62 Results 

 Between Analysts – Fish 2 ...................................................................................28 

Table IV-28: Z-Scores for Laboratory Quality Assurance Samples .........................................30 

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

Phase III Statistical Analysis Report    Page 1

I. INTRODUCTION 

Objective 

Fish tissue extract and quality control sample data collected from Phase III of the SW-846 

Method 8276 validation study was assessed using statistical methodologies in order to determine 

the robustness and ruggedness of Method 8276 for use in the analysis of technical toxaphene and 

toxaphene congeners in fish tissue. The method performance characteristics used to evaluate the 

data included the accuracy/bias and precision of the data sets. Additionally, the data sets were 

subjected to distribution analysis to determine the normality and overall variance. Data sets were 

assessed considering the entire population of data submitted by all participating laboratories 

(inter-laboratory data), with specific evaluations for inter-laboratory data sets as well as data sets 

which compared results between analysts from a single laboratory (intra-laboratory). 

Prior to conducting the statistical evaluation, data were first subjected to validation to ensure all 

method and quality control parameter requirements were met for the analysis. Only valid data 

that were determined to be usable for the purpose of evaluating the efficacy of Method 8276 for 

fish tissue analysis were included in the statistical evaluation. Data validation resulted in the 

elimination of two data sets. These two data sets were generated using a HP-5MS analytical 

column, which was allowed by Method 8276, but was not the recommended or preferred DBXLB column. Data generated using this column resulted in toxaphene congener results which 

did not conform to the distribution of results reported by all other participating laboratories, or 

which were not reportable due to co-elution problems. All other data were deemed valid and 

usable for inclusion in the statistical evaluation. 

Method Performance Characteristics 

Bias/Trueness 

For the purposes of this study, trueness is a performance characteristic that represents the known 

systematic error in a result; therefore, bias is a measure of trueness. According to EPA guidance 

document QA/G-5, Guidance for Quality Assurance Project Plans, bias is the systematic or 

persistent distortion of a measurement process and is measured as a function of the difference 

between a reported value, or the statistical mean for a set of reported values, and the known 

amount of the analyte present. Usually, systematic error is caused by the effect a specific sample 

matrix has on the ability to recover and quantitate a target analyte using a specific method. In 

the Phase III validation study for technical toxaphene and toxaphene congeners, bias was 

evaluated through the analysis of fish tissue sample extracts prepared by EPA Region 4 Lab, 

matrix spikes, surrogate recoveries, and evaluation of the laboratory control samples. 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation: August 2012

Phase III Statistical Analysis Report    Page 2

Percent recovery provides a measure of the bias in the results, and is calculated as 

follows: 

Recovery (% ) 100 



 



  

n

m s

Conc

Conc Conc R

 Concm = Concentration of target analyte measured in analysis of spiked sample 

 Concs = Concentration of target analyte in the unspiked sample 

 Concn = Nominal concentration of the spiked aliquot 

Precision 

Precision is a measure of the magnitude of random error(s), which can be attributed to the degree 

of repeatability and reproducibility of the results from a specific preparatory and/or analytical 

method. The precision of the technical toxaphene and toxaphene congeners results were 

determined using the statistical calculations for standard deviation (SD) and relative standard 

deviation (RSD) on the mean. 

Data values reported by each Phase III participant were compiled to include each concentration 

of technical toxaphene and toxaphene congeners, surrogates in spiked samples, and each spiked 

QC sample. The reported values from the Phase III participants were summed for each 

concentration level reported. A mean value was calculated using the equation below. 

The arithmetic mean is the sum of the results, divided by the number of measurements, as 

follows: 





n

i

i x

n

x

1

1

x = mean 

n = number of measurements 

 i x = result 

The SD and RSD represent the amount of variability or statistical dispersion of the results from 

the mean value, and provide an indication of the magnitude of random error. Relative standard 

deviation (% RSD) is the absolute value of the coefficient of variation and is determined by 

dividing the variance of the results by the average (mean) and multiplying by 100. 

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

Phase III Statistical Analysis Report    Page 3

 Standard Deviation (SD) measures the amount of dispersion of the result, as follows: 

ܵܦ ൌ ඪቌ

n

i 1

ሺx୧ െ x ሻቍ

ሺ݊െ1ሻ

 Percent relative standard deviation (%RSD) is a measure of variance, expressed as a 

percentage, as follows: 

ൌ ܦ%ܴܵ

ܦܵ

x

100	ݔ	

 Precision can also be evaluated for sample pairs (duplicates) by calculating a percent 

difference (%D), also known as the relative percent difference (RPD), as follows: 

%	ܦ݂݂݅ ൌ ቮ ݔଵ െ ݔଶ

ቀ

ଶݔ ൅ ଵݔ

2 ቁ

ቮ 	ܺ	100

II. INTER-LABORATORY COMPARISONS 

Ruggedness is a measure of the degree to which an analytical method results in accurate and 

reproducible results when performed multiple times by independent laboratories. The 

Toxaphene Phase III method validation study primarily focused on the evaluation of interlaboratory data generated by several laboratories that were invited from inside and outside of 

EPA to join this Phase III study. This evaluation included an assessment of the degree to which 

inter-laboratory results for fish tissue samples and quality control samples met reasonable 

benchmarks for acceptable bias/trueness, and precision/variance. The measurement performance 

criteria for bias and variance, as well as control charts were developed, and are included in this 

report for the purpose of establishing the validity of the analytical protocol in Method 8276 for 

fish tissue analysis. 

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

Phase III Statistical Analysis Report    Page 4

Table II-1 

Terry Creek 1 Fish Sample Results 

Sample ID No. of 

Participants 

Grand Mean 

(ug/kg) 

Standard 

Deviation 

Reproducibility 

(%RSD) 

Toxaphene 8 7030 1170 16.7 

Hx-Sed 8 160 10.7 6.65 

Hp-Sed 8 184 10.3 5.59 

P26 8 16.0 0.738 4.62 

P40 8 21.8 2.05 9.37 

P41 8 8.93 0.322 3.60 

P44 8 9.53 0.693 7.28 

P50 8 16.5 1.20 7.25 

P62 8 22.3 7.01 31.5 

Table II-2 

Terry Creek 2 Fish Sample Results 

Sample ID No. of 

Participants 

Grand Mean 

(ug/kg) 

Standard 

Deviation 

Reproducibility 

(%RSD) 

Toxaphene 8 650 112 17.2 

Hx-Sed 8 10.8 0.838 7.75 

Hp-Sed 8 15.1 0.963 6.37 

P26 8 2.32 0.063 2.71 

P40 8 2.49 0.114 4.57 

P41 8 1.05 0.027 2.53 

P44 8 1.34 0.099 7.40 

P50 8 2.57 0.125 4.87 

P62 8 3.07 1.02 33.3 

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

Phase III Statistical Analysis Report    Page 5

Technical Toxaphene 2nd Source Standard and LCS Recoveries 

Table II-3 

2nd Source 

Standard Toxaphene 

ID No. of 

Participants 

True Value 

(pg/uL) 

Grand Mean

(pg/uL) % Recovery Std. Deviation 

Reproducibility

(% RSD) 

Second 

Source Std. 8 150 159 106 9.85 6.20 

LCS 1 8 50 57.3 115 9.7 16.9 

LCS 2 8 200 207 104 13.4 6.50 

PCB 209 

LCS1 8 100 95.0 95.0 1.9 2.00 

eHCH 

LCS1 8 250 230.5 92.2 21.0 9.10 

PCB 209 

LCS2 8 100 90.2 90.2 5.4 6.00 

eHCH 

LCS2 8 250 240 95.8 15.4 6.40 

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

Phase III Statistical Analysis Report    Page 6

Toxaphene Congeners LCS Recoveries 

Table II-4

Hx-Sed 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %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 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %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 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %RSD 

LCS1 8 100 97.9 97.9 5.27 5.39 

LCS2 8 2 1.83 91.4 0.36 19.7 

P40 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %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 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %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 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %RSD 

LCS1 8 100 99.4 99.4 8.85 8.91 

LCS2 8 2 1.99 99.8 0.16 8.09 

P50 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %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 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %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

Phase III Statistical Analysis Report    Page 7

Technical Toxaphene Matrix Spike Recoveries 

Table II-5 

ID No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation % RSD 

Matrix 

Spike 8 200 186 92.8 23.0 12.4 

Matrix 

Spike 

Duplicate 

8 200 182 90.9 21.3 11.7 

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

Phase III Statistical Analysis Report    Page 8

Toxaphene Congeners Matrix Spike Recoveries 

Table II-6

Hx-Sed 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %RSD 

MS 8 100 92.6 92.6 6.29 6.79 

MSD 8 100 89.8 89.8 5.92 6.60 

Hp-Sed 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %RSD 

MS 8 100 91.9 91.9 5.56 6.05 

MSD 8 100 89.2 89.2 4.78 5.36 

P26 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %RSD 

MS 8 100 88.5 88.5 4.93 5.57 

MSD 8 100 83.3 83.3 4.23 5.08 

P40 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %RSD 

MS 8 100 91.9 91.9 6.11 6.65 

MSD 8 100 88.9 88.9 4.66 5.24 

P41 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %RSD 

MS 8 100 91.8 91.8 6.67 7.26 

MSD 8 100 88.0 88.0 6.00 6.81 

P44 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %RSD 

MS 8 100 95.7 95.7 8.94 9.34 

MSD 8 100 91.2 91.2 7.63 8.37 

P50 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %RSD 

MS 8 100 90.4 90.4 6.67 7.37 

MSD 8 100 85.1 85.1 6.54 7.68 

P62 

ID 

No. of 

Participants 

True 

Value 

Grand 

Mean 

% 

Recovery 

Std. 

Deviation %RSD 

MS 8 226 227 101 33.5 14.7 

MSD 8 226 217 95.9 29.0 13.4 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation: August 2012

Phase III Statistical Analysis Report    Page 9

III. INTRA-LABORATORY COMPARISONS 

Robustness is a measure of the degree to which the method is unaffected by minor variations in 

operating conditions and/or analysts and laboratories. Robustness was generally assessed by 

comparison of intra-laboratory analyst precision. As part of this evaluation, the precision or 

agreement between fish tissue and quality control sample results among analysts within each lab 

was assessed. The EPA Region 4 laboratory in Athens, GA reported data from three analysts. 

The intra-laboratory data was evaluated for analyst precision and therefore was evaluated against 

the benchmarks of obtaining a percent relative standard deviation (%RSD) of less than 30% for 

all measurements. This benchmark criteria was met for this evaluation. 

Table III-1 

Intra-Laboratory Comparison For Terry Creek Samples 

ID % RSD Fish 1 % RSD Fish 2 

EPA Region 4 Lab – 3 analysts 

Toxaphene 7.78 5.17 

Hx-Sed 4.07 7.01 

Hp-Sed 4.47 7.61 

P26 4.48 6.74 

P40 2.19 4.60 

P41 2.58 5.07 

P44 6.68 7.37 

P50 3.51 4.85 

P62 13.9 11.5 

Fish tissue Terry Creek 1 and Terry Creek 2 variance for technical toxaphene results 

 %RSD < 7.78% for all three analysts from EPA Region 4 laboratory 

Fish tissue Terry Creek 1 and Terry Creek 2 variance for toxaphene congener results 

 %RSD < 13.9% for all three analysts from EPA Region 4 laboratory 

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

Phase III Statistical Analysis Report    Page 10

Table III-2 

Intra-Laboratory Comparison For Laboratory Control Samples (LCS)

ID % RSD LCS 1 % RSD LCS 2 

EPA Region 4 Lab – 3 analysts 

Toxaphene 17.6 9.54 

Hx-Sed 4.15 5.69 

Hp-Sed 4.93 4.10 

P26 4.57 8.71 

P40 3.40 5.03 

P41 3.63 5.55 

P44 4.42 5.27 

P50 3.60 4.93 

P62 5.88 5.14 

Laboratory Control Sample 1 (LCS 1) and LCS 2 variance for technical toxaphene results 

 %RSD < 17.6% for all three analysts from EPA Region 4 laboratory 

LCS 1 and LCS 2 variance for toxaphene congener results 

 %RSD < 8.71% for all three analysts from EPA Region 4 laboratory 

Table III-3 

Intra-Laboratory Comparison For Matrix Spikes/Matrix Spike Duplicates (MS/MSD) 

ID % RSD 

MATRIX SPIKE 

% RSD 

MATRIX SPIKE 

DUPLICATE 

EPA Region 4 Lab – 3 analysts 

Toxaphene 4.92 4.57 

Hx-Sed 5.74 4.42 

Hp-Sed 6.18 4.74 

P26 5.84 3.93 

P40 4.66 3.26 

P41 4.76 3.33 

P44 6.36 4.67 

P50 4.46 3.10 

P62 7.06 6.53 

Matrix Spike (MS) and Matrix Spike Duplicate (MSD) variance for technical toxaphene results 

 %RSD < 4.92% for all three analysts from EPA Region 4 laboratory 

Matrix Spike (MS) and Matrix Spike Duplicate (MSD) variance for toxaphene congener results 

 %RSD < 7.06% for all three analysts from EPA Region 4 laboratory 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation: August 2012

Phase III Statistical Analysis Report    Page 11

IV. STATISTICAL TESTS 

Normality Testing 

The distribution of the data generated during Phase III of the SW-846 Method 8276 validation 

study is important to ascertain for several reasons: 1) it can indicate the need to transform a 

dataset prior to evaluation; 2) it can influence the decision to use parametric versus nonparametric statistical evaluation methods (since some methods require data to be normally 

distributed); and 3) it can signal potential biases or other issues associated with the analytical 

method used to generate the data. For the purposes of this study, statistical methods were used to 

determine if the results reported by Method 8276 on the fish tissue extracts and quality control 

samples met certain population characteristics for normality and were within reasonable 

agreement and/or specified variance limits. Normality testing was performed using the Minitab 

statistical software program. In order to detect departures from normality present in the 

analytical results, the Anderson-Darling Test for Normality (ADT) was used. The ADT is 

considered one of the more robust statistical tests to detect departures from normality and was 

applied to the Terry Creek analytical results for toxaphene and for each congener. The test was 

run independently for each fish (i.e., Fish 1 and Fish 2). ADT results are included in graphical 

form in Appendix A. 

Interpretation of the ADT output provided in Appendix A is relatively straightforward. The 

ADT returns what is termed an A-squared test statistic, as well as an associated p-value. The ‘A 

squared’ value is obtained from a probability distribution which defines whether to accept or 

reject the null hypothesis at the defined level of significance, which in this case is 0.05 or 95% 

confidence level. When the associated p-value is less than or equal to 0.05, the hypothesis of 

normality is rejected at the 95% confidence level. In other words, when the p-value is less than 

or equal to 0.05, we can say with 95% certainty that the data are not normally distributed. 

Conversely, when the p-value is greater than 0.05, it can be said that no significant deviation 

from normality was observed. 

For the Terry Creek results, no significant deviation from normality was observed (i.e., all p 

values were greater than 0.05), with the following exceptions: 

 Fish 1, P40 (A-squared = 0.88, p = 0.019) 

 Fish 2, Toxaphene (A-squared = 1.41, p < 0.005) 

 Fish 2, P50 (A-squared = 0.96, p = 0.012) 

A lognormal transformation was performed for each of the above datasets to mitigate the 

observed deviations in normality. After transformation, the ADT was once again performed. In 

each case, the deviation from normality was not mitigated by lognormal transformation. ADT 

output for lognormal transformed data is provided in Appendix A. Given these results, it appears 

that in these limited cases, there is a significant deviation from normality. 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation: August 2012

Phase III Statistical Analysis Report    Page 12

In order to determine whether these departures from normality indicate a methodological bias or 

other systemic issue, the Phase III data were evaluated following the Inter-laboratory Validation 

for Fish Tissue Study Plan, dated September 2011, using the method performance characteristics 

and evaluation criteria. The data from the Terry Creek fish tissue were assessed for 

variance/statistical dispersion by calculating the standard deviation and relative standard 

deviation (RSD) for the fish tissue Terry Creek samples, as well as for the quality control 

samples, including the LCS and Matrix Spikes. A 30% RSD was used as the benchmark, which 

would indicate variance was within an acceptable limit. However, since the benchmarks for 

acceptable precision (dispersion) of 30 % RPD and/or 30 % RSD were met for all interlaboratory and intra-laboratory Terry Creek 1 and 2 sample data and quality control sample data, 

the few exceptions to normality in the data distribution do not appear to indicate there is a 

problem with the method. Rather, it is likely the variability in analytical technique or process. 

The variability in the analyses can sometimes be correlated to the quality control results. For the 

Technical Toxaphene analyses, variability was primarily noted in LCS and matrix spikes results. 

For the LCS results, variability was evident in the high recoveries reported for the Low-Level 

LCS toxaphene (LCS 1 spiked at 50 pg/uL) reported by NEIC (141% and 132%) and EPANERL/ORD-LV-2 (133% and 150%). As reported in the Analytical Data Report, one possible 

source of variability occurred as a result of the presence of contaminant peaks that eluted within 

the retention times/peak area assigned to quantitation of technical toxaphene, as evidenced by 

blank contamination. Variability was also noted in the LCS and matrix spike results for 

congeners. The variability in LCS congeners results stems from the low recoveries reported for 

Parlar 62 in the Low-Level LCS (LCS 2 spiked at 2 pg/uL) by SCCWRP (69.4%, 67.8%, for two 

of the three replicates); EPA-NERL/ORD-LV-2 (45.8% and 46.5%); and EPA-NERL/ORD-LV1 (59.8% and 74.6%). The low recoveries for the LCS results reported by SCCWRP may be a 

result of variability in instrument response near the LLOQ. The low LCS recoveries reported by 

the EPA-NERL/ORD-LV-1 participant may be due to the method of quantitation used. The 

EPA-NERL/ORD-LV-1 participant used a linear regression curve in the calibration rather than a 

relative response factor or quadratic curve method. As noted in Method 8276, Section 11.4.5.4, 

the use of linear regression analysis has the potential to cause a significant bias in the lower 

portion of the calibration curve, while the relative percent difference and quadratic methods do 

not. 

Matrix spike recoveries were low for technical toxaphene results reported by all laboratories 

except for SCCWRP, while matrix spike results were slightly low for toxaphene congener results 

reported by all laboratories except for EPA-R4-1. The low matrix spike results may indicate 

possible matrix interference due to the fish matrix. 

Other than the potential sources of variability, no trends or biases were noted in the Analytical 

Data Report for the congener data. Therefore, the deviations from normality demonstrated for 

the P40 and P50 data were most likely a result of normal statistical variability in the analytical 

process, and do not appear to indicate a significant problem with the Method 8276 methodology. 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation: August 2012

Phase III Statistical Analysis Report    Page 13

Given this, as well as the fact that the deviations from normality were limited to only three 

analytes across both sets of fish samples, the data will be evaluated in its raw (i.e., 

untransformed) state using standard parametric analytical techniques. 

Bar Graphs and 3-sigma Control Limits – Terry Creek 

In order to statistically evaluate the data generated during this study, upper control limits (UCL) 

and lower control limits (LCL) were established using what is termed a 3-sigma approach (a 

standard approach for generating statistical quality control charts). For ease of display, bar 

graphs depicting analytical results were constructed for toxaphene and each congener for the 

Terry Creek data and are included in Appendix B. The bar graphs represent individual analytical 

results (for each replicate). A center line representing the Grand Mean is indicated on the 

graphs, along with lines representing the UCL and LCL. The UCLs and LCLs represent three 

standard deviations (or 3-sigma) above (UCL) and below (LCL) the Grand Mean. These control 

levels were selected because in a normal distribution, 99.7% of observations will fall within three 

standard deviations of the mean. Therefore, if a process is in a state of statistical control, all data 

points should fall within the 3-sigma UCL and LCL. Data points that fall outside of the control 

limits may be indicative of a process problem (such as the nature of the media, method of sample 

preparation, and/or analytical technique) that may warrant further investigation. Table IV-1 

shows the number of individual analytical results outside of the 3-sigma control limits. Table 

IV-2 shows the total number of observations for each analyst, and the number of those 

observations that fell outside of the control limits. 

Table IV-1 

Individual Values Outside of 3-sigma Control Limits*

Analyte Number of Individual Values 

Outside of Control Limits - Fish 1

Number of Individual Values 

Outside of Control Limits - Fish 2

Toxaphene 0 (18) 0 (18) 

Hx-Sed 0 (18) 0 (18) 

Hp-Sed 0 (18) 0 (18) 

P26 0 (18) 0 (18) 

P40 0 (18) 0 (18) 

P41 0 (18) 0 (18) 

P44 0 (18) 2 (18) 

P50 0 (18) 1 (18) 

P62 0 (16) 0 (18) 

Total 0 (160) 3 (162) 

*Total number of individual values is included in parentheses. 

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

Phase III Statistical Analysis Report    Page 14

Table IV-2 

Laboratory Observations Within and Outside of Control Limits 

Laboratory (Analyst) Total 

Number of 

Observations

Number of 

Observations Outside 

of Control Limits 

Percentage of 

Observations Outside 

of Control Limits 

Ashland 36 1 2.8 

EPA NEIC 34 0 0.0 

EPA R4 1 54 0 0.0

EPA R4 2 36 0 0.0

EPA R4 3 36 0 0.0

SCCWRP 54 0 0.0

EPA ORD-LV 1 36 0 0.0

EPA ORD-LV 2 36 2 5.6 

Total 322 3 0.9 

As shown in Table IV-1, none of the 160 individual measurements for Fish 1 and only three (two 

for P44 and one for P50) of the 162 individual measurements (< 2%) for Fish 2 fall outside of the 

3-sigma control limits. In each of these cases, the analytical value outside of the 3-sigma control 

limits was one of two replicates, with the other falling within the control limits. If an average of 

replicates is taken to generate a single analytical result for the analyst (as was done to generate 

the Grand Mean), then the average of each of these replicates falls within the control limits. 

Based on this evaluation, it appears that the analytical process is in a state of statistical control. 

Control Charts – Laboratory Quality Control Samples 

Individual control charts (I-charts) were constructed for laboratory quality control samples and 

are included in Appendix C. Charts were developed for the following quality control samples: 

 Blank Samples 

o Method Blanks 

o Source Fish 

 Spiked Samples 

o Second Source Standard 

o LCS (low-level and mid-level) 

o Surrogates 

o Matrix Spikes/Matrix Spike Duplicates 

I-charts developed for the quality control samples do not employ a standard 3-sigma UCL and 

LCL approach as was done for the Terry Creek samples. Rather, alternative reference lines have 

been provided to assist in evaluating laboratory performance. 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation: August 2012

Phase III Statistical Analysis Report    Page 15

For the method blanks and source fish, the following reference lines are included on the I-charts: 

 zero concentration line (this includes “non-detects” as well as laboratory results reported 

as “<”) 

 mean concentration line 

 calibration standard lines (set at 50% of the lowest calibration standard [25 pg/uL] for 

technical toxaphene, and at 50-100% of the lowest calibration standard for toxaphene 

congeners) 

For spiked samples, the following reference lines are included: 

 mean concentration line 

 true value line (actual spiked concentration of the second source standard, LCS, 

surrogates, and MS/MSDs) 

 true value reference lines (+/- 20% and +/- 30% of true value for second source standard; 

+/- 10%, +/- 15% and +/- 20% of true value for mid-level LCS; +/- 20%, +/- 30% and +/-

50% of true value for low-level LCS; +/- 20% and +/- 30% of true value for surrogates 

and MS/MSDs) 

A discussion of laboratory quality control sample results is provided below. 

Blank Samples 

Tables IV-3 and IV-4 show the distribution of analytical results compared to the reference points 

discussed above for method blanks and source fish, as well as the analytical laboratories 

associated with analyte detections. 

Table IV-3 

Method Blanks – Detections and Associated Laboratories*

Analyte Number 

of 

Detections 

Number of 

Detections ≤ 50% 

of the lowest 

calibration 

standard 

Number of 

Detections 

Between 50%-

100% of the lowest 

calibration standard 

Number of 

Detections 

>100% of the 

lowest calibration 

standard 

Toxaphene 12 (18) 12 (18) 0 (18) 0 (18) 

Hx-Sed 3 (18) 3 (18) 0 (18) 0 (18) 

Hp-Sed 3 (18) 3 (18) 0 (18) 0 (18) 

P26 2 (18) 0 (18) 2 (18) 0 (18) 

P40 2 (18) 0 (18) 2 (18) 0 (18) 

P41 2 (18) 0 (18) 2 (18) 0 (18) 

P44 2 (18) 0 (18) 2 (18) 0 (18) 

P50 2 (18) 0 (18) 2 (18) 0 (18) 

P62 2 (18) 2 (18) 0 (18) 0 (18) 

Total 30 (162) 20 (162) 10 (18) 0 (18) 

*Total number of individual values is included in parentheses. 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation: August 2012

Phase III Statistical Analysis Report    Page 16

Table IV-4 

Source Fish – Detections and Associated Laboratories*

Analyte Number 

of 

Detections 

Number of 

Detections ≤ 50% 

of the lowest 

calibration 

standard 

Number of 

Detections 

Between 50-100% 

of the lowest 

calibration standard 

Number of 

Detections 

>100% of the 

lowest calibration 

standard 

Toxaphene 17 (18) 13 (18) 4 (18) 0 (18) 

Hx-Sed 5 (18) 5 (18) 0 (18) 0 (18) 

Hp-Sed 5 (18) 5 (18) 0 (18) 0 (18) 

P26 9 (18) 7 (18) 1 (18) 1 (18) 

P40 5 (18) 3 (18) 2 (18) 0 (18) 

P41 6 (18) 4 (18) 2 (18) 0 (18) 

P44 6 (18) 4 (18) 2 (18) 0 (18) 

P50 10 (18) 6 (18) 4 (18) 0 (18) 

P62 5(18) 5 (18) 0 (18) 0 (18) 

Total 68 (162) 52 (162) 15 (162) 1 (162) 

*Total number of individual values is included in parentheses. 

As shown in Table IV-3, and Appendix C-1 to C-5, laboratories reported method blank 

detections in 30 (19%) of 162 individual measurements. Of those 30 detections, 20 fell below 

50% of the lowest calibration standard reference line, with the remaining 10 falling between 50% 

and 100% of the lowest calibration standard reference line. As shown in Table IV-4, and 

Appendix C-6 to C-10, laboratories reported source fish detections in 68 (42%) of 162 individual 

measurements. Of those 68 detections, 52 fell below 50% of the lowest calibration standard 

reference line; 15, fell between 50% and 100%; and one, above 100% of the lowest calibration 

standard reference line. 

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

Phase III Statistical Analysis Report    Page 17

Spiked Samples 

Tables IV-5 through IV-9 show the distribution of analytical results compared to the reference 

points discussed above for the following spiked samples: second source standard, low-level LCS, 

mid-level LCS, spiked surrogates and MS/MSDs. 

Table IV-5 

Second Source Standard – Toxaphene and Surrogates*

Analyte Number of Observations 

 +/- 20% of True Value Between +/- 20% and 

+/- 30% of True Value 

> +/- 30% of True 

Value 

Toxaphene 18 (18) 0 (18) 0 (18) 

PCB 209 18 (18) 0 (18) 0 (18) 

ε-HCH 17 (18) 1 (18) 0 (18) 

Total 53 (54) 1 (54) 0 (54) 

*Total number of individual values is included in parentheses. 

As shown in Table IV-5 and Appendix C-11 to C-12 of the 54 individual results for the second 

source standard samples, 53 (98%) were within +/- 20% of the true value. One result (2%) fell 

between +/- 20% and +/- 30% of the true value, with none exceeding +/- 30%. 

Table IV-6 

Low-Level LCS Results – Toxaphene and Congeners* 

Analyte Number of Observations 

 +/- 20% of 

True Value 

Between +/- 20% 

and +/- 30% of 

True Value 

Between +/- 30% 

and +/- 50% of 

True Value 

> +/- 50% of 

True Value 

Toxaphene 10 (18) 2 (18) 6 (18) 0 (18) 

Hx-Sed 17 (18) 1 (18) 0 (18) 0 (18) 

Hp-Sed 17 (18) 1 (18) 0 (18) 0 (18) 

P26 15 (18) 0 (18) 2 (18) 1 (18) 

P40 17 (18) 0 (18) 1 (18) 0 (18) 

P41 17 (18) 1 (18) 0 (18) 0 (18) 

P44 17 (18) 0 (18) 1 (18) 0 (18) 

P50 18 (18) 0 (18) 0 (18) 0 (18) 

P62 14 (18) 1 (18) 3 (18) 0 (18) 

Total 143 (162) 5 (162) 13 (162) 1 (162) 

*Total number of individual values is included in parentheses. 

As shown in Table IV-6 and Appendix C-13, and C-15 to C-22, of the 162 individual results for 

the low-level LCS, 143 (88%) were within +/- 20% of the true value. Five measurements (3%) 

fell between +/- 20% and +/- 30% of the true value, and 13 (8%) between +/- 30% and +/- 50%. 

Only one result (1%) was more than 50% lower than the true spiked value. 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation: August 2012

Phase III Statistical Analysis Report    Page 18

Table IV-7 

Mid-Level LCS Results – Toxaphene and Congeners* 

Analyte Number of Observations 

 +/- 10% of 

True Value 

Between +/- 10% 

and +/- 15% of 

True Value 

Between +/- 15% 

and +/- 20% of 

True Value 

> +/- 20% of 

True Value 

Toxaphene 13 (18) 4 (18) 1 (18) 0 (18) 

Hx-Sed 17 (18) 1 (18) 0 (18) 0 (18) 

Hp-Sed 17 (18) 1 (18) 0 (18) 0 (18) 

P26 17 (18) 0 (18) 1 (18) 0 (18) 

P40 15 (18) 3 (18) 0 (18) 0 (18) 

P41 16 (18) 2 (18) 0 (18) 0 (18) 

P44 14 (18) 2 (18) 1 (18) 1 (18) 

P50 16 (18) 0 (18) 2 (18) 0 (18) 

P62 16 (18) 0 (18) 2 (18) 0 (18) 

Total 141(162) 13 (162) 7 (162) 1(162) 

*Total number of individual values is included in parentheses. 

As shown in Table IV-7 and Appendix C-13, and C-15 to C-22, of the 162 individual results for 

the mid-level LCS, 141 (87%) were within +/- 10% of the true spiked value. Thirteen 

measurements (8%) fell between +/- 10% and +/- 15% of the true value, and 7 (4%) between +/- 

15% and +/- 20%. Only one result (1%) was 20% lower than the true spiked value. 

 

Table IV-8 

Spiked Surrogates* 

Analyte Number of Observations 

 +/- 20% of True 

Value 

Between +/- 20% and +/- 

30% of True Value 

> +/- 30% of True 

Value 

PCB 209 52 (54) 2 (54) 0 (54) 

ε-HCH 52 (54) 2 (54) 0 (54) 

Total 104 (108) 4 (108) 0 (108) 

*Total number of individual values is included in parentheses. 

As shown in Table IV-8 and Appendix C-14, of the 108 individual results for the spiked 

surrogates, 104 (96%) were within +/- 20% of the true spiked value. Four measurements (4%) 

fell between +/- 20% and +/- 30% and no results exceeded +/- 30% of the true spiked value. 

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

Phase III Statistical Analysis Report    Page 19

Table IV-9 

MS/MSD Results – Toxaphene, Surrogates and Congeners* 

Analyte Number of Observations 

 +/- 20% of True 

Value 

Between +/- 20% and +/- 

30% of True Value 

> +/- 30% of True Value

Toxaphene 29 (36) 6 (36) 1 (36) 

PCB 209 0 (36) 11 (36) 25 (36) 

ε-HCH 18 (36) 18 (36) 0 (36) 

Hx-Sed 36 (36) 0 (36) 0 (36) 

Hp-Sed 36 (36) 0 (36) 0 (36) 

P26 32 (36) 4 (36) 0 (36) 

P40 32 (36) 4 (36) 0 (36) 

P41 32 (36) 4 (36) 0 (36) 

P44 32 (36) 4 (36) 0 (36) 

P50 32 (36) 4 (36) 0 (36) 

P62 32 (36) 4 (36) 0 (36) 

Total 311 (396) 59 (396) 26 (396) 

*Total number of individual values is included in parentheses. 

As shown in Table IV-9 and Appendix C-23 to C-28, of the 396 individual results for the 

MS/MSDs, 311 (79%) were within +/- 20% of the true value. Fifty-nine measurements (15%) 

fell between +/- 20% and +/- 30% of the true value, and 26 (7%) exceeded +/- 30% of the true 

spiked value. 

Analytical Means Testing 

In order to determine if there are significant differences in mean analyte concentrations 

(toxaphene and associated congeners) between laboratories (specifically among laboratory 

analysts), One-way Analysis of Variance (ANOVA) was performed. Results of the ANOVA 

yield what is termed an F-statistic, as well as an associated p-value. When the associated p-value 

is less than or equal to 0.05, it can be said with 95% confidence that there is a significant 

difference in analytical results between laboratories (and/or analysts). Conversely, when the pvalue is greater than 0.05, no significant difference (at the 95% confidence level) is observed. In 

cases where a significant difference between laboratories was observed, post-hoc Tukey’s 

comparisons were performed to elucidate specific differences in mean concentrations. In the 

tables below, means that do not share a letter in the “Grouping” column are significantly 

different from one another (based on 95% confidence). Results of this analysis are included 

below. Note that as discussed above, there is a significant deviation from normality in the 

distribution of data for three analytes. However, ANOVA is robust against the assumption of 

normality, and therefore is an appropriate test for evaluating differences in mean concentrations 

in this case. 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation: August 2012

Phase III Statistical Analysis Report    Page 20

Toxaphene 

A statistically significant difference was found among laboratory analysts on toxaphene results 

for Fish 1 (F(7,10) = 176.54, p= < 0.001) and Fish 2 (F(7,10) = 151.77, p = < 0.001). Tables IV10 and IV-11 show mean toxaphene concentrations for each laboratory (by analyst) for each fish. 

Means that do not share a letter in the “Grouping” column are significantly different from one 

another (based on 95% confidence). 

Table IV-10 

Means and Standard Deviations Comparing Toxaphene Results between Analysts – Fish 1 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA ORD-LV 2 2 475 7.85 A 

SCCWRP 3 424 1.15 B 

EPA R4 1 3 368 14.2 C 

Ashland 2 355 1.70 CD 

EPA R4 3 2 338 4.07 DE 

EPA R4 2 2 312 3.05 E 

EPA ORD-LV 1 2 275 11.5 F 

EPA NEIC 2 263 1.91 F 

Table IV-11 

Means and Standard Deviations Comparing Toxaphene Results between Analysts – Fish 2 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA ORD-LV 2 2 492 3.96 A 

Ashland 2 327 14.6 B 

EPA NEIC 2 326 1.58 B 

EPA ORD-LV 1 2 324 0.421 B 

SCCWRP 3 314 10.1 B 

EPA R4 1 3 264 12.6 C 

EPA R4 2 2 245 9.13 C 

EPA R4 3 2 245 4.12 C 

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

Phase III Statistical Analysis Report    Page 21

Hx-Sed 

A statistically significant difference was found among laboratory analysts on Hx-Sed results for 

Fish 1 (F(7,10) = 71.35, p = < 0.001) and Fish 2 (F(7,10) = 15.80, p = < 0.001). Tables IV-12 

and IV-13 show mean Hx-Sed concentrations for each laboratory (by analyst) for each fish. 

Means that do not share a letter in the “Grouping” column are significantly different from one 

another (based on 95% confidence). 

Table IV-12 

Means and Standard Deviations Comparing Hx-Sed Results Between Analysts – Fish 1 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 87.9 1.19 A 

Ashland 2 86.6 0.072 AB 

EPA R4 2 2 82.9 0.521 BC 

EPA R4 3 2 80.8 0.421 CD 

SCCWRP 3 80.4 1.74 CD 

EPA NEIC 2 77.8 0.312 D 

EPA ORD-LV 2 2 73.3 0.141 E 

EPA ORD-LV 1 2 72.6 0.642 E 

Table IV-13 

Means and Standard Deviations Comparing Hx-Sed Results Between Analysts – Fish 2 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 61.3 2.88 A 

Ashland 2 60.0 2.90 AB 

EPA R4 2 2 55.6 0.522 ABC 

EPA R4 3 2 53.6 0.322 BCD 

SCCWRP 3 52.5 1.26 CD 

EPA ORD-LV 1 2 51.4 0.571 CD 

EPA NEIC 2 51.4 0.424 CD 

EPA ORD-LV 2 2 48.1 1.04 D 

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

Phase III Statistical Analysis Report    Page 22

Hp-Sed 

A statistically significant difference was found among laboratory analysts on Hp-Sed results for 

Fish 1 (F(7,10) = 14.09, p = < 0.001) and Fish 2 (F(7,10) =8.48, p = < 0.002). Tables IV-14 and 

IV-15 show mean Hp-Sed concentrations for each laboratory (by analyst) for each fish. Means 

that do not share a letter in the “Grouping” column are significantly different from one another 

(based on 95% confidence). 

Table IV-14 

Means and Standard Deviations Comparing Hp-Sed Results Between Analysts – Fish 1 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 99.9 1.27 A 

Ashland 2 97.5 1.13 AB 

SCCWRP 3 94.1 2.69 AB 

EPA R4 3 2 92.2 0.983 ABC 

EPA R4 2 2 92.0 1.07 BC 

EPA NEIC 2 90.2 0.201 BCD 

EPA ORD-LV 2 2 85.0 1.71 CD 

EPA ORD-LV 1 2 83.4 5.30 D 

Table IV-15 

Means and Standard Deviations Comparing Hp-Sed Results Between Analysts – Fish 2 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 85.3 4.54 A 

Ashland 2 81.5 6.22 AB 

SCCWRP 3 76.3 2.15 ABC 

EPA R4 2 2 75.7 0.452 ABC 

EPA R4 3 2 74.5 0.453 BC 

EPA NEIC 2 72.9 1.05 BC 

EPA ORD-LV 1 2 71.9 0.142 BC 

EPA ORD-LV 2 2 66.4 1.84 C 

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

Phase III Statistical Analysis Report    Page 23

P26 

No statistically significant differences were found among laboratory analysts on P26 results for 

Fish 1 (F(7,10) = 2.24, p = 0.12) or Fish 2 (F(7,10) = 1.9, p = 0.17). Tables IV-16 and IV-17 

show P26 mean concentrations for each laboratory (by analyst) for each fish. Note that all 

means are in the same grouping since, based on a 95% confidence level, they are not 

significantly different. 

Table IV-16 

Means and Standard Deviations Comparing P26 Results Between Analysts – Fish 1 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 8.58 0.142 A 

SCCWRP 3 8.47 0.424 A 

EPA ORD-LV 1 2 8.35 0.503 A 

EPA R4 3 2 8.09 0.072 A 

EPA NEIC 2 8.00 0.133 A 

EPA R4 2 2 7.84 0.231 A 

EPA ORD-LV 2 2 7.67 0.840 A 

Ashland 2 7.45 0.504 A 

Table IV-17 

Means and Standard Deviations Comparing P26 Results Between Analysts – Fish 2 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 12.8 0.493 A 

SCCWRP 3 11.8 0.402 A 

EPA NEIC 2 11.8 0.522 A 

EPA R4 2 2 11.5 0.280 A 

EPA R4 3 2 11.4 0.541 A 

EPA ORD-LV 1 2 11.3 0.214 A 

Ashland 2 11.3 1.34 A 

EPA ORD-LV 2 2 11.2 0.662 A 

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

Phase III Statistical Analysis Report    Page 24

P40 

A statistically significant difference was found among laboratory analysts on P40 results for Fish 

1 (F(7,10) = 4.39, p = 0.018) and Fish 2 (F(7,10) =6.69, p = 0.004). Tables IV-18 and IV-19 

show mean P40 concentrations for each laboratory (by analyst) for each fish. Means that do not 

share a letter in the “Grouping” column are significantly different from one another (based on 

95% confidence). 

Table IV-18 

Means and Standard Deviations Comparing P40 Results Between Analysts – Fish 1 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 12.2 0.333 A 

EPA R4 2 2 12.1 0.144 AB 

EPA R4 3 2 11.8 0.051 AB 

EPA NEIC 2 11.7 0.042 AB 

SCCWRP 3 11.3 0.701 AB 

EPA ORD-LV 2 2 10.8 0.742 AB 

EPA ORD-LV 1 2 9.75 1.06 AB 

Ashland 2 9.55 1.49 B 

Table IV-19 

Means and Standard Deviations Comparing P40 Results Between Analysts – Fish 2 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 13.7 0.582 A 

EPA ORD-LV 2 2 13.1 0.152 AB 

EPA NEIC 2 12.8 0.011 AB 

EPA R4 2 2 12.8 0.092 AB 

EPA R4 3 2 12.8 0.153 AB 

SCCWRP 3 12.4 0.481 B 

EPA ORD-LV 1 2 11.7 0.781 B 

Ashland 2 11.6 0.144 B 

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

Phase III Statistical Analysis Report    Page 25

P41 

A statistically significant difference was found among laboratory analysts on P41 results for Fish 

1 (F(7,10) = 4.71, p = 0.014). No significant differences were found among laboratory analysts 

for Fish 2 (F(7,10) =3.2, p = 0.051). Tables IV-20 and IV-21 show mean P41 concentrations for 

each laboratory (by analyst) for each fish. Means that do not share a letter in the “Grouping” 

column are significantly different from one another (based on 95% confidence). Note that for 

Fish 2, all means are in the same grouping since, based on a 95% confidence level, they are not 

significantly different. 

Table IV-20 

Means and Standard Deviations Comparing P41 Results Between Analysts – Fish 1 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 4.71 0.082 A 

SCCWRP 3 4.63 0.231 AB 

EPA ORD-LV 1 2 4.60 0.000 ABC 

EPA NEIC 2 4.56 0.082 ABC 

EPA R4 2 2 4.53 0.062 ABC 

EPA R4 3 2 4.51 0.013 ABC 

Ashland 2 4.25 0.213 BC 

EPA ORD-LV 2 2 4.15 0.044 C 

Table IV-21 

Means and Standard Deviations Comparing P41 Results Between Analysts – Fish 2 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 5.66 0.212 A 

EPA ORD-LV 1 2 5.40 0.141 A 

SCCWRP 3 5.37 0.314 A 

EPA NEIC 2 5.33 0.162 A 

EPA R4 2 2 5.30 0.013 A 

EPA R4 3 2 5.14 0.012 A 

Ashland 2 5.05 0.071 A 

EPA ORD-LV 2 2 5.05 0.064 A 

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

Phase III Statistical Analysis Report    Page 26

P44 

No statistically significant differences were found among laboratory analysts on P44 results for 

Fish 1 (F(7,10) = 3.13, p = 0.05) or Fish 2 (F(7,10) = 1.92, p = 0.17). Tables IV-22 and IV-23 

show mean P44 concentrations for each laboratory (by analyst) for each fish. Note that all 

means are in the same grouping since, based on 95% confidence, they are not significantly 

different. 

Table IV-22 

Means and Standard Deviations Comparing P44 Results Between Analysts – Fish 1 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA NEIC 2 5.28 0.012 A 

EPA R4 1 3 5.16 0.254 A 

SCCWRP 3 4.90 0.101 A 

EPA R4 2 2 4.70 0.340 A 

EPA R4 3 2 4.65 0.042 A 

EPA ORD-LV 1 2 4.55 0.641 A 

EPA ORD-LV 2 2 4.43 0.113 A 

Ashland 2 4.40 0.280 A 

Table IV-23 

Means and Standard Deviations Comparing P44 Results Between Analysts – Fish 2 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

Ashland 2 7.55 1.06 A 

EPA R4 1 3 7.04 0.293 A 

EPA ORD-LV 2 2 6.74 0.383 A 

SCCWRP 3 6.67 0.354 A 

EPA NEIC 2 6.61 0.221 A 

EPA R4 2 2 6.32 0.151 A 

EPA R4 3 2 6.16 0.302 A 

EPA ORD-LV 1 2 5.75 1.20 A 

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

Phase III Statistical Analysis Report    Page 27

P50 

A statistically significant difference was found among laboratory analysts on P50 results for Fish 

1 (F(7,10) = 15.97, p < 0.001) and Fish 2 (F(7,10) =6.50, p = 0.004). Tables IV-24 and IV-25 

show mean P50 concentrations for each laboratory (by analyst) for each fish. Means that do not 

share a letter in the “Grouping” column are significantly different from one another (based on 

95% confidence). 

Table IV-24 

Means and Standard Deviations Comparing P50 Results Between Analysts – Fish 1 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 9.32 0.114 A 

EPA R4 2 2 8.79 0.103 AB 

EPA R4 3 2 8.73 0.124 AB 

SCCWRP 3 8.60 0.363 AB 

EPA NEIC 2 8.50 0.182 AB 

EPA ORD-LV 2 2 8.03 0.221 B 

Ashland 2 7.80 0.571 BC 

EPA ORD-LV 1 2 6.95 0.212 C 

Table IV-25 

Means and Standard Deviations Comparing P50 Results Between Analysts – Fish 2 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

EPA R4 1 3 14.3 0.552 A 

EPA ORD-LV 2 2 13.4 0.143 A 

EPA R4 2 2 13.3 0.000 A 

EPA NEIC 2 13.3 0.301 A 

EPA R4 3 2 13.1 0.214 A 

SCCWRP 3 13.0 0.473 A 

Ashland 2 12.4 0.642 AB 

EPA ORD-LV 1 2 10.7 1.49 B 

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

Phase III Statistical Analysis Report    Page 28

P62 

A statistically significant difference was found among laboratory analysts on P62 results for Fish 

1 (F(6,9) = 8.18, p = 0.003) and Fish 2 (F(6,9) = 6.24, p = 0.005). Tables IV-26 and IV-27 show 

mean P62 concentrations for each laboratory (by analyst) for each fish. Means that do not share 

a letter in the “Grouping” column are significantly different from one another (based on 95% 

confidence). 

Table IV-26 

Means and Standard Deviations Comparing P62 Results Between Analysts – Fish 1 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

SCCWRP 3 16.4 0.903 A 

EPA ORD-LV 1 2 11.0 0.991 AB 

EPA R4 1 3 10.7 0.394 B 

EPA ORD-LV 2 2 9.51 4.48 B 

Ashland 2 8.90 0.281 B 

EPA R4 2 2 8.47 0.493 B 

EPA R4 3 2 8.26 0.253 B 

EPA NEIC * * * * 

*No data reported for this laboratory. 

Table IV-27 

Means and Standard Deviations Comparing P62 Results Between Analysts – Fish 2 

Laboratory (Analyst) Number of 

Observations

Mean Concentration 

(pg/uL) 

Standard 

Deviation 

Grouping 

SCCWRP 3 20.1 3.20 A 

EPA NEIC 2 19.9 2.25 A 

EPA ORD-LV 2 2 17.0 4.56 AB 

EPA ORD-LV 1 2 14.7 2.69 AB 

EPA R4 1 3 14.1 0.473 AB 

EPA R4 3 2 13.1 2.21 AB 

EPA R4 2 2 11.8 1.34 AB 

Ashland 2 7.90 0.00 B 

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

Phase III Statistical Analysis Report    Page 29

Z-Scores – Laboratory Quality Control Samples 

In addition to using modified I-Charts to evaluate laboratory performance during this study, Zscores 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 = 

25% X), yielding the following: 

Z-score = (laboratory analytical result – average recovery) / (25% average recovery) 

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 

Table IV-28 summarizes the Z-scores (based on a 25% X criterion) for each participant and each 

laboratory quality control sample. 
Method 8276 U.S. EPA ORCR Inter‐laboratory Validation: August 2012

Phase III Statistical Analysis Report    Page 30

Table IV-28 

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

Phase III Statistical Analysis Report    Page 31

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 

 

As Table IV-28 indicates, 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. 

Please note that the percent recoveries, as well as the percent relative, percent differences, and 

relative standard deviation values for each laboratory control sample and matrix spike sample for 

all participants can be found in the Draft Phase III Toxaphene Data Tables in Attachment 3 of 

the Analytical Data Report. 

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

Phase III Statistical Analysis Report    Page 32

V. REFERENCES

1. TechLaw Incorporated, “Inter-laboratory Validation for Fish Tissue Study Plan,” 

Submitted to U.S. Environmental Protection Agency, September 2011. 

2. TechLaw Incorporated, “Inter-laboratory Validation for Fish Tissue Analytical Data 

Report,” Submitted to U.S. Environmental Protection Agency, May 2012. 

3. TechLaw Incorporated, “Inter-laboratory Validation for Fish Tissue Data Validation 

Report,” Submitted to U.S. Environmental Protection Agency, May 2012. 

4. International Union of Pure and Applied Chemistry (1993). The International 

Harmonized Protocol for the Proficiency Testing of (Chemical) Analytical Laboratories, Pure & 

Applied Chem., 65 (9), 2123-2144. 
APPENDIX A 

Normality Testing of Technical Toxaphene and Toxaphene Congener Data 

 
Normality Testing - Toxaphene 

250 300 350 400 450

Median

Mean

300 320 340 360 380 400

1st Q uartile 302.81

Median 355.50

3rd Q uartile 423.61

Maximum 480.30

322.50 390.00

311.72 402.94

50.93 101.74

A -Squared 0.32

P-V alue 0.502

Mean 356.25

StDev 67.87

V ariance 4606.10

Skewness 0.296818

Kurtosis -0.779550

N 18

Minimum 261.86

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Toxaphene - Terry Creek

Fish = 1

250 300 350 400 450 500

Median

Mean

250 275 300 325 350

1st Q uartile 250.65

Median 315.45

3rd Q uartile 325.20

Maximum 494.40

277.17 350.17

259.97 324.39

55.08 110.04

A -Squared 1.41

P-V alue < 0.005

Mean 313.67

StDev 73.40

V ariance 5387.40

Skewness 1.59491

Kurtosis 2.52641

N 18

Minimum 238.23

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Toxaphene - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-1 Normality Testing 

7/12/12
200 300 400 500

9

8

7

6

5

4

3

2

1

0

200 300 400 500

1

Toxaphene

Frequency

2

Mean 356.3

StDev 67.87

N 18

1

Mean 313.7

StDev 73.40

N 18

2

Normal 

Panel variable: Fish

Histogram (with Normal Curve) of Toxaphene by Fish - Terry Creek

1 2

500

450

400

350

300

250

200

Fish

Toxaphene

Boxplot of Toxaphene - Terry Creek

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-2 Normality Testing 

7/12/12
Normality Testing - Congeners 

68 72 76 80 84 88 92

Median

Mean

78.0 79.5 81.0 82.5 84.0 85.5

1st Q uartile 76.560

Median 81.185

3rd Q uartile 86.520

Maximum 88.860

78.009 83.418

77.838 84.832

4.081 8.153

A -Squared 0.38

P-V alue 0.370

Mean 80.714

StDev 5.438

V ariance 29.577

Skewness -0.15323

Kurtosis -1.07402

N 18

Minimum 72.100

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener Hx-Sed - Terry Creek

Fish = 1

78.5 83.0 87.5 92.0 96.5 101.0 105.5

Median

Mean

90.0 91.5 93.0 94.5 96.0 97.5

1st Q uartile 89.343

Median 92.145

3rd Q uartile 97.220

Maximum 101.320

89.504 95.238

90.235 96.777

4.327 8.644

A -Squared 0.24

P-V alue 0.734

Mean 92.371

StDev 5.766

V ariance 33.245

Skewness -0.477244

Kurtosis -0.042916

N 18

Minimum 79.600

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener Hp-Sed

Fish = 1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-3 Normality Testing 

7/12/12
7.2 7.6 8.0 8.4 8.8 9.2

Median

Mean

8.0 8.2 8.4 8.6

1st Q uartile 7.8750

Median 8.0650

3rd Q uartile 8.6125

Maximum 8.8000

7.8572 8.3584

7.9466 8.5068

0.3781 0.7555

A -Squared 0.46

P-V alue 0.232

Mean 8.1078

StDev 0.5039

V ariance 0.2539

Skewness -0.616858

Kurtosis 0.135978

N 18

Minimum 7.0700

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congner P26 - Terry Creek

Fish = 1

8 9 10 11 12 13

Median

Mean

10.50 10.75 11.00 11.25 11.50 11.75 12.00

1st Q uartile 10.565

Median 11.700

3rd Q uartile 12.030

Maximum 12.520

10.648 11.753

10.693 11.942

0.834 1.665

A -Squared 0.88

P-V alue 0.019

Mean 11.201

StDev 1.111

V ariance 1.234

Skewness -1.25647

Kurtosis 1.09522

N 18

Minimum 8.500

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P40 - Terry Creek

Fish = 1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-4 Normality Testing 

7/12/12
4.05 4.20 4.35 4.50 4.65 4.80 4.95

Median

Mean

4.40 4.45 4.50 4.55 4.60 4.65

1st Q uartile 4.4600

Median 4.5050

3rd Q uartile 4.6300

Maximum 4.9000

4.4067 4.6177

4.4904 4.6248

0.1592 0.3180

A -Squared 0.67

P-V alue 0.067

Mean 4.5122

StDev 0.2121

V ariance 0.0450

Skewness -0.519048

Kurtosis 0.354174

N 18

Minimum 4.1000

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P41 - Terry Creek

Fish = 1

4.08 4.32 4.56 4.80 5.04 5.28 5.52

Median

Mean

4.5 4.6 4.7 4.8 4.9 5.0

1st Q uartile 4.4975

Median 4.8500

3rd Q uartile 5.0400

Maximum 5.4000

4.6038 4.9728

4.5566 4.9793

0.2784 0.5562

A -Squared 0.18

P-V alue 0.904

Mean 4.7883

StDev 0.3710

V ariance 0.1376

Skewness -0.117458

Kurtosis -0.811090

N 18

Minimum 4.1400

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P44 - Terry Creek

Fish = 1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-5 Normality Testing 

7/12/12
6.6 7.2 7.8 8.4 9.0 9.6

Median

Mean

8.0 8.2 8.4 8.6 8.8

1st Q uartile 8.1025

Median 8.5650

3rd Q uartile 8.8950

Maximum 9.4300

8.0477 8.7734

8.1904 8.8341

0.5475 1.0938

A -Squared 0.41

P-V alue 0.306

Mean 8.4106

StDev 0.7296

V ariance 0.5323

Skewness -0.784967

Kurtosis 0.123521

N 18

Minimum 6.8300

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P50 - Terry Creek

Fish = 1

4.8 7.2 9.6 12.0 14.4 16.8

Median

Mean

9 10 11 12 13

1st Q uartile 8.497

Median 10.275

3rd Q uartile 12.425

Maximum 17.400

9.151 12.530

8.636 11.902

2.342 4.907

A -Squared 0.66

P-V alue 0.071

Mean 10.841

StDev 3.171

V ariance 10.052

Skewness 0.885252

Kurtosis -0.033584

N 16

Minimum 6.340

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P62 - Terry Creek

Fish = 1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-6 Normality Testing 

7/12/12
45 48 51 54 57 60 63

Median

Mean

51 52 53 54 55 56 57

1st Q uartile 51.177

Median 53.540

3rd Q uartile 57.910

Maximum 63.040

52.217 56.813

51.453 56.905

3.467 6.927

A -Squared 0.56

P-V alue 0.128

Mean 54.515

StDev 4.620

V ariance 21.349

Skewness 0.654736

Kurtosis -0.387504

N 18

Minimum 47.400

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener Hx-Sed - Terry Creek

Fish = 2

66 72 78 84 90

Median

Mean

72 74 76 78 80

1st Q uartile 72.105

Median 75.125

3rd Q uartile 78.775

Maximum 88.000

73.057 79.221

72.912 77.707

4.650 9.290

A -Squared 0.59

P-V alue 0.109

Mean 76.139

StDev 6.197

V ariance 38.403

Skewness 0.570807

Kurtosis 0.258507

N 18

Minimum 65.120

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener Hp-Sed

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-7 Normality Testing 

7/12/12
10.35 10.80 11.25 11.70 12.15 12.60 13.05

Median

Mean

11.4 11.6 11.8 12.0 12.2

1st Q uartile 11.243

Median 11.640

3rd Q uartile 12.192

Maximum 13.110

11.332 12.045

11.342 12.159

0.538 1.075

A -Squared 0.24

P-V alue 0.742

Mean 11.689

StDev 0.717

V ariance 0.514

Skewness 0.233200

Kurtosis 0.168740

N 18

Minimum 10.300

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P26 - Terry Creek

Fish = 2

11.1 11.7 12.3 12.9 13.5 14.1

Median

Mean

12.2 12.4 12.6 12.8 13.0

1st Q uartile 12.122

Median 12.825

3rd Q uartile 12.993

Maximum 14.090

12.266 13.036

12.293 12.918

0.581 1.160

A -Squared 0.55

P-V alue 0.136

Mean 12.651

StDev 0.774

V ariance 0.599

Skewness -0.119636

Kurtosis 0.279969

N 18

Minimum 11.100

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P40 - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-8 Normality Testing 

7/12/12
4.8 5.0 5.2 5.4 5.6 5.8

Median

Mean

5.1 5.2 5.3 5.4

1st Q uartile 5.1000

Median 5.2950

3rd Q uartile 5.4600

Maximum 5.7800

5.1888 5.4379

5.1155 5.4296

0.1879 0.3754

A -Squared 0.55

P-V alue 0.131

Mean 5.3133

StDev 0.2504

V ariance 0.0627

Skewness 0.711675

Kurtosis -0.469443

N 18

Minimum 5.0000

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P41 - Terry Creek

Fish = 2

4.8 5.4 6.0 6.6 7.2 7.8 8.4

Median

Mean

6.2 6.4 6.6 6.8 7.0

1st Q uartile 6.3525

Median 6.6250

3rd Q uartile 7.0025

Maximum 8.3000

6.2938 6.9639

6.3959 6.8964

0.5056 1.0100

A -Squared 0.66

P-V alue 0.073

Mean 6.6289

StDev 0.6737

V ariance 0.4539

Skewness -0.09792

Kurtosis 3.41128

N 18

Minimum 4.9000

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P44 - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-9 Normality Testing 

7/12/12
9.0 9.9 10.8 11.7 12.6 13.5 14.4 15.3

Median

Mean

12.50 12.75 13.00 13.25 13.50

1st Q uartile 12.750

Median 13.270

3rd Q uartile 13.505

Maximum 14.710

12.441 13.543

12.800 13.484

0.832 1.662

A -Squared 0.96

P-V alue 0.012

Mean 12.992

StDev 1.108

V ariance 1.229

Skewness -1.57657

Kurtosis 4.37345

N 18

Minimum 9.640

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P50 - Terry Creek

Fish = 2

6 9 12 15 18 21 24

Median

Mean

13 14 15 16 17 18

1st Q uartile 12.445

Median 14.395

3rd Q uartile 18.815

Maximum 23.200

12.905 17.263

12.776 17.547

3.288 6.569

A -Squared 0.26

P-V alue 0.667

Mean 15.084

StDev 4.382

V ariance 19.200

Skewness 0.180205

Kurtosis -0.543473

N 18

Minimum 7.900

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Congener P62 - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-10 Normality Testing 

7/12/12
Normality Testing – Transformed Data 

2.1 2.2 2.3 2.4 2.5 2.6

Median

Mean

2.350 2.375 2.400 2.425 2.450 2.475

1st Q uartile 2.3585

Median 2.4596

3rd Q uartile 2.4874

Maximum 2.5273

2.3588 2.4638

2.3696 2.4801

0.0792 0.1583

A -Squared 1.06

P-V alue 0.007

Mean 2.4113

StDev 0.1056

V ariance 0.0111

Skewness -1.46363

Kurtosis 1.77870

N 18

Minimum 2.1401

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Ln(Congener P40) - Terry Creek

Fish = 1

5.6 5.8 6.0 6.2

Median

Mean

5.55 5.60 5.65 5.70 5.75 5.80 5.85

1st Q uartile 5.5241

Median 5.7540

3rd Q uartile 5.7844

Maximum 6.2033

5.6214 5.8306

5.5600 5.7820

0.1579 0.3154

A -Squared 0.97

P-V alue 0.011

Mean 5.7260

StDev 0.2104

V ariance 0.0443

Skewness 1.07516

Kurtosis 1.20279

N 18

Minimum 5.4732

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Ln(Toxaphene) - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-11 Normality Testing 

7/12/12
2.0 2.2 2.4 2.6

Median

Mean

2.52 2.54 2.56 2.58 2.60 2.62

1st Q uartile 2.5455

Median 2.5855

3rd Q uartile 2.6031

Maximum 2.6885

2.5141 2.6065

2.5494 2.6015

0.0697 0.1392

A -Squared 1.22

P-V alue < 0.005

Mean 2.5603

StDev 0.0929

V ariance 0.0086

Skewness -2.01768

Kurtosis 6.00112

N 18

Minimum 2.2618

A nderson-Darling Normality Test

95% C onfidence Interv al for Mean

95% C onfidence Interv al for Median

95% Confidence Intervals 95% C onfidence Interv al for StDev

Summary for Ln(Congener P50) - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

A-12 Normality Testing 

7/12/12
APPENDIX B 

Results and 3-Sigma Control Limits for Terry Creek Fish Tissue Samples 

 
Results and 3-Sigma Control Limits for Toxaphene – Terry Creek – Fish 1 

Results and 3-Sigma Control Limits for Congeners – Terry Creek – Fish 1 

Laboratory

Replicate

EPA_NERL/ORD_LV_2 (2)

EPA_NERL/ORD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

600

500

400

300

200

100

0

Toxaphene Concentration (pg/uL)

567 (+ 3-sigma)

351 (Grand Mean)

135 (- 3-sigma)

Toxaphene Results and Control Limits - Terry Creek

Fish = 1

Laboratory

Rep

EPA_NERL/ORD_LV_2(2)

EPA_NERL/ORD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

100

80

60

40

20

Hx-Sed Concentration (pg/uL)

0

97.1 (+ 3-sigma)

80.3 (Grand Mean)

63.5 (- 3-sigma)

Hx-Sed Results and Control Limits - Terry Creek

Fish = 1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

B-1 Results and 3-Sigma Control Limits for 

Terry Creek Samples 

7/12/12
Results and 3-Sigma Control Limits for Congeners – Terry Creek – Fish 1 

Laboratory

Rep

EPA_NERL/ORD_LV_2 (2)

EPA_NERL/ORD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

120

100

80

60

40

20

Hp-Sed concentration (pg/uL)

0

109 (+ 3-sigma)

91.8 (Grand Mean)

74.8 (- 3-sigma)

Hp-Sed Results and Control Limits - Terry Creek

Fish = 1

Laboratory

Rep

EPA_NERL/ORD_LV_2 (2)

EPA_NERL/ORD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

9

8

7

6

5

4

3

2

1

0

P26 Concentration (pg/uL)

9.25 (+ 3-sigma)

8.05 (Grand Mean)

6.85 (- 3-sigma)

P26 Results and Control Limits - Terry Creek

Fish = 1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

B-2 Results and 3-Sigma Control Limits for 

Terry Creek Samples 

7/12/12
Results and 3-Sigma Control Limits for Congeners – Terry Creek – Fish 1 

Laboratory

Rep

EPA_NERL/ORD_LV_2 (2)

EPA_NERL/ORD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

14

12

10

8

6

4

2

0

P40 Concentration (pg/uL)

14.1 (+ 3-sigma)

11.1 (Grand Mean)

8.04 (- 3-sigma)

P40 Results and Control Limits - Terry Creek

Fish = 1

Laboratory

Rep

EPA_NERL/ORD_LV_2 (2)

EPA_NERL/ORD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

5

4

3

2

1

0

P41 Concentration (pg/uL)

5.06 (+ 3-sigma)

4.49 (Grand Mean)

3.92 (- 3-sigma)

P41 Results and Control Limits - Terry Creek

Fish = 1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

B-3 Results and 3-Sigma Control Limits for 

Terry Creek Samples 

7/12/12
Results and 3-Sigma Control Limits for Congeners – Terry Creek – Fish 1 

Laboratory

Rep

EPA_NERL/ORD_LV_2(2)

EPA_NERL/ORD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

6

5

4

3

2

1

0

P44 Concentration (pg/uL)

5.75 (+ 3-sigma)

4.76 (Grand Mean)

3.77 (- 3-sigma)

P44 Results and Control Limits - Terry Creek

Fish = 1

Laboratory

Rep

EPA_NERL/ORD_LV_2(2)

EPA_NERL/ORD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

12

10

8

6

4

2

0

P50 Concentration (pg/uL)

10.5 (+ 3-sigma)

8.34 (Grand Mean)

6.15 (- 3-sigma)

P50 Results and Control Limits - Terry Creek

Fish = 1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

B-4 Results and 3-Sigma Control Limits for 

Terry Creek Samples 

7/12/12
Results and 3-Sigma Control Limits for Congeners – Terry Creek – Fish 1 

 

Laboratory

Rep

EPA_NERL/ORD_LV_2(2)

EPA_NERL/ORD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

1

2

3

20

15

10

5

0

P62 Concentration (pg/uL)

18.9 (+ 3-sigma)

2.07 (- 3-sigma)

10.5 (Grand Mean)

P62 Results and Control Limits - Terry Creek

Fish = 1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

B-5 Results and 3-Sigma Control Limits for 

Terry Creek Samples 

7/12/12
Results and 3-Sigma Control Limits for Toxaphene – Terry Creek – Fish 2 

Results and 3-Sigma Control Limits for Congeners – Terry Creek – Fish 2 

Laboratory

Replicate

EPA_NERL/ORD_LV_2 (2)

EPA_NERL/ORD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

123

123

12 3

12 3

12 3

1 23

1 23

1 23

600

500

400

300

200

100

0

Toxaphene Concentration (pg/uL)

554 (+ 3-sigma)

316 (Grand Mean)

78.1 (- 3-sigma)

Toxaphene Results and Control Limits - Terry Creek

Fish = 2

Laboratory

Rep

EPA_NERL/O RD_LV_2 (2)

EPA_NERL/O RD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

123

1 23

123

123

12 3

123

12 3

123

70

60

50

40

30

20

10

Hx-Sed Concentration (pg/uL)

0

67.7 (+ 3-sigma)

40.7 (- 3-sigma)

54.2 (Grand Mean)

Hx-Sed and Control Limits - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

B-6 Results and 3-Sigma Control Limits for 

Terry Creek Samples 

7/12/12
Results and 3-Sigma Control Limits for Congeners – Terry Creek – Fish 2 

Laboratory

Rep

EPA_NERL/O RD_LV_2 (2)

EPA_NERL/O RD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

123

1 23

123

123

12 3

123

12 3

123

90

80

70

60

50

40

30

20

10

Hp-Sed Concentration (pg/uL)

0

93.0 (+ 3-sigma)

58.2 (- 3-sigma)

75.6 (Grand Mean)

Hp-Sed and Control Limits - Terry Creek

Fish = 2

Laboratory

Rep

EPA_NERL/O RD_LV_2 (2)

EPA_NERL/O RD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

123

1 23

123

123

12 3

123

12 3

123

14

12

10

8

6

4

2

0

P26 Concentration (pg/uL)

13.2 (+ 3-sigma)

10.0 (- 3-sigma)

11.6 (Grand Mean)

P26 Results and Control Limits - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

B-7 Results and 3-Sigma Control Limits for 

Terry Creek Samples 

7/12/12
Results and 3-Sigma Control Limits for Congeners – Terry Creek – Fish 2 

Laboratory

Rep

EPA_NERL/O RD_LV_2 (2)

EPA_NERL/O RD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

123

1 23

123

123

12 3

123

12 3

123

16

14

12

10

8

6

4

2

0

P40 Concentration (pg/uL)

14.7 (+ 3-sigma)

12.6 (Grand Mean)

10.5 (- s-sigma)

P40 Results and Control Limits - Terry Creek

Fish = 2

Laboratory

Rep

EPA_NERL/O RD_LV_2 (2)

EPA_NERL/O RD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

123

1 23

123

123

12 3

123

12 3

123

6

5

4

3

2

1

0

P41 Concentration (pg/uL)

5.92 (+ 3-sigma)

5.29 (Grand Mean)

4.66 (- 3-sigma)

P41 Results and Control Limits - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

B-8 Results and 3-Sigma Control Limits for 

Terry Creek Samples 

7/12/12
Results and 3-Sigma Control Limits for Congeners – Terry Creek – Fish 2 

Laboratory

Rep

EPA_NERL/O RD_LV_2 (2)

EPA_NERL/O RD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

123

1 23

123

123

12 3

123

12 3

123

9

8

7

6

5

4

3

2

1

0

P44 Concentration (pg/uL)

8.25 (+ 3-sigma)

6.60 (Grand Mean)

4.95 (- 3-sigma)

P44 Results and Control Limits - Terry Creek

Fish = 2

Laboratory

Rep

EPA_NERL/O RD_LV_2 (2)

EPA_NERL/O RD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

123

1 23

123

123

12 3

123

12 3

123

18

16

14

12

10

8

6

4

2

0

P50 Concentration (pg/uL)

16.1 (+ 3-sigma)

12.9 (Grand Mean)

9.72 (- 3-sigma)

P50 Results and Control Limits - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

B-9 Results and 3-Sigma Control Limits for 

Terry Creek Samples 

7/12/12
Results and 3-Sigma Control Limits for Congeners – Terry Creek – Fish 2 

Laboratory

Rep

EPA_NERL/O RD_LV_2 (2)

EPA_NERL/O RD_LV_1 (2)

SCCWRP

EPA_R4_3

EPA_R4_2

EPA_R4_1

EPA_ NEIC

ASHLAND

123

1 23

123

123

12 3

123

12 3

123

30

25

20

15

10

5

0

P62 Concentration (pg/uL)

2.41 (- 3-sigma)

14.8 (Grand Mean)

27.2 (+ 3-sigma)

P62 Results and Control Limits - Terry Creek

Fish = 2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

B-10 Results and 3-Sigma Control Limits for 

Terry Creek Samples 

7/12/12
Appendix C 

Results and 3-Sigma Control Charts for Quality Control Samples 
Control Chart for Toxaphene – Method Blank 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

1 3 975 1311 1715

25

20

15

10

5

0

Observation

Indi

vid

u

al V

alu

e (pg/

uL)

_

X=3.39

25 pg/uL,

0 pg/uL

I Chart of Toxaphene - Method Blank

50% of LLOQ

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-1 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Control Chart for Congeners – Method Blank 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

1 3 975 11 13 1715

1.0

0.8

0.6

0.4

0.2

0.0

Observation

Indi

vid

u

al V

a

ul e (pg/uL)

_

X=0.042

0.5 pg/uL,

0 pg/uL

1 pg/uL,

I Chart of Hx-Sed - Method Blank

LLOQ

97531 11 13 15 17

1.0

0.8

0.6

0.4

0.2

0.0

Observation

In

d

vi id

u

al V

a

ul e (pg/uL)

_

X=0.035

1 pg/uL,

0.5 pg/uL,

0 pg/uL

I Chart of Hp-Sed - Method Blank

50% of LLOQ

LLOQ

50% of LLOQ

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-2 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Control Chart for Congeners – Method Blank 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

1 3 975 17151311

1.0

0.8

0.6

0.4

0.2

0.0

Observation

Indi

vid

u

al V

alu

e (pg/uL)

_

X=0.092

0.5 pg/uL,

0 pg/uL

1 pg/uL,

I Chart of P26 - Method Blank

50% of LLOQ

1 3 975 17151311

1.0

0.8

0.6

0.4

0.2

0.0

Observation

In

divid

u

al V

alu

e (pg/uL)

_

X=0.066

0.5 pg/uL,

0 pg/uL

1 pg/uL,

I Chart of P40 - Method Blank

50% of LLOQ

LLOQ

LLOQ

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-3 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Control Chart for Congeners – Method Blank 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

1 3 975 151311 17

1.0

0.8

0.6

0.4

0.2

0.0

Observation

Indi

vid

u

al V

alu

e (pg/uL)

_

X=0.073

0.5 pg/uL,

0 pg/uL

1 pg/uL,

I Chart of P41 - Method Blank

50% of LLOQ

LLOQ

1 3 975 151311 17

1.0

0.8

0.6

0.4

0.2

0.0

Observation

Indi

vid

u

al V

alu

e (pg/uL)

_

X=0.101

0.5 pg/uL,

0 pg/uL

1 pg/uL,

I Chart of P44 - Method Blank

50% of LLOQ

LLOQ

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-4 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Control Chart for Congeners – Method Blank 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

1 3 975 11 13 1715

1.0

0.8

0.6

0.4

0.2

0.0

Observation

Indi

vid

u

al V

a

ul e (pg/uL)

_

X=0.074

0.5 pg/uL,

0 pg/uL

1 pg/uL,

I Chart of P50 - Method Blank

50% of LLOQ

LLOQ

1 9753 11 13 15 17

5

4

3

2

1

0

Observation

In

d

vi id

u

al V

a

ul e (pg/uL)

_

X=0.161

2.5 pg/uL,

0 pg/uL

5 pg/uL,

I Chart of P62 - Method Blank

50% of LLOQ

LLOQ

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-5 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation	

Source	Fish	Control	Charts	

Phase III Statistical Analysis Report Page	1	

Control Chart for Toxaphene – Source Fish 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

31 975 11 13 15 17

50

40

30

20

10

0

Observation

In

d

vi di u

al V

alu

e (p

g/uL)

_

X=16.54

50 pg/uL,

0 pg/uL

25 pg/uL,

I Chart of Toxaphene - Source Fish

50% of LLOQ

LLOQ

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-6 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation	

Source	Fish	Control	Charts	

Phase III Statistical Analysis Report Page	2	

Control Chart for Congeners – Source Fish 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

1 3 975 17151311

1.0

0.8

0.6

0.4

0.2

0.0

Observation

Indi

vid

u

al V

alu

e (pg/

uL)

_

X=0.043

1 pg/uL,

0.5 pg/uL,

0 pg/uL

I Chart of Hx-Sed - Source Fish

50% of LLOQ

LLOQ

1 3 975 17151311

1.0

0.8

0.6

0.4

0.2

0.0

Observation

In

divid

u

al V

alu

e (pg/uL)

_

X=0.039

1 pg/uL,

0.5 pg/uL,

0 pg/uL

I Chart of Hp Sed - Source Fish

50% of LLOQ

LLOQ

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-7 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation	

Source	Fish	Control	Charts	

Phase III Statistical Analysis Report Page	3	

Control Chart for Congeners – Source Fish 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

1 9753 17151311

1.4

1.2

1.0

0.8

0.6

0.4

0.2

0.0

Observation

Indi

vid

u

al V

alu

e (pg/uL)

_

X=0.217

1 pg/uL,

0.5 pg/uL,

0 pg/uL

I Chart of P26 - Source Fish

50% of LLOQ

LLOQ

1 9753 17151311

1.0

0.8

0.6

0.4

0.2

0.0

Observation

In

d

vi id

u

al V

alu

e (pg/uL)

_

X=0.07

1 pg/uL,

0.5 pg/uL,

0 pg/uL

I Chart of P40 - Source Fish

50% of LLOQ

LLOQ

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-8 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation	

Source	Fish	Control	Charts	

Phase III Statistical Analysis Report Page	4	

Control Chart for Congeners – Source Fish 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

1 3 975 151311 17

1.0

0.8

0.6

0.4

0.2

0.0

Observation

Indi

vid

u

al V

alu

e (pg/uL)

_

X=0.098

1 pg/uL,

0.5 pg/uL,

0 pg/uL

I Chart of P41 - Source Fish

50% of LLOQ

LLOQ

1 3 975 151311 17

1.0

0.8

0.6

0.4

0.2

0.0

Observation

Indi

vid

u

al V

alu

e (pg/uL)

_

X=0.12

1 pg/uL,

0.5 pg/uL,

0 pg/uL

I Chart of P44 - Source Fish

50% of LLOQ

LLOQ

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-9 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation	

Source	Fish	Control	Charts	

Phase III Statistical Analysis Report Page	5	

Control Chart for Congeners – Source Fish 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

Notes: Non-detects and results reported as “<” are indicated as “0” on the chart. 

1 3 975 17151311

1.0

0.8

0.6

0.4

0.2

0.0

Observation

Indi

vid

u

al V

alu

e (pg/uL)

_

X=0.201

1 pg/uL,

0.5 pg/uL,

0 pg/uL

I Chart of P50 - Source Fish

50% of LLOQ

LLOQ

1 3 975 11 13 15 17

5

4

3

2

1

0

Observation

In

d

vi id

u

al V

a

ul e (pg/uL)

5 pg/uL,

2.5 pg/uL,

0 pg/uL

_

X=0.173

I Chart of P62 - Source Fish

50% of LLOQ

LLOQ

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-10 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Control Charts for Toxaphene and Surrogates – Second Source Standard (Toxaphene spiked at 150 

pg/uL; PCB209, 100 pg/uL; and eHCH, 250 pg/uL ) 

97531 17151311

200

180

160

140

120

100

Observation

Individual Value (pg/uL)

_

X=159.5

195 (+30%)

120 (-20%)

180 (+20%)

150 - True Value

105 (-30%)

I Chart of Toxaphene - Second Source Standard

97531 17151311

130

120

110

100

90

80

70

Observation

Individual Value (pg/uL)

_

X=109.29

130 (+30%)

80 (-20%)

120 (+20%)

100 - True Value

70 (-30%)

I Chart of PCB209 - Second Source Standard

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-11 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Control Charts for Toxaphene and Surrogates – Second Source Standard (Toxaphene spiked at 150 

pg/uL; PCB209, 100 pg/uL; and eHCH, 250 pg/uL ) 

97531 11 13 1715

340

320

300

280

260

240

220

200

180

160

Observation

Individual Value (pg/uL)

_

X=263.7

325 (+30%)

200 (-20%)

300 (+20%)

250 - True Value

175 (-30%)

I Chart of eHCH - Second Source Standard

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-12 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		

LCS	Control	Charts		

Phase III Statistical Analysis Report Page	1	

Control Charts for Toxaphene – LCS-1 (Low-50 pg/uL, at LLOQ) and LCS-2 (Mid-200 pg/uL) 

97531 1311 1715

80

70

60

50

40

30

20

Observation

Individual Value (pg/uL)

_

X=56.74

75 (+50%)

65 (+30%)

60 (+20%)

25 (-50%)

35 (-30%)

40 (-20%)

50 - True Value

I Chart of Toxaphene - LCS-1 

97531 17151311

240

230

220

210

200

190

180

170

160

150

Observation

Individual Value (pg/uL)

_

X=208.66

160 (-20%)

170 (-15%)

180 (-10%)

240 (+20%)

230 (+15%)

220 (+10%)

200 - True Value

I Chart of Toxaphene - LCS-2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-13 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		

LCS	Control	Charts		

Phase III Statistical Analysis Report Page	2	

Control Charts for Spiked Surrogates – PCB209 (100 pg/uL) and eHCH (250 pg/uL) 

61 4641363126211611 51

130

120

110

100

90

80

70

Observation

Individual Value (pg/uL)

_

X=96.07

130 (+30%)

120 (+20%)

100 - True Value

80 (-20%)

70 (-30%)

I Chart of PCB209 - Spiked Surrogate

61 4641363126211611 51

340

320

300

280

260

240

220

200

180

160

Observation

Individual Value (pg/uL)

_

X=238.8

325 (+30%)

300 (+20%)

200 (-20%)

250 - True Value

175 (-30%)

I Chart of eHCH - Spiked Surrogate

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-14 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		

LCS	Control	Charts		

Phase III Statistical Analysis Report Page	3	

Control Charts for Congeners – LCS-1 (Mid-100 pg/uL for all, except 226 pg/uL for P62) 

97531 11 13 1715

120

110

100

90

80

Observation

Individual Value (pg/uL)

_

X=98.77

120 (+20%)

115 (+15%)

85 (-15%)

110 (+10%)

90 (-10%)

100 - True Value

80 (-20%)

I Chart of Hx-Sed - LCS-1

97531 11 13 1715

120

110

100

90

80

Observation

Individual Value (pg/uL)

_

X=99.46

120 (+20%)

80 (-20%)

115 (+15%)

85 (-15%)

110 (+10%)

90 (-10%)

100 - True Value

I Chart of Hp-Sed - LCS-1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-15 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		

LCS	Control	Charts		

Phase III Statistical Analysis Report Page	4	

Control Charts for Congners – LCS-1 (Mid-100 pg/uL for all, except 226 pg/uL for P62)

97531 151311 17

120

110

100

90

80

Observation

Individual Value (pg/uL)

_

X=98.40

120 (+20%)

80 (-20%)

115 (+15%)

85 (-15%)

110 (+10%)

90 (-10%)

100 - True Value

I Chart of P26 - LCS-1

97531 151311 17

120

110

100

90

80

Observation

Individual Value (pg/uL)

_

X=98.65

120 (+20%)

80 (-20%)

115 (+15%)

85 (-15%)

110 (+10%)

90 (-10%)

100 - True Value

I Chart of P40 - LCS-1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-16 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		

LCS	Control	Charts		

Phase III Statistical Analysis Report Page	5	

Control Charts for Congners – LCS-1 (Mid-100 pg/uL for all, except 226 pg/uL for P62)

97531 11 13 1715

120

110

100

90

80

Observation

Individual Value (pg/uL)

_

X=99.20

120 (+20%)

115 (+15%)

85 (-15%)

110 (+10%)

90 (-10%)

100 - True Value

80 (-20%)

I Chart of P41 - LCS-1

97531 11 13 1715

120

110

100

90

80

Observation

Individual Value (pg/uL)

_

X=100.17

120 (+20%)

115 (+15%)

85 (-15%)

110 (+10%)

90 (-10%)

100 - True Value

80 (-20%)

I Chart of P44 - LCS-1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-17 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		

LCS	Control	Charts		

Phase III Statistical Analysis Report Page	6	

Control Charts for Congners – LCS-1 (Mid-100 pg/uL for all, except 226 pg/uL for P62)

97531 11 13 1715

120

110

100

90

80

Observation

Individual (pg/uL)

_

X=97.66

120 (+20%)

115 (+15%)

85 (-15%)

110 (+10%)

90 (-10%)

100 - True Value

80 (-20%)

I Chart of P50 - LCS-1

97531 11 13 1715

280

260

240

220

200

180

Observation

Individual Value (pg/uL)

_

X=239.4

271.2 (+20%)

192.1 (-15%)

259.9 (+15%)

203.4 (-10%)

248.6 (+10%)

226 - True Value

180.8 (-20%)

I Chart of P62 - LCS-1

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-18 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		

LCS	Control	Charts		

Phase III Statistical Analysis Report Page	7	

Control Charts for Congners – LCS-2 (Low-2 pg/uL for all, except 22.6 pg/uL for P62)

97531 17151311

3.0

2.5

2.0

1.5

1.0

Observation

Individual Value (pg/uL)

_

X=1.955

3 (+50%)

1.4 (-30%)

2.6 (+30%)

1.6 (-20%)

2.4 (+20%)

2 - True Value

1 (-50%)

I Chart of Hx-Sed - LCS-2

97531 17151311

3.0

2.5

2.0

1.5

1.0

Observation

Individual Value (pg/uL)

_

X=1.989

3 (+50%)

1 (-50%)

1.4 (-30%)

2.6 (+30%)

1.6 (-20%)

2.4 (+20%)

2 - True Value

I Chart of Hp-Sed - LCS-2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-19 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		

LCS	Control	Charts		

Phase III Statistical Analysis Report Page	8	

Control Charts for Congners – LCS-2 (Low-2 pg/uL for all, except 22.6 pg/uL for P62)

97531 11 13 15 17

3.0

2.5

2.0

1.5

1.0

Observation

Individual Value (pg/uL)

_

X=1.844

3 (+50%)

1 (-50%)

1.4 (-30%)

2.6 (+30%)

1.6 (-20%)

2.4 (+20%)

2 - True Value

I Chart of P26 - LCS-2

97531 11 13 15 17

3.0

2.5

2.0

1.5

1.0

Observation

Individual Value (pg/uL)

_

X=1.948

3 (+50%)

1.4 (-30%)

2.6 (+30%)

1.6 (-20%)

2.4 (+20%)

2 - True Value

1 (-50%)

I Chart of P40 - LCS-2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-20 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		

LCS	Control	Charts		

Phase III Statistical Analysis Report Page	9	

Control Charts for Congners – LCS-2 (Low-2 pg/uL for all, except 22.6 pg/uL for P62)

97531 11 13 15 17

3.0

2.5

2.0

1.5

1.0

Observation

Individual Value (pg/uL)

_

X=2.031

3 (+50%)

1.4 (-30%)

2.6 (+30%)

1.6 (-20%)

2.4 (+20%)

2 - True Value

1 (-50%)

I Chart of P41 - LCS-2

97531 11 13 15 17

3.0

2.5

2.0

1.5

1.0

Observation

Individual Value (pg/uL)

_

X=2.003

3 (+50%)

1.4 (-30%)

2.6 (+30%)

1.6 (-20%)

2.4 (+20%)

2 - True Value

1 (-50%)

I Chart of P44 - LCS-2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-21 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:		

LCS	Control	Charts		

Phase III Statistical Analysis Report Page	10	

Control Charts for Congners – LCS-2 (Low-2 pg/uL for all, except 22.6 pg/uL for P62)

97531 11 13 15 17

3.0

2.5

2.0

1.5

1.0

Observation

Individual Value (pg/uL)

_

X=2.014

3 (+50%)

1.4 (-30%)

2.6 (+30%)

1.6 (-20%)

2.4 (+20%)

2 - True Value

1 (-50%)

I Chart of P50 - LCS-2

97531 11 13 1715

35

30

25

20

15

10

Observation

Individual Value (pg/uL)

_

X=21.16

33.9 (+50%)

15.82 (-30%)

29.38 (+30%)

18.08 (-20%)

27.12 (+20%)

22.6 - True Value

11.3 (-50%)

I Chart of P62 - LCS-2

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-22 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:	

Matrix	Spikes	Control	Charts	

Phase III Statistical Analysis Report

Page	1	

Control Charts for Toxaphene and Surrogates– MS/MSD (Toxaphene spiked at 200 pg/uL; PCB20, 

100 pg/uL; and eHCH, 250 pg/uL) 

951 1713 21 25 3329

275

250

225

200

175

150

Observation

Individual Value (pg/uL)

_

X=185.7

260 (+30%)

160 (-20%)

240 (+20%)

200 - True Value

140 (-30%)

I Chart of Toxaphene - MS/MSD

951 1713 21 25 3329

130

120

110

100

90

80

70

60

50

Observation

Individual Value (pg/uL)

_

X=68.29

130 (+30%)

80 (-20%)

120 (+20%)

100 - True Value

70 (-30%)

I Chart of PCB209 - MS/MSD

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-23 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:	

Matrix	Spikes	Control	Charts	

Phase III Statistical Analysis Report

Page	2	

Control Charts for Toxaphene and Surrogates– MS/MSD (Toxaphene spiked at 200 pg/uL; PCB20, 

100 pg/uL; and eHCH, 250 pg/uL) 

951 2925211713 33

340

320

300

280

260

240

220

200

180

160

Observation

Individual Value (pg/uL)

_

X=201.4

325 (+30%)

200 (-20%)

300 (+20%)

250 - True Value

175 (-30%)

I Chart of eHCH - MS/MSD

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-24 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:	

Matrix	Spikes	Control	Charts	

Phase III Statistical Analysis Report

Page	3	

Control Charts for Congeners – MS/MSD (All congeners spiked at 100 pg/uL, except for P62 which is 

spiked at 226 pg/uL)

951 2925211713 33

130

120

110

100

90

80

70

Observation

Individual Value (pg/uL)

_

X=91.61

130 (+30%)

80 (-20%)

120 (+20%)

100 - True Value

70 (-30%)

I Chart of Hx-Sed - MS/MSD

951 2925211713 33

130

120

110

100

90

80

70

Observation

Individual Value (pg/uL)

_

X=90.93

130 (+30%)

80 (-20%)

120 (+20%)

100 - True Value

70 (-30%)

I Chart of Hp-Sed - MS/MSD

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-25 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:	

Matrix	Spikes	Control	Charts	

Phase III Statistical Analysis Report

Page	4	

Control Charts for Congeners – MS/MSD (All congeners spiked at 100 pg/uL, except for P62 which is 

spiked at 226 pg/uL) 

951 2925211713 33

130

120

110

100

90

80

70

Observation

Individual Value (pg/uL)

_

X=90.80

130 (+30%)

80 (-20%)

120 (+20%)

100 - True Value

70 (-30%)

I Chart of P40 - MS/MSD

1 5 9 332925211713

130

120

110

100

90

80

70

Observation

In

d

vi id

ual

Val

u

e (pg/uL)

_

X=86.22

130 (+30%)

80 (-20%)

120 (+20%)

100 - True Value

70 (-30%)

I Chart of P26 - MS/MSD

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-26 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:	

Matrix	Spikes	Control	Charts	

Phase III Statistical Analysis Report

Page	5	

Control Charts for Congeners – MS/MSD (All congeners spiked at 100 pg/uL, except for P62 which is 

spiked at 226 pg/uL) 

951 2925211713 33

130

120

110

100

90

80

70

Observation

Individual Value (pg/uL)

_

X=90.48

130 (+30%)

80 (-20%)

120 (+20%)

100 - True Value

70 (-30%)

I Chart of P41 - MS/MSD

951 332925211713

130

120

110

100

90

80

70

Observation

Individual Value (pg/uL)

_

X=94.18

130 (+30%)

80 (-20%)

120 (+20%)

100 - True Value

70 (-30%)

I Chart of P44 - MS/MSD

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-27 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12
Method	8276	U.S.	EPA	ORCR	Inter‐laboratory	Validation:	

Matrix	Spikes	Control	Charts	

Phase III Statistical Analysis Report

Page	6	

Control Charts for Congeners – MS/MSD (All congeners spiked at 100 pg/uL, except for P62 which is 

spiked at 226 pg/uL) 

951 332925211713

130

120

110

100

90

80

70

Observation

Individual Value (pg/uL)

_

X=88.29

130 (+30%)

80 (-20%)

120 (+20%)

100 - True Value

70 (-30%)

I Chart of P50 - MS/MSD

951 332925211713

300

275

250

225

200

175

150

Observation

Individual Value (pg/uL)

_

X=224.6

158.2 (-30%)

293.8 (+30%)

180.8 (-20%)

271.2 (+20%)

226 - True Value

I Chart of P62 - MS/MSD

Method 8276 U.S. EPA ORCR Inter-Laboratory Validation 

Phase III Statistical Analysis Report 

C-28 Results and 3-Sigma Control Charts for 

Quality Control Samples 

7/12/12