NISTIR 7230 

NIST Intercomparison Exercise 

Program for Organic Contaminants in 

the Marine Environment: 

Description and Results of 2003 Organic 

Intercomparison Exercises 

Michele M. Schantz 

John R. Kucklick 

Reenie M. Parris 

Dianne L. Poster 

Stephen A. Wise 
 

NISTIR 7230 

NIST Intercomparison Program for 

Organic Contaminants in the 

Marine Environment: 

Description and Results of 2003 

Organic Intercomparison Exercises 

Michele M. Schantz, John R. Kucklick,1

 Reenie M. Parris, Dianne L. Poster 

 and Stephen A. Wise 

Analytical Chemistry Division 

National Institute of Standards and Technology 

Gaithersburg, MD 20899-8392 and 

1

Charleston, SC 29412 

 

May 2005 

U.S. DEPARTMENT OF COMMERCE

Carlos M. Gutierrez, Secretary

TECHNOLOGY ADMINISTRATION

Phillip J. Bond, Under Secretary of Commerce for Technology

NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY

Hratch G. Semerjian, Acting Director
 

Table of Contents

Abstract............................................................................................................................................1 

Introduction......................................................................................................................................2 

Sources and Preparation of Materials Used in 2003 Intercomparison Exercises ............................3 

Storage and Distribution of Materials..............................................................................................4 

Evaluation of Exercise Results ........................................................................................................4 

Establishment of the Assigned Values.................................................................................4 

Reported Results ..............................................................................................................................6 

Performance Scores .........................................................................................................................6 

Accuracy Assessment (z-score) ...........................................................................................7 

Precision Assessment (p-score) ...........................................................................................8 

Discussion........................................................................................................................................8 

Acknowledgments..........................................................................................................................13 

Disclaimer and References ............................................................................................................13 

Tables.............................................................................................................................................16 

Table 1. Target analytes in NIST Intercomparison Exercise Program for 

Organic Contaminants in the Marine Environment ...............................................17 

Table 2. Mussel Tissue XI (QA03TIS11): Laboratory means of three replicates and 

exercise assigned values - Water, TEO, and PAHs................................................19 

Table 3. Mussel Tissue XI (QA03TIS11): Laboratory means of three replicates and 

exercise assigned values - Pesticides......................................................................20 

Table 4. Mussel Tissue XI (QA03TIS11): Laboratory means of three replicates 

and exercise assigned values - PCBs......................................................................21 

Table 5. SRM 1974b: Laboratory means of three replicates 

and target values - Water, TEO, and PAHs............................................................22 
 

Table 6. SRM 1974b: Laboratory means of three replicates 

and target values - Pesticides..................................................................................23 

Table 7. SRM 1974b: Laboratory means of three replicates 

and target values - PCBs ........................................................................................24 

Table 8. Marine Sediment XII (QA03SED12): Laboratory means of three replicates and 

exercise assigned values - Water, TOC, and PAHs ...............................................25 

Table 9. Marine Sediment XII (QA03SED12): Laboratory means of three replicates and 

exercise assigned values - Pesticides......................................................................26 

Table 10. Marine Sediment XII (QA03SED12): Laboratory means of three replicates 

and exercise assigned values - PCBs......................................................................27 

Table 11. SRM 1941b: Laboratory means of three replicates 

and target values - Water, TOC, and PAHs ...........................................................28 

Table 12. SRM 1941b: Laboratory means of three replicates 

and target values - Pesticides..................................................................................29 

Table 13. SRM 1941b: Laboratory means of three replicates 

and target values - PCBs ........................................................................................30 

Table 14. Mussel Tissue XI (QA03TIS11): z-scores (25 %) by laboratory - PAHs 

and Water ...............................................................................................................31 

Table 15. Mussel Tissue XI (QA03TIS11): z-scores (25 %) by laboratory - Pesticides .......32 

Table 16. Mussel Tissue XI (QA03TIS11): z-scores (25 %) by laboratory - PCBs ..............33 

Table 17. Marine Sediment XII (QA03SED12): z-scores (25 %) by laboratory - PAHs, 

Water, and TOC .....................................................................................................34 

Table 18. Marine Sediment XII (QA03SED12): z-scores (25 %) by laboratory - Pesticides35 

Table 19. Marine Sediment XII (QA03SED12): z-scores (25 %) by laboratory - PCBs.......36 

Table 20. p-scores (15 %) for water, TEO, and PAHs in Mussel Tissue XI and 

SRM 1974b.............................................................................................................37 

Table 21. p-scores (15 %) for pesticides in Mussel Tissue XI and SRM 1974b....................39 
 

Table 22. p-scores (15 %) for PCBs in Mussel Tissue XI and SRM 1974b ..........................41 

Table 23. p-scores (15 %) for water, TOC, and PAHs in Marine Sediment XII and 

SRM 1941b.............................................................................................................43 

Table 24. p-scores (15 %) for pesticides in Marine Sediment XII and SRM 1941b..............46 

Table 25. p-scores (15 %) for PCBs in Marine Sediment XII and SRM 1941b ....................49 

Table 26. Comparison to previous exercise assigned values for PAHs (ng/g dry-mass basis)52 

Table 27. Comparison to previous exercise assigned values for pesticides (ng/g dry-mass 

basis).......................................................................................................................53

Table 28. Comparison to previous exercise assigned values for PCBs (ng/g dry-mass basis) 

and water (%) .........................................................................................................54 
 

Appendices

Appendix A: Description, Storage, Use, and Reporting Instructions 

 for Mussel Tissue XI (QA03TIS11) ...........................................................................................55 

Appendix B: Description, Storage, Use, and Reporting Instructions 

 for Marine Sediment XII (QA03SED12)....................................................................................70 

Appendix C: Laboratory Notes Accompanying Data, Mussel Tissue XI.....................................79 

Appendix D: Laboratory Notes Accompanying Data, Marine Sediment XII ..............................82 

Appendix E: Laboratory Methods Used, Mussel Tissue XI.........................................................85 

Appendix F: Laboratory Methods Used, Marine Sediment XII ...................................................92 

Appendix G: Charts of Mussel Tissue XI and SRM 1974b, Results by Analyte .........................99 

Appendix H: Charts of Marine Sediment XII and SRM 1941b, Results by Analyte .................157 

Appendix I: List of Laboratories Participating in 2003 Intercomparison Exercises ...................223 
 

 

Abstract

In support of marine monitoring measurement programs, the National Institute of Standards and 

Technology (NIST) conducts yearly interlaboratory comparison exercises to provide one 

mechanism for participating laboratories/monitoring programs to evaluate the quality and 

comparability of their performance in measuring selected organic contaminants in environmental 

samples. In this report, results of the 2003 exercises of the NIST Intercomparison Exercise 

Program for Organic Contaminants in the Marine Environment are described in which selected 

polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyl (PCB) congeners, and 

chlorinated pesticides were determined in Mussel Tissue XI and Marine Sediment XII exercise 

materials. The analytical methods used by each participating laboratory in this performancebased program are also summarized. 
 

Introduction

The preparation and distribution of two materials, Mussel Tissue XI (QA03TIS11) and Marine 

Sediment XII (QA03SED12), used in interlaboratory comparison exercises in 2003 for the 

National Institute of Standards and Technology (NIST) Intercomparison Exercise Program for 

Organic Contaminants in the Marine Environment and the results of these exercises are 

described in this report. The analytical methods used by each participating laboratory are also 

summarized. 

Tools and mechanisms for the assessment of data produced by laboratories providing 

environmental analyses are critical because decision-making based on inaccurate results or data 

of unknown quality can have significant economic and health consequences. NIST provides a 

variety of activities in support of environmental monitoring programs for organic contaminants. 

The largest of these programs was initiated and funded in part for 12 years (until 1999) by the 

National Oceanic and Atmospheric Administration (NOAA) National Status and Trends (NS&T) 

Marine Monitoring Program [1,2,3]. The Environmental Protection Agency (EPA) 

Environmental Monitoring and Assessment Program (EMAP) also participated in the 

NIST/NOAA NS&T effort for a number of years. Private sector and other laboratories that 

could not be accommodated under the NOAA, EPA, and NIST funding have reimbursed NIST 

for participation costs and have participated in these exercises and workshops as part of the NIST 

Intercomparison Exercise Program for Organic Contaminants in the Marine Environment. NIST 

is now continuing this program on a pay-to-participate basis. Through this program, NIST 

provides mechanisms for assessing the interlaboratory and temporal comparability of data with 

the goal of improving measurements for the monitoring of organic contaminants such as 

polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyl (PCB) congeners, and 

chlorinated pesticides in bivalve, sediment, and fish samples. This program includes the 

development of improved analytical methods, production of needed NIST Standard Reference 

Materials (SRMs) and other control materials, conduct of annual interlaboratory comparison 

exercises, and the coordination of workshops to discuss the results of these exercises and to 

provide a forum for cooperative problem-solving efforts by participants. Current participants 

represent multi-laboratory monitoring programs as well as a number of individual programs, and 

include federal, state/municipal, university/college, private sector, and international laboratories. 

In this performance-based program, each participating laboratory uses its current methods for 

analysis of similar materials for its program customers. 

For the annual intercomparison exercises, samples of two natural-matrix, homogeneous materials 

that are derived from the marine environment and that have not been fortified with any of the 

target analytes are analyzed by the participating laboratories. Typical materials, such as mussel 

or fish tissue homogenates or wetted marine sediment, have levels of target analytes in the 1 ng/g 

to 15000 ng/g range. The target analytes are listed in Table 1. 

Numerical indices, z- and p-scores, are used to assess and track laboratory performance for 

accuracy and precision, respectively, and to provide a mechanism for assessing the comparability 
 

of data being produced by the participating laboratories for over 75 target analytes, total organic 

carbon (TOC), percent total extractable organics (TEO), and percent moisture. 

Sources and Preparation of Materials used in 2003 Intercomparison Exercises 

Mussel Tissue XI. Mussel Tissue XI was the same material as Mussel Tissue IX (QA98TIS9) 

used as the 1998 exercise material [4] and Mussel Tissue IV (QA92TIS4) used as the 1992 

exercise material [3]. This sample is a cryogenically homogenized “fresh” material prepared 

from mussels collected in Boston Harbor in February 1992. Colorless, 2-oz, wide-mouth, glass 

bottles were rinsed with deionized water, thermally cleaned at 450 °C for 12 h in a ventilated 

oven, cooled, capped, and labeled. Each label contained the material's name and code (Mussel 

Tissue XI, QA03TIS11) as well as an individual bottle number. The Teflon liners of the 

phenolic screw caps had been removed from the caps, cleaned with hexane, dried, and reinserted 

in the caps. The bottles of Mussel Tissue IV were emptied into new precleaned, prelabeled 

(Mussel Tissue XI, QA03TIS11 with individual bottle numbers), precooled (-80 °C) bottles. 

This sample is a cryogenically homogenized “fresh” material prepared from mussels collected in 

Boston Harbor in February 1992. 

Each of the three bottles sent to each participant contained approximately 17 g (wet-mass basis) 

of Mussel Tissue XI. This frozen mussel tissue homogenate material had not been enriched or 

spiked. 

Marine Sediment XII. Marine Sediment XII was prepared from Certified Reference Material 

(CRM) PACS-2 (Marine Sediment Reference Material for Trace Elements and Other 

Constituents, National Research Council Canada), a marine sediment that was collected from 

Esquimalt Harbor in British Columbia and has been freeze-dried, passed through a No. 120 (125 

μm) screen, blended, bottled, and radiation sterilized (2.5 mrad). PACS-2 was also used to 

prepare the sediment used in the 1998 exercise (Marine Sediment VIII, QA98SED8) [4]. The 

sediment material was issued as a wet sediment to more closely match the matrix of wet 

sediments routinely analyzed by the laboratories. 

Colorless, 2-oz, wide-mouth, glass bottles were rinsed with deionized water, thermally cleaned at 

450 °C for 12 h in a ventilated oven, cooled, capped, and labeled. Each label contained the 

material's name and code (Marine Sediment XII, QA03SED12) as well as an individual bottle 

number. The Teflon liners of the phenolic screw caps had been removed from the caps, cleaned 

with hexane, dried, and reinserted in the caps. A calibrated toploader balance (resolution of 0.01 

g) was used for weighing the PACS-2 sediment and water. For each sample, 11.00 g of PACS-2 

sediment (as received) was weighed into a tared bottle. The bottle was then capped and stored in 

the dark at room temperature. Approximately four days before samples were to be shipped to 

laboratories participating in the intercomparison exercise, 9.0 g of HPLC-grade water were 

added by pipet to each tared bottle of sediment. (Preliminary trials had shown that a minimum of 

9 g of water would moisten 11 g of this sediment.) The mass of sediment and water in each 

bottle were recorded. Each sample was tilted by hand until no dry sediment was visible. Only a 
 

very small amount of water was observed on the top of the wet sediment. After 24 h at room 

temperature (in the dark), followed by approximately 4 h at -20 °C, each bottle of material was 

stored at -80 °C until shipped. The bottles were never inverted until the wet samples had been 

frozen in the bottom of the bottles. The material was not enriched or spiked with any of the 

analytes of interest in this intercomparison exercise. 

Storage and Distribution of Materials

Each bottle of Mussel Tissue XI and Marine Sediment XII material was stored at -80 °C until 

shipped via overnight delivery to participating laboratories. Instructions for the storage and use 

of the exercise material and a diskette with files for electronic submission of data were included 

with each set of material shipped. These instructions are reproduced in Appendices A and B. 

Each laboratory participating in these intercomparison exercises was sent the following by 

overnight delivery: 

Exercise 1: Mussel Tissue XI (QA03TIS11) 

Three bottles of Mussel Tissue XI material (shipped on dry ice) 

Three bottles of SRM 1974b, Organics in Mussel Tissue, (shipped on dry 

ice) 

Description of the materials and storage/use/reporting instructions for 

 the exercise (See Appendix A.) 

Data diskette with files for the reporting of results 

Exercise 2: Marine Sediment XII (QA02SED11) 

Three bottles of Marine Sediment XII material (shipped on dry ice) 

Description of the materials and storage/use/reporting instructions for 

 the exercise (See Appendix B.) 

Data diskette with files for the reporting of results 

In the letter accompanying each shipment each participant was asked to analyze each of three 

replicate samples (one from each jar) to provide a more realistic assessment of laboratory 

precision and, if possible, to concurrently analyze the NIST SRM 1974b [5] with Mussel Tissue 

XI and NIST SRM 1941b Organics in Marine Sediment [6] with Marine Sediment XII. 

Evaluation of Exercise Results

Establishment of the Assigned Values

The following guidelines were used by the NIST exercise coordinators for the establishment of 

the exercise "Assigned Values" for these two exercises. Each laboratory’s performance on 

concurrent reference material analyses was used to determine if that laboratory’s results would 

be eligible for inclusion in the calculation of the exercise assigned value for the unknown 
 

material for a particular analyte. The results reported for the unknown materials from 

laboratories that did not report results for the reference materials were not used in these 

calculations. After the exercise assigned values, standard deviations, and 95% confidence limits 

had been calculated, all reported results for the Mussel Tissue XI and Marine Sediment XII 

materials were evaluated relative to the exercise assigned values. 

Laboratory data submission: Each participating laboratory was to submit data from three 

replicate determinations of the “unknown” materials (Mussel Tissue XI and Marine Sediment 

XII) and was requested to report results of concurrent analyses of NIST SRM 1974b, a 

cryogenically homogenized mussel tissue reference material, and SRM 1941b, a marine 

sediment reference material. Laboratories were requested to report these results to three 

significant figures, and to provide brief descriptions of their extraction, cleanup, and analytical 

procedures. 

Determination of laboratory analyte means: For each laboratory, the laboratory analyte mean of 

the three sample results (S1, S2, and S3) was calculated for each analyte. Non-numerical data 

were treated as follows: A mean "<value" was used when three "<values" were reported; NA 

(not analyzed/determined) was used for three reported NA's; and, if the reported results were of 

mixed type, e.g., S1 and S2 were numerical values and S3 was reported as “<value”, the two 

similar "types" were used to either determine the mean or to set a non-numerical descriptor. 

Determination of assigned values: The assigned values are the means of the acceptable data as 

defined here. For a particular analyte, the performance on the reference material was deemed 

acceptable for the purpose of this exercise if the laboratory result was within 30 % of the upper 

and lower limits of the confidence interval for analytes listed in the Certificates of Analysis for 

SRM 1974b and SRM 1941b. For each analyte of interest not certified for these materials, a 

“target” concentration and the associated uncertainty were calculated. The targets for SRM 

1974b were based on reference concentrations for SRM 1974b and on results of the 2000 

exercise in which SRM 1974b was used as an unknown. The targets for SRM 1941b were based 

on results of the 1999 exercise in which SRM 1941b was used as the unknown material 

Laboratory results within target upper and lower limits, typically 30 % to 40 %, of these 

concentrations were deemed acceptable for this exercise. If a laboratory demonstrated 

acceptable performance on a particular analyte in the reference material, that laboratory’s results 

for that analyte in the corresponding “unknown” exercise material was then used in the 

calculation of the analyte’s exercise assigned value, unless it was deemed an outlier. For 

evaluation of potential outliers, statistical tests and expert analyst judgement were used after 

viewing both normal and log normal plots of the data. This judgement utilized knowledge of 

potential coeluters based on the laboratory's reported methods. In instances in which the analyte 

concentration was below the detection limit of most participating laboratories, no exercise 

assigned value was calculated. In data sets where a number of laboratories report results as "not 

detected" at various detection limits, there is no consensus as to what numerical value should be 

assigned to these results in the computation of grand means, etc.; e.g., "0,” half Detection Limit 

(DL), and the DL value itself have all been used and the choice is influenced by the particular 

data set. 
 

Reported Results

Laboratories were assigned numerical identification codes in order of receipt of data with the 

exception of NIST, which is Laboratory 1 in these exercises. A laboratory was assigned the 

same code for each material. There are three results from NIST reported: 1a and 1b both 

generated in the NIST Gaithersburg laboratory and 1c generated in the NIST Charleston 

laboratory. For the NIST data, the following extraction methods were used: pressurized fluid 

extraction (PFE) with dichloromethane for 1a; Soxhlet extraction with dichloromethane for the 

1b; and PFE with dichloromethane for 1c. For the PAHs, methods 1a, 1b, and 1c used gas 

chromatography/mass spectrometry (GC/MS) for analysis with either a proprietary nonpolar 

phase (1a) or a 50 % (mole fraction) phenyl phase (1b and 1c). For the chlorinated analytes, 1a 

and 1b used GC/MS with the proprietary nonpolar phase while the 1c method used GC with 

electron capture detection (GC-ECD), combining results obtained with a 5 % (mole fraction) 

phenyl phase and a proprietary nonpolar phase. 

A laboratory was assigned the same code for each material. The laboratory mean replicate data 

are shown in Tables 2 to 4 and Tables 5 to 7 for the Mussel Tissue XI and SRM 1974b, 

respectively, and in Tables 8 to 10 and 11 to 13 for Marine Sediment XII and SRM 1941b, 

respectively. Included in the means tables for Mussel Tissue XI and Marine Sediment XII are 

the exercise assigned values, the standard deviation of the assigned value, the percent relative 

standard deviation (% RSD), and the calculated 95 % confidence limit of the assigned value for 

the percent water, percent total extractable organics, TEO (mussel tissue), total organic carbon, 

TOC (sediment), PAHs, chlorinated pesticides, and PCB congeners. Notes included by a 

laboratory with its data are listed in Appendices C (Mussel Tissue XI) and D (Marine Sediment 

XII). Summaries of the methods used by each laboratory are in Appendices E (Mussel Tissue 

XI) and F (Marine Sediment XII). Tables 5 through 7 and 11 through 13 summarize the data 

received from the participating laboratories for SRM 1974b and 1941b, respectively. The 

certified and target values for the analytes of interest are also shown in these tables. For the 

Mussel Tissue XI and SRM 1974b, laboratory 9 originally submitted their data in terms of dry 

mass. The laboratory sent revised data (lab 9 rev in Tables 2 through 7) in terms of wet mass. 

In Appendices G (Mussel Tissue XI) and H (Marine Sediment XII), charts of the mean numerical 

results reported by each laboratory for each analyte are shown for the exercise material and the 

corresponding reference material. In these Appendices, only lab 9’s original data submissions 

are included. The revised data from Lab 9 (Lab 9 rev) should be used in evaluating their 

performance. 

Performance Scores

The exercise coordinators recognize that different programs have different data quality needs. 

The acceptability of the results submitted by a particular laboratory will be decided by the 
 

individual program(s) for which the laboratory provides data. Typically, the program will use 

these exercise results in conjunction with the laboratory's performance in the analysis of certified 

reference materials and/or control materials, and of other quality assurance samples. These 

exercise results are exhibited in a number of ways in this report to facilitate their use by these 

programs in their acceptability assessments. 

IUPAC guidelines [7] describe the use of z-scores and p-scores for assessment of accuracy and 

precision in intercomparison exercises such as those described in this report. These indices 

assess the difference between the result of the laboratory and the exercise assigned value and can 

be used, with caution, to compare performance on different analytes and on different materials. 

Accuracy Assessment (z-score)

z-score = (bias estimate)/(performance criterion) = (x - X)/ σ

where x is the individual laboratory result, X is the "Exercise Assigned Value,” and σ is the 

target value for standard deviation. 

As described in the IUPAC guidelines, the choice of σ is dependent upon data quality objectives 

of a particular program. It can be "fixed" and arrived at by perception, prescription, or reference 

to validated methodology (e.g., σ = 0.025 X; X is the exercise assigned value,), or it can be an 

estimate of the actual variation (e.g., the calculated sample standard deviation, s, from the 

exercise data). The "fixed" performance criterion is more useful in the comparison of a 

laboratory's performance on different materials while the use of the actual variation may be more 

useful within a given exercise, for example, if the determination of a particular analyte is 

exceptionally problematic. 

 

We have calculated and reported z-scores using the fixed performance criterion for each analyte 

for each laboratory. At a previous workshop, it was decided to use "25 % of the exercise 

assigned value" as the fixed target value for standard deviation for this program. The z-scores 

calculated for these exercises can thus be interpreted as shown in the following examples: 
z-score (25 % X): 

+1 ⇒ laboratory result is 25 % higher than the assigned value 

-2 ⇒ laboratory result is 50 % lower than the assigned value 

From a scientific point of view, IUPAC does not recommend the classification of zscores but allows that a common classification is: 

z ≤ 2 Satisfactory 

2 < z < 3 Questionable 

z ≥ 3 Unsatisfactory 

Tables 14 through 16 summarize the z-scores (25 %) for each laboratory for each 

reported analyte in Mussel Tissue XI while Tables 17 through 19 summarize the z-scores 

(25 %) for each laboratory for each reported analyte in Marine Sediment XII. 

Precision Assessment (p-score)

 p-score = σlab / σtarget

Prior to the 1994 exercises, participating laboratories typically analyzed the three 

replicate samples for an exercise with the same sample set, i.e., one set of samples with 

the same blank, calibration curve, etc. applicable for each. Since the repeatability for 

replicates within a set generally shows better reproducibility than for replicates across 

different sets, this does not result in data that are very useful for realistic uncertainty 

assessment. Since 1994, laboratories have been requested to process each replicate in a 

different sample set for uncertainty assessment. For the calculation of p-scores for this 

program, the σ values used are coefficients of variation (CV calculated as relative 

standard deviations) with the current target σ (CV) for the three replicates being 15 %. 

Tables 20 through 22 summarize the p-scores (15 %) for each laboratory for each 

reported analyte in Mussel Tissue XI while Tables 23 through 25 summarize the p-scores 

(15 %) for each laboratory for each reported analyte in Marine Sediment XII . 

Discussion

Laboratories were requested to quantify 26 PAHs, 25 chlorinated pesticides, and 25 PCB 

congeners in this year’s exercise. A total of 17 sets of results were submitted for Mussel 

Tissue XI, and 21 sets of results were submitted for Marine Sediment XII. For the 

sediment exercise, one laboratory (3) reported data for SRM 1941a Organics in Marine 

Sediment as the control material, and four laboratories (5, 6, 17, and 18) reported data for 

SRM 1944 as the control material. Their data were evaluated based on the certified and 

target values for these SRMs (see Evaluation of Exercise Results above). Laboratories 

12 and 14 did not submit data for a sediment reference material so the data from these 

laboratories were not used for the determination of the exercise assigned values for 

Marine Sediment XII. 
 

The concentrations of the PAHs of interest in Mussel Tissue XI range from < 1 ng/g wetmass basis to 30 ng/g wet-mass basis, the concentrations of the pesticides of interest 

range from < 1 ng/g wet-mass basis to 3 ng/g wet-mass basis, and the concentrations of 

the PCB congeners range from < 1 ng/g wet-mass basis to 10 ng/g wet-mass basis. For 

the chlorinated pesticides, 13 of the 25 compounds were above the detection limits for the 

majority of the laboratories reporting, while 21 of the 25 PCB congeners were above the 

detection limits for the majority of the laboratories. There was good agreement among 

the laboratories for the percent water in Mussel Tissue XI, but poor agreement among the 

laboratories for the TEOs, ranging from 0.27 % to 7.49 %. 

The concentrations of all of the analytes of interest were very similar between Mussel 

Tissue XI and SRM 1974b. Both materials were collected from Dorchester Bay, but the 

mussels used to prepare Mussel Tissue XI were collected in February 1992 while the 

mussels used to prepare SRM 1974b were collected in October 1999. 

The z-scores for the PAHs, pesticides, and PCB congeners in Mussel Tissue XI based on 

25 % of the exercise assigned value are summarized in Tables 14 to 16, respectively. The 

majority of the z-scores based on 25 % are within ± 2 (± 50 % of the exercise assigned 

value). The p-scores for the Mussel Tissue XI based on a 15 % relative standard 

deviation are summarized in Tables 20 to 22 for the PAHs, pesticides, and PCB 

congeners, respectively. It should be noted that the p-scores (15 %) for a number of 

laboratories are greater than 1. This means that the relative standard deviation for the 

three aliquots of Mussel Tissue XI from the one laboratory is greater than 15 %. 

The PAH concentrations in Marine Sediment XII range from 20 ng/g dry-mass basis to 

1100 ng/g dry-mass basis. The pesticide concentrations range from below the detection 

limits of the methods used to 20 ng/g dry-mass basis, while the PCB concentrations range 

from 1 ng/g dry-mass basis to 40 ng/g dry-mass basis. There was good agreement among 

the laboratories for percent water in the wet sediment. Only four laboratories returned 

data for the TOC with the values ranging from 1.82 % to 3.02 %. 

As has been mentioned above, the mussel tissue used in this exercise was relabeled 

(QA03TIS11) after being used in two previous exercises (QA92TIS4 and QA98TIS9), 

and the dry sediment used to prepare Marine Sediment XII (QA03SED12) was also used 

to prepare the sediment used in the 1998 exercise (QA98SED8). The exercise assigned 

values for the three exercises in the case of the mussel tissue and for the two exercises in 

the case of the marine sediment are summarized in Tables 26, 27, and 28 for the PAHs, 

pesticides, and PCBs, respectively, and selected compounds are shown graphically 

below. 
 

0

50

100

150

200

250

300

350

phen anth pyrene B[a]A B[e]P B[a]P I[1,2,3-

cd]P

B[ghi]P

ng/g dry basis

QA92TIS4

QA98TIS9

QA03TIS11

0

10

20

30

40

50

60

cischlortransnonadieldrin 4,4'-

DDE

2,4'-

DDD

4,4'-

DDD

2,4'-

DDT

4,4'-

DDT

ng/g dry basis

QA92TIS4

QA98TIS9

QA03TIS11

0

20

40

60

80

100

120

140

160

PCB 28 PCB 52 PCB

101

PCB

105

PCB

118

PCB

153

PCB

170

PCB

180

ng/g dry basis

QA92TIS4

QA98TIS9

QA03TIS11
 

0

5

10

15

20

25

30

cischlortransnonacisnona4,4'-

DDE

2,4'-

DDD

4,4'-

DDD

2,4'-

DDT

4,4'-

DDT

ng/g dry basis

QA98SED8

QA03SED12

0

10

20

30

40

50

60

70

80

PCB

28

PCB

52

PCB

101

PCB

105

PCB

118

PCB

153

PCB

170

PCB

180

ng/g dry basis

QA98SED8

QA03SED12

Overall, the agreement among the consensus means from the three exercises for the 

mussel tissue and the two exercises for the marine sediment is good (falling within one 

standard deviation of the exercise assigned value). There are some cases where 

improvements in the analytical methods used from 1992 to 2003 may explain the 

differences in the mussel tissue data. For example, the consensus mean data for 2,6-

dimethylnaphthalene and 1,6,7-trimethylnaphthalene dropped 70 % and 34 %, 

respectively, from the 1992 to 1998 exercise and then were consistent between the 1998 

and 2003 exercise. Both of these compounds can potentially coelute with other di- and 

trimethylnaphthalenes. Participants are now aware of these potential coelutions and have 

taken steps (i.e., longer columns, modified temperature programs) to separate the 

isomers. Similar examples for the pesticides include dieldrin and 4,4’-DDE which elute 

near one another and can sometimes switch retention order depending on column and 

temperature program. The PCB congener data are fairly consistent among the three 

exercises for the mussel tissue. This may be attributed to the discussions of elution order 

for the PCB congeners in the early meetings that were held for the intercomparison 

exercises. The marine sediment exercises do not show as much of a difference, probably 
 

because the first use of this sediment was in 1998 after methods had been changed and 

refined. 

 

The z-scores for the PAHs, pesticides, and PCB congeners based on 25 % of the exercise 

assigned value are summarized for Marine Sediment XII in Tables 17 to 19, respectively. 

In general, the z-scores based on 25 % were within ± 2 (± 50 % of the exercise assigned 

value) for Marine Sediment XII. The p-scores for the Marine Sediment XII based on a 

15 % relative standard deviation are summarized in Tables 23 to 25 for the PAHs, 

pesticides, and PCB congeners, respectively. As for the Mussel Tissue XI, it should be 

noted that the p-scores (15 %) for a number of laboratories are greater than 1 (the relative 

standard deviation for the three aliquots of Marine Sediment XII from the one laboratory 

is greater than 15 %). 

As in the past exercises, a variety of methods were used for extraction, extract cleanup, 

and analysis. These are summarized in Appendix E for the mussel tissue and Appendix F 

for the marine sediment. For the PAHs in the mussel tissue and marine sediment, 

laboratory 19 used gas chromatography with ion trap mass spectrometry (GC/ITMS) 

while the remainder of the participating laboratories in each exercise specified GC/MS. 

For the chlorinated analytes in the mussel tissue, laboratory 16 specified the use of highresolution MS and 10 of the remaining laboratories used GC-ECD. Laboratory 16 also 

specified the use of high-resolution GC/MS for the chlorinated compounds in the marine 

sediment, and 11 of the remaining laboratories used GC-ECD. There was no obvious 

correlation between z-scores and method used. 

For the 2003 exercises, the data provided in the various figures and tables of this report 

can be used for assessing the comparability of results of over 75 analytes of interest in 

this program and the performance of individual laboratories. The z-scores and the pscores for the mussel tissue are summarized in Tables 14 to 16 and Tables 20 to 22, 

respectively, and the z-scores and the p-scores for the marine sediment are summarized in 

Tables 17 to 19 and Tables 23 to 25, respectively. For both materials, the highest 

percentage of z-scores and p-scores that were in the unsatisfactory category were for the 

chlorinated pesticides. In both of these materials, the chlorinated pesticides were 

typically present at lower concentrations than the concentrations of the PAHs and PCB 

congeners. In these exercises, interlaboratory variability is a greater contributor to 

measurement incomparability than intralaboratory variability. Laboratories reporting 

results of concurrent reference material analyses typically demonstrate better 

performance than those laboratories that do not analyze the reference materials. 

Subgroups of the exercise participants have demonstrated comparability of results for 

many analytes within the 0 to 2 z-range based on use of 25 % of the exercise assigned 

concentration as the performance criterion. This implies that this subgroup can 

distinguish between two samples that have an analyte concentration difference of 100 %. 

The reported accuracy and reproducibility indices (z- and p-scores, respectively) can be 

easily converted to conform to the acceptability requirements of a particular program. 

For example, a z-score based on 25 % can be multiplied by two to convert to a z-score 

based on 12.5 % of the analyte concentration. 
 

It is important to evaluate the non-quantitative results reported by each laboratory as well. 

Although these results are not easily presented or numerically evaluated, they are 

included in the various tables of this report that list the mean and individual results of the 

laboratories. The laboratory and its data users should closely examine these nonquantitative results. Decisions based on false negative or false positive results from a 

laboratory can lead to significant environmental and/or economic consequences. Some 

laboratories reported detection limits in these “real” matrix materials that may be too high 

for the data quality needs of their program(s), and these issues should be assessed as well. 

Intercomparison exercises provide an important mechanism for assessing the 

comparability, accuracy, precision, and reproducibility of data being produced by the 

participating laboratories. Exercise materials similar in matrix, form, and analyte 

concentration to typical samples routinely analyzed by the laboratories are most useful 

for demonstrating the level of comparability and for revealing potential problem areas. 

For the determination of the target compounds in these complex marine matrices with 

relatively low levels of these analytes, the levels of bias and reproducibility of many of 

the participating laboratories meet their current acceptability requirements; however, 

there is certainly room for improvement. Minimizing the among-laboratory biases so that 

the analytical variability is significantly less than the field sampling variability should be 

an achievable goal. 

Acknowledgments

The time and effort of the analysts and management of the participating laboratories and 

the assistance of the NIST Standard Reference Materials Program with the procurement 

and preparation of the exercise materials are gratefully acknowledged. 

Disclaimer 

Certain commercial equipment, instruments, or materials are identified in this report to 

specify adequately the experimental procedure. Such identification does not imply 

recommendation or endorsement by the National Institute of Standards and Technology, 

nor does it imply that the materials or equipment identified are the best available for the 

purpose. 

References

1. A. Y. Cantillo and R. M. Parris, “Evaluation of Trace Organic NOAA Status and 

Trends Quality Assurance Project Performance,” in Quality Assurance for 

Analytical Laboratories, M. Parkany (ed.), Royal Society of Chemistry, Spec. 

Publ. No. 130 (1993). 
 

2. A. Y. Cantillo and R. M. Parris, National Status and Trends Program Quality 

Assurance Project: Trace Organic Intercomparison Exercise Results 1986-1990, 

NOAA Tech. Memo. NOS/ORCA 69, Silver Spring, MD (1994). 

3. A. Y. Cantillo, NS&T Quality Assurance Project Intercomparison Exercise 

Results 1991-1993, NOAA Tech. Memo. NOS/ORCA 79, Silver Spring, MD 

(1995). 

4. Schantz, M.M., Parris, R.M., and Wise, S.A., NIST/NOAA NS&T 

Intercomparison Exercise Program for Organic Contaminants in the Marine 

Environment: Description and Results of 1998 Organic Intercomparison 

Exercises, NOAA Tech Memo NOS ORCA 138, Silver Spring, MD (1998). 

5. Certificate of Analysis for Standard Reference Material (SRM) 1974b, Organics 

in Mussel Tissue (Mytilus edulis), National Institute of Standards and Technology 

(NIST), Gaithersburg, MD, 2003. 

https://srmors.nist.gov/view_detail.cfm?srm=1974B

6. Certificate of Analysis for Standard Reference Material (SRM) 1941b, Organics 

in Marine Sediment, National Institute of Standards and Technology (NIST), 

Gaithersburg, MD, 2002. https://srmors.nist.gov/view_detail.cfm?srm=1941B

7. IUPAC “The International Harmonized Protocol for the Proficiency Testing of 

(Chemical) Analytical Laboratories,” Pure Appl. Chem. 65 (9), 2123-2144 

(1993). 
 

List of Tables

Table 1. Target Analytes in NIST Intercomparison Exercise Program for Organic 

Contaminants in the Marine Environment. 

Table 2. Mussel Tissue XI (QA03TIS11): Laboratory means of three replicates and 

exercise assigned values –Water, TEO, and PAHs 

Table 3. Mussel Tissue XI (QA03TIS11): Laboratory means of three replicates and 

exercise assigned values –Pesticides 

Table 4. Mussel Tissue XI (QA03TIS11): Laboratory means of three replicates and 

exercise assigned values –PCBs. 

Table 5. SRM 1974b: Laboratory means of three replicates and target values – Water, 

TEO, and PAHs. 

Table 6. SRM 1974b: Laboratory means of three replicates and target values – 

Pesticides. 

Table 7. SRM 1974b: Laboratory means of three replicates and target values – PCBs. 

Table 8. Marine Sediment XII (QA03SED12): Laboratory means of three replicates 

and exercise assigned values –Water, TOC, and PAHs 

Table 9. Marine Sediment XII (QA03SED12): Laboratory means of three replicates 

and exercise assigned values – Pesticides 

Table 10. Marine Sediment XII (QA03SED12): Laboratory means of three replicates 

and exercise assigned values – PCBs 

Table 11. SRM 1941b: Laboratory means of three replicates and target values – Water, 

TOC, and PAHs. 

Table 12. SRM 1941b: Laboratory means of three replicates and target values – 

Pesticides. 

Table 13. SRM 1941b: Laboratory means of three replicates and target values – PCBs. 

Table 14. Mussel Tissue XI (QA03TIS11): z-scores (25 %) by laboratory- PAHs and 

Water 

Table 15. Mussel Tissue XI (QA03TIS11): z-scores (25 %) by laboratory – Pesticides 

Table 16. Mussel Tissue XI (QA03TIS11): z-scores (25 %) by laboratory – PCBs 
 

Table 17. Marine Sediment XII (QA03SED12): z-scores (25 %) by laboratory – PAHs, 

Water, TOC 

Table 18. Marine Sediment XII (QA03SED12): z-scores (25 %) by laboratory – 

Pesticides 

Table 19. Marine Sediment XII (QA03SED12): z-scores (25 %) by laboratory – PCBs 

Table 20. p-scores (15 %) for water, TEO, and PAHs in Mussel Tissue XI and SRM 

1974b 

Table 21. p-scores (15 %) for pesticides in Mussel Tissue XI and SRM 1974b 

Table 22. p-scores (15 %) for PCBs in Mussel Tissue XI and SRM 1974b 

Table 23. p-scores (15 %) for water, TOC, and PAHs in Marine Sediment XII and SRM 

1941b 

Table 24. p-scores (15 %) for pesticides in Marine Sediment XII and SRM 1941b 

Table 25. p-scores (15 %) for PCBs in Marine Sediment XII and SRM 1941b 

Table 26. Comparison to previous exercise assigned values for PAHs (ng/g dry basis) 

Table 27. Comparison to previous exercise assigned values for pesticides (ng/g dry 

basis) 

Table 28. Comparison to previous exercise assigned values for PCBs (ng/g dry basis) 

and water (%) 
 

Table 1: Analytes of Interest in NIST Intercomparison Exercise Program for 

Organic Contaminants in the Marine Environment 

Chlorinated Pesticides 

hexachlorobenzene 2,4'-DDE 

alpha-HCH (alpha-BHC) 4,4'-DDE 

beta-HCH (beta-BHC) 2,4'-DDD 

gamma-HCH (gamma-BHC, lindane) 4,4'-DDD 

heptachlor 2,4'-DDT 

heptachlor epoxide 4,4'-DDT 

cis-chlordane (alpha-chlordane) chlorpyrifos 

trans-chlordane (gamma-chlordane) aldrin 

oxychlordane dieldrin 

cis-nonachlor endrin 

trans-nonachlor endosulfan I 

mirex endosulfan II 

endosulfan sulfate 

Polychlorinated Biphenyl Congeners

 PCB No. Compound Name

 8 2,4'-dichlorobiphenyl 

 18 2,2',5-trichlorobiphenyl 

 28 2,4,4'-trichlorobiphenyl 

 31 2,4',5-trichlorobiphenyl 

 44 2,2',3,5'-tetrachlorobiphenyl 

 49 2,2',4,5'-tetrachlorobiphenyl 

 52 2,2',5,5'-tetrachlorobiphenyl 

 66 2,3',4,4'-tetrachlorobiphenyl 

 95 2,2',3,5',6-pentachlorobiphenyl 

 99 2,2',4,4',5-pentachlorobiphenyl 

 101 2,2',4,5,5'-pentachlorobiphenyl 

 105 2,3,3',4,4'-pentachlorobiphenyl 

 118 2,3',4,4',5-pentachlorobiphenyl 

 128 2,2',3,3',4,4'-hexachlorobiphenyl 

 138 2,2',3,4,4',5'-hexachlorobiphenyl 

 149 2,2',3,4',5',6-hexachlorobiphenyl 

 153 2,2',4,4',5,5'-hexachlorobiphenyl 

 156 2,3,3',4,4',5-hexachlorobiphenyl 

 170 2,2',3,3',4,4',5-heptachlorobiphenyl 

 180 2,2',3,4,4',5,5'-heptachlorobiphenyl 

 187 2,2',3,4',5,5',6-heptachlorobiphenyl 

 194 2,2',3,3',4,4',5,5'-octachlorobiphenyl 

 195 2,2',3,3',4,4',5,6-octachlorobiphenyl 

 206 2,2',3,3',4,4',5,5',6-nonachlorobiphenyl 

 209 decachlorobiphenyl 
 

Table 1. (continued) 

Polycyclic aromatic hydrocarbons (PAH)

naphthalene pyrene 

2-methylnaphthalene benz[a]anthracene 

1-methylnaphthalene chrysene 

biphenyl triphenylene 

2,6-dimethylnaphthalene benzo[b]fluoranthene 

acenaphthylene benzo[j]fluoranthene 

acenaphthene benzo[k]fluoranthene 

1,6,7-trimethylnaphthalene benzo[e]pyrene 

fluorene benzo[a]pyrene 

phenanthrene perylene 

anthracene indeno[1,2,3-cd]pyrene 

1-methylphenanthrene dibenz[a,h]anthracene 

fluoranthene benzo[ghi]perylene 

 
Table 2. Mussel TissueXI (QA03TIS11): Laboratory means of three replicates and exercise assigned values - Water, TEO, and PAHs 

 (reported to three significant figures) Exercise Assigned

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20 Value s %RSD

Water (percent) 91.6 NA 90.1 NA NA 91.1 91.9 91.2 91.2 92.0 89.7 91.7 91.6 91.9 84.9 92.4 91.1 93.1 91.5 0.8 0.9

TEO (percent) 0.617 NA 0.610 0.270 0.367 0.623 0.400 NA NA 7.49 0.267 0.699 0.288 0.332 NA 0.424 0.563 5.12 not calculatedPAHs (ng/g wet mass) Exercise Assigned

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20 Value s %RSD 95% CL

naphthalene 1.94 3.80 2.20 <4.0 NA 2.31 1.41 78.5 6.85 16.9 2.49 NA 1.25 NA 1.21 5.48 <6.55 NA 2.19 0.85 38.8 0.71

2-methylnaphthalene 3.17 3.18 5.30 <4.0 NA 2.99 1.68 35.5 3.10 34.0 1.76 NA 1.64 NA 1.82 4.27 <3.59 3.19 2.27 0.78 34.5 0.72

1-methylnaphthalene 2.06 1.90 3.35 <4.0 NA <2.0 1.01 21.1 1.84 23.9 1.14 34.2 0.903 NA 1.28 2.97 <2.61 1.79 1.65 0.86 52.2 0.80

biphenyl 1.00 1.22 1.49 <4.0 NA <2.0 <1.0 13.1 1.15 11.9 NA NA 1.03 NA 0.557 2.27 <4.11 NA 1.06 0.34 32.3 0.36

2,6-dimethylnaphthalene 2.87 2.11 3.11 <4.0 NA 3.23 3.48 35.6 3.11 47.8 1.85 NA 2.83 NA 2.87 4.70 2.585 2.30 2.77 0.52 18.8 0.37

acenaphthylene 0.545 <0.1 0.476 <4.0 NA <2.0 <1.3 8.10 0.705 21.4 1.04 NA 0.471 NA 0.550 1.49 <1.10 0.879 0.584 0.169 28.9 0.177

acenaphthene 0.741 <0.3 1.79 <4.0 NA <2.0 <1.3 7.42 0.640 15.9 1.14 NA 0.675 NA 0.647 1.40 <4.21 0.920 1.05 0.52 49.2 0.481,6,7-trimethylnaphthalene 2.74 NA 4.02 <4.0 NA <2.0 NA NA NA 48.8 1.53 NA 2.85 NA 2.28 4.80 3.84 1.75 2.50 0.84 33.6 0.88

fluorene 1.75 1.49 3.26 <4.0 NA <2.0 2.67 <57.0 <4.96 30.7 NA 1.91 1.60 NA 1.16 3.62 <1.82 1.53 2.26 0.93 41.1 0.98

phenanthrene 10.8 11.6 12.5 8.42 NA 9.50 32.1 157 13.7 123 9.90 10.2 11.8 NA 8.11 11.8 12.1 11.1 10.8 1.4 12.6 0.9

anthracene 0.923 <2 1.67 <4.0 NA <2.0 <0.7 17.3 1.51 25.1 NA 1.01 0.954 NA 0.827 1.57 <2.26 NA 0.939 0.022 2.3 0.054

1-methylphenanthrene 5.11 NA 5.49 4.06 NA 3.75 5.42 40.0 3.50 57.8 NA NA 5.24 NA 3.01 3.59 4.10 4.43 4.42 0.86 19.4 0.58

fluoranthene 27.6 29.3 33.4 23.3 NA 24.6 31.8 252 22.0 331 23.3 41.7 31.9 NA 21.0 28.1 30.3 28.9 28.2 3.9 13.7 2.6

pyrene 21.8 20.4 23.9 18.0 NA 18.8 23.9 191 16.7 264 18.1 21.5 24.4 NA 16.4 17.0 20.9 20.4 20.4 2.7 13.1 1.4

benz[a]anthracene 5.51 6.41 8.70 4.67 NA 7.08 7.06 72.7 6.34 91.2 5.78 NA 9.88 NA 4.83 9.24 7.54 6.54 6.41 1.25 19.6 0.84

chrysene 10.8 11.1 NA NA NA 16.2 20.8 173 15.2 205 NA NA NA NA 14.5 NA NA NA 12.8 2.4 18.8 6.0

triphenylene 6.26 6.24 NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 6.25 ND ND ND

benzo[b ]fluoranthene 6.90 7.50 5.83 NA NA 6.98 9.07 106 9.25 122 NA NA 8.24 NA 5.42 8.72 7.19 NA 7.32 1.23 16.8 0.94benzo[j ]fluoranthene 3.05 3.06 2.51 NA NA NA NA NA NA NA NA NA NA NA 4.89 NA NA NA 3.38 1.04 30.8 1.65benzo[k ]fluoranthene 3.32 3.46 2.97 <4.0 NA 2.28 6.07 28.1 2.47 27.5 3.60 5.67 NA NA NA NA NA 2.28 3.43 1.28 37.5 1.07

benzo[e]pyrene 8.29 9.42 7.88 7.77 NA 6.31 11.4 85.0 7.43 95.0 8.41 3.09 10.3 NA 7.56 8.99 9.65 10.7 8.89 1.48 16.6 0.94

benzo[a]pyrene 1.98 2.27 10.3 <4.0 NA <2.0 2.88 <57.0 <4.96 34.5 4.28 NA 2.89 NA 1.56 4.36 <6.31 1.86 2.76 1.07 38.7 0.89

perylene 0.683 1.09 NA <4.0 NA <2.0 1.01 <57.0 <4.96 10.4 0.808 NA 1.03 NA 0.543 1.35 <3.67 0.796 0.914 0.257 28.1 0.215

indeno[1,2,3-cd]pyrene 1.37 2.34 1.51 <4.0 NA <2.0 2.31 16.2 1.41 18.5 2.09 NA 2.30 NA 1.16 3.90 <6.13 1.37 2.04 0.84 41.2 0.60

dibenz[a,h]anthracene 0.475 0.554 0.232 <4.0 NA <2.0 <1.3 <57.0 <4.96 4.37 1.58 NA NA NA 0.263 NA <1.06 0.376 0.380 0.137 36.0 0.170

benzo[ghi]perylene 1.50 2.68 2.06 <4.0 NA <2.0 2.08 17.1 1.49 22.5 0.793 NA 2.60 NA 1.29 3.79 <3.95 1.51 2.19 0.82 37.6 0.63

chrysene/triphenylene 20.8 13.9 15.0 22.8 19.0 19.5 17.5 16.3 2.8 17.1 2.6benzo[b+j]fluoranthene 6.79 8.90 7.85 ND ND NDbenzo[b+a]fluoranthene 9.79 9.79 ND ND NDbenzo[j+k]fluoranthene 6.96 7.03 6.11 6.70 ND ND NDdibenz[a,h+a,c]anthracene 0.540 1.33 0.935 ND ND ND

Note: Bolded values were not used in the calculation of the exercise assigned value.*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 3. Mussel Tissue XI (QA03TIS11): Laboratory means of three replicates and exercise assigned values - Pesticides

 (reported to three significant figures)ng/g wet mass Exercise Assigned

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20 Value s %RSD 95% CL

alpha-HCH (a-BHC) <0..2 NA <0.3 NA <1 <0.5 <0.5 <2.85 <0.496 0.433 NA 0.252 <0.424 0.116 DL <0.423 NA < 0.1 <1hexachlorobenzene <0..2 <0.4 <0.3 NA <1 <0.5 <0.4 <2.85 <0.496 0.877 DL NA <0.424 0.136 0.0533 <0.423 <0.062 0.0392 <1gamma-HCH (g-BHC,lindane) <0..2 NA <0.3 NA <1 <0.5 <0.4 <2.85 <0.496 0.113 DL 0.198 <0.425 0.0547 0.0667 <0.423 0.501 0.0430 <1

beta-HCH (b-BHC) <0..2 NA <0.3 NA <1 <0.5 NA <2.85 <0.496 0.320 NA 0.044 <1.15 <0.019 0.0300 <0.423 NA 0.0543 <1heptachlor <0..2 NA 0.566 NA <1 <0.5 <0.3 <2.85 <0.496 2.24 DL 0.246 <0.426 0.114 DL <0.423 0.125 < 0.11 0.263 0.211 80.2 0.335aldrin <0..2 NA <0.3 NA <1 <0.5 <0.5 <2.85 <0.496 2.60 NA 0.112 1.56 0.0685 DL <0.423 <0.012 < 0.1 <1heptachlor epoxide <0..2 NA <0.3 NA <1 <0.5 <0.4 <2.85 <0.496 ND DL NA <0.426 0.0653 DL <0.423 0.285 < 0.1 <1oxychlordane <0..2 NA 0.370 NA <1 <0.5 NA <2.85 <0.496 3.77 NA NA <1.14 <0.089 DL 17.3 NA 0.290 0.330 ND ND ND

gamma-chlordane 0.918 1.60 1.06 NA 1.14 1.03 0.852 17.0 1.71 15.6 NA 2.53 1.09 1.37 1.17 0.799 NA 0.683 1.19 0.52 43.3 0.33

2,4'-DDE <0..2 <0.4 0.211 NA NA <1.0 NA <2.85 <0.496 2.29 DL 1.42 <0.439 <0.105 DL <0.423 NA 0.241 0.226 ND ND ND

endosulfan I <0..2 NA <0.3 NA NA <1.0 <0.4 <2.85 <0.496 ND NA 0.164 <1.14 <0.207 DL 29.4 <0.1 < 0.1 <2cis-chlordane (alpha-chlordane 1.23 1.57 1.37 NA 1.12 0.970 1.65 11.2 0.982 15.2 1.37 0.872 1.22 1.19 1.28 0.897 2.62 0.778 1.19 0.26 22.2 0.15

trans-nonachlor 1.15 1.47 1.06 NA 0.758 0.845 1.10 9.85 0.863 14.7 1.08 1.28 1.08 1.68 1.22 0.749 1.29 0.713 1.13 0.28 25.1 0.17

dieldrin 0.448 NA 0.453 NA <1 <0.5 0.421 5.33 0.466 8.92 NA NA <1.12 0.269 DL <0.423 NA 0.344 0.417 0.050 12.1 0.062

4,4'-DDE 2.97 3.23 3.49 NA 2.79 2.20 3.10 51.6 4.52 39.7 3.18 1.70 3.72 2.87 3.26 2.66 3.19 2.10 2.89 0.56 19.4 0.32

2,4'-DDD 0.902 1.18 0.723 NA <1 1.17 0.829 <2.85 <0.496 13.6 0.967 0.313 0.831 0.611 0.873 0.966 0.968 1.11 0.928 0.172 18.6 0.109

endrin <0..2 NA <0.3 NA <1 <0.5 <0.5 <2.85 <0.496 1.76 NA 0.335 NA <0.209 DL <4.23 NA < 0.09 <1endosulfan II <0..2 NA <0.3 NA NA <2.0 <0.7 <2.85 <0.496 20.5 NA NA <3.70 <0.434 DL <4.23 <0.1 < 0.1 <154,4'-DDD 2.45 3.65 2.41 NA 1.26 2.02 2.34 30.1 2.64 30.6 NA 1.60 5.04 1.78 2.93 2.15 3.40 1.88 2.54 0.98 38.4 0.62

2,4'-DDT 0.531 <0.5 0.937 NA <1 <1.0 <0.7 <2.85 <0.496 8.92 NA 1.72 <0.422 <0.162 DL <4.23 0.959 0.462 0.722 0.262 36.3 0.417

cis-nonachlor 0.437 0.707 0.321 NA <1 <0.5 NA 8.27 0.723 8.93 NA 0.659 0.457 0.176 DL 0.282 NA 0.442 0.435 0.181 41.5 0.139

4,4'-DDT 0.806 1.24 6.22 NA <1 <1.0 other 10.6 0.932 9.78 DL 1.81 1.20 0.625 1.18 <4.23 0.846 0.434 0.903 0.312 34.6 0.261

mirex <0..2 NA <0.3 NA <1 <1.5 <0.5 <2.85 <0.496 0.917 DL NA <0.429 0.0700 DL <0.423 <0.157 0.0395 <1endosulfan sulfate <0..2 NA <0.3 NA NA <2.0 NA <2.85 <0.496 NA NA NA <1.14 0.0403 DL <4.23 <0.1 < 0.11 <3chlorpyrifos <0..2 NA NA NA NA <1.0 NA NA NA 3.16 NA NA NA NA DL <0.423 NA < 0.1 <1

Note: Bolded values were not used in the calculation of the exercise assigned value.*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 4. Mussel Tissue XI (QA03TIS11): Laboratory means of three replicates and exercise assigned values - PCBs

 (reported to three significant figures)ng/g wet mass Exercise Assigned

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20 Value s %RSD 95% CL

PCB 8 0.267 0.299 0.323 <2.1 NA 0.255 <0.7 3.37 0.296 29.1 NA NA NA 0.303 1.03 <0.133 0.550 0.4636 0.437 0.262 60.0 0.202

PCB 18 0.905 0.970 1.02 <0.89 NA 0.530 0.709 8.41 0.737 13.0 0.714 0.553 1.06 0.593 1.03 0.780 0.768 0.7091 0.796 0.186 23.3 0.112

PCB 28 3.19 3.08 3.63 2.37 NA 2.78 3.12 29.7 2.60 44.3 NA NA 2.59 3.67 3.19 6.00 2.80 2.6401 3.00 0.42 13.8 0.28

PCB 31 2.92 2.37 2.92 1.72 NA 2.62 NA 15.3 1.34 17.5 NA NA 4.49 2.48 NA NA NA 2.61 2.52 0.41 16.2 0.38

PCB 44 3.36 3.50 3.75 2.88 NA 3.38 3.22 33.9 2.96 41.8 3.37 2.51 3.48 5.14 3.60 3.47 3.40 2.81 3.41 1.96 57.5 1.2

PCB 49 5.41 4.36 5.97 3.59 NA 3.56 NA 18.8 1.65 64.5 4.01 2.90 4.11 3.25 4.18 3.39 NA 3.84 4.04 0.92 22.9 0.62

PCB 52 4.90 5.40 5.90 4.00 NA 4.64 4.64 35.5 3.12 69.9 4.61 3.06 5.40 4.60 5.30 4.70 5.31 4.09 4.71 0.73 15.5 0.44

PCB 66 4.01 5.35 5.76 3.44 NA 5.01 5.72 65.7 5.76 61.8 5.937 5.94 6.11 6.40 5.52 4.58 5.36 3.99 5.35 0.80 14.9 0.54PCB 95 2.91 4.80 4.25 5.13 NA 4.58 NA 39.1 3.42 62.6 2.626 2.63 4.58 4.43 NA 4.16 NA 3.35 4.24 0.70 16.5 0.54

PCB 99 4.72 4.16 6.17 3.27 NA 4.11 NA 27.0 2.37 63.7 4.14 2.33 4.59 4.84 NA 3.79 NA 3.86 4.36 0.79 18.1 0.56

PCB 101 8.39 7.95 9.78 6.76 NA 7.83 6.78 70.6 6.19 109 7.30 3.99 8.53 7.83 8.16 8.57 8.49 6.93 7.95 0.86 10.8 0.52

PCB 105 3.34 2.98 3.05 <2.7 NA 2.96 3.12 30.3 2.65 41.5 NA NA 3.54 3.19 3.21 2.91 2.89 1.84 3.00 0.43 14.4 0.29

PCB 118 8.33 6.87 6.44 6.86 NA 7.53 6.71 67.1 5.88 104 4.086 4.09 7.94 8.13 7.40 7.70 7.89 6.78 7.13 1.10 15.4 0.70

PCB 128 1.38 1.27 1.19 1.19 NA 1.26 1.20 14.1 1.24 17.5 0.769 0.769 1.33 1.15 1.24 1.20 1.55 0.8466 1.17 0.23 19.4 0.14

PCB 138 8.45 6.70 4.42 5.83 NA 8.79 7.14 69.8 6.11 109 NA NA 9.80 8.35 8.20 7.52 10.0 6.77 7.62 1.69 22.1 1.13

PCB 149 5.04 5.00 5.49 4.82 NA 5.08 NA 39.5 3.46 67.3 3.562 3.56 5.34 5.41 NA 4.09 NA 2.96 4.74 0.73 15.5 0.56

PCB 153 9.52 10.2 9.57 6.73 NA 8.20 9.20 63.6 5.58 143 NA NA 11.5 8.23 10.7 7.34 8.56 9.85 9.14 1.39 15.2 0.88

PCB 156 0.482 0.475 0.469 0.694 NA 0.424 NA 10.0 0.876 17.1 6.06 NA 0.564 0.574 NA 0.433 NA 0.573 0.521 0.087 16.7 0.067

PCB 170 0.164 0.112 <0.3 <0.78 NA <0.2 <0.5 1.68 0.148 5.56 NA NA <0.426 0.110 0.223 <0.133 0.2023 0.3255 0.178 0.101 57.0 0.161PCB 180 0.915 0.715 0.738 <0.62 NA 0.673 0.536 7.14 0.623 35.1 0.562 0.914 0.718 0.745 0.797 0.871 0.744 0.460 0.716 0.144 20.1 0.103

PCB 187 2.19 2.153 2.01 1.81 NA 2.16 2.33 20.9 1.83 29.8 NA NA 2.17 2.10 2.25 1.84 1.82 1.76 2.05 0.19 9.5 0.12

PCB 194 <0..2 <0.2 <0.3 <0.43 NA <0.2 NA 0.410 <0.496 0.573 DL 0.131 <0.431 0.0327 NA <0.133 NA 0.0234 <1PCB 195 <0..2 <0.2 <0.3 <0.33 NA <0.2 <0.5 <2.85 <0.496 0.723 NA NA <0.432 0.0100 DL <0.133 <0.12 < 0.11 <1PCB 206 <0..2 <0.1 <0.3 <0.37 NA <0.2 <0.5 <2.85 <0.496 0.433 DL 0.0920 <0.428 0.0130 DL <0.133 <0.098 0.0449 <1PCB 209 <0..2 <0.1 <0.3 <0.36 NA <0.2 <0.5 <2.85 <0.496 0.963 DL 0.0277 <0.427 0.0140 DL <0.133 <0.1 < 0.1 <1

Note: Bolded values were not used in the calculation of the exercise assigned value.*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 5. SRM 1974b: Laboratory mean three replicates and target values - water, TEO, and PAHs Certificate Values

1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20 conc 95%C

L type

Water (percent) 89.9 NA 89.6 NA NA 89.6 90.3 89.6 89.6 NA 90.9 1.40 90.0 90.2 NA 91.1 89.6 NA 89.87 0.05 Reference

TEO (percent) 0.630 NA 0.431 NA 0.440 0.720 0.450 NA NA 10.6 NA 1.29 0.351 0.430 NA 0.670 0.610 0.505 0.640 0.130 Reference ng/g wet basis (reported to three significant figures)

Certificate Values

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20 conc 95%C

L type

naphthalene 2.43 4.46 2.15 <4.0 NA <2.0 <1.3 70.7 7.28 15.0 2.53 NA 1.43 NA 1.30 5.27 <6.55 NA 2.43 0.12 Certified2-methylnaphthalene 1.21 2.16 2.12 <4.0 NA <2.0 <1.0 26.7 2.76 7.92 1.07 NA 1.01 NA 0.710 4.25 <3.59 1.50 1.25 0.09 Reference1-methylnaphthalene 0.624 1.23 0.871 <4.0 NA <2.0 <1.0 <71.2 <7.22 4.95 0.600 36.5 0.443 NA 0.416 2.64 <2.61 0.800 0.614 0.050 Referencebiphenyl 0.673 0.760 0.739 <4.0 NA <2.0 <1.0 <71.2 <7.22 3.32 <71.2 NA 0.457 NA 0.174 2.70 <4.11 NA 0.61 0.14 Reference2,6-dimethylnaphthalene 0.306 <0.6 <0.5 <4.0 NA <2.0 <1.3 <71.2 <7.22 3.47 0.579 NA 0.473 NA 0.325 3.05 <2.44 1.10 0.33 0.16 Referenceacenaphthylene 0.543 0.430 0.307 <4.0 NA <2.0 <1.3 <71.2 <7.22 6.60 1.14 NA 0.198 NA 0.678 2.64 <1.10 0.950 0.48 0.12 Referenceacenaphthene 2.89 0.360 0.725 <4.0 NA <2.0 <1.3 <71.2 <7.22 4.94 0.554 NA 0.365 NA 0.422 2.02 <4.21 0.650 0.274 0.054 Reference1,6,7-trimethylnaphthalene 0.422 NA 0.799 <4.0 NA <2.0 NA NA <7.22 4.67 DL NA 0.390 NA 0.351 4.62 <1.22 0.500 0.400 0.032 Referencefluorene 0.481 0.560 1.20 <4.0 NA <2.0 <1.3 <71.2 <7.22 6.04 <71.2 0.970 0.466 NA 0.475 3.93 <1.82 0.700 0.494 0.036 Certified

phenanthrene 2.68 2.51 3.08 10.6 NA 2.54 5.43 31.9 3.32 21.3 2.62 3.31 2.65 NA 1.82 4.35 3.01 2.70 2.58 0.11 Certifiedanthracene 0.538 0.540 0.896 <5.9 NA <2.0 1.73 15.8 1.64 15.6 15.80 2.03 0.551 NA 0.889 1.44 <2.26 NA 0.527 0.071 Certified

1-methylphenanthrene 1.04 NA 0.941 <5.9 NA <2.0 <1.3 <71.2 <7.22 9.59 <71.2 NA 0.822 NA 0.902 0.920 <2.42 1.00 0.98 0.13 Certifiedfluoranthene 17.3 17.8 20.9 24.5 NA 16.2 18.6 120 12.5 169 15.6 27.2 19.6 NA 14.7 17.6 19.1 20.6 17.10 0.70 Certified

pyrene 18.0 17.7 21.2 22.6 NA 19.7 19.1 132 13.7 176 17.0 20.8 20.2 NA 15.1 15.9 20.0 21.2 18.04 0.60 Certified

benz[a]anthracene 4.74 4.55 6.04 5.50 NA 4.25 4.62 48.7 5.05 56.5 4.51 NA 7.09 NA 2.59 7.05 5.27 5.15 4.74 0.53 Certified

chrysene 6.58 5.61 NA NA NA 10.2 11.7 87.8 9.11 98.3 87.77 NA NA NA 8.06 NA NA NA 6.3 1.0 Certifiedtriphenylene 4.56 5.01 NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 4.33 0.72 Certified

benzo[b ]fluoranthene 6.86 6.48 5.72 NA NA 6.38 7.34 80.1 8.31 79.5 80.07 0.855 7.19 NA 3.64 7.09 5.65 NA 6.46 0.59 Certifiedbenzo[j ]fluoranthene 3.07 2.73 2.44 NA NA NA NA NA NA NA NA NA NA NA 3.32 NA NA NA 2.99 0.29 Certifiedbenzo[k ]fluoranthene 3.16 3.09 3.08 <4.0 NA 2.31 4.86 22.7 2.35 24.0 3.48 14.3 NA NA NA NA NA 3.10 3.16 0.18 Certified

benzo[e]pyrene 10.4 9.79 9.07 10.2 NA 7.00 10.9 61.6 6.42 85.0 10.4 4.86 10.9 NA 7.53 8.83 10.0 11.3 10.3 1.1 Certifiedbenzo[a]pyrene 2.88 2.96 13.4 <5.9 NA <2.0 2.90 79.2 8.23 31.4 4.68 7.03 2.81 NA 1.38 3.30 <6.31 2.30 2.80 0.38 Certifiedperylene 1.04 1.11 NA <5.9 NA <2.0 <1.0 <71.2 <7.22 9.45 1.04 NA 1.15 NA 0.663 1.01 <3.67 1.00 0.99 0.14 Certifiedindeno[1,2,3-cd]pyrene 2.13 2.36 2.17 <5.9 NA <2.0 2.58 18.4 1.90 21.3 2.58 NA 2.68 NA 1.10 2.84 <6.13 1.85 2.14 0.11 Certifieddibenz[a,h]anthracene 0.333 0.490 0.356 <5.9 NA <2.0 <1.3 <71.2 <7.22 4.31 1.45 NA NA NA 0.289 NA <1.06 0.400 0.327 0.031 Certified

benzo[ghi]perylene 3.29 2.95 3.37 <5.9 NA <2.0 2.91 22.6 2.35 29.7 1.16 NA 3.80 NA 1.83 3.42 <3.95 2.50 3.12 0.33 Certifiedchrysene/triphenylene 13.9 12.6 9.76 13.9 11.8 11.9 7.60 10.6 1.2 Targetbenzo[b+j]fluoranthene 8.13 7.80benzo[b+a]fluoranthene 9.51benzo[j+k]fluoranthene 5.79 5.58 6.40dibenz[a,h+a,c]anthracene 0.660 1.17

*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 6. SRM 1974b: Laboratory mean three replicates and target values - pesticides

 ng/g wet basis (reported to three significant figures) Certificate Values

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20 conc 95%CL type

alpha-HCH (a-BHC) <0.2 NA <0.3 NA <1 <0.5 <0.5 <3.5 <0.722 0.320 NA 0.232 <0.434 0.0763 NA <0.423 NA < 0.1 no target Target

hexachlorobenzene <0.2 <0.4 <0.3 NA <1 <0.5 <0.4 <3.5 <0.722 0.220 DL NA <0.424 0.0983 NA <0.423 <0.062 0.0358no target Targetgamma-HCH (g-BHC,lindane) <0.2 NA <0.3 NA <1 <0.5 <0.4 <3.5 <0.722 0.173 DL 0.191 <0.425 0.0475 NA <0.423 0.890 0.0257no target Targetbeta-HCH (b-BHC) <0.2 NA <0.3 NA <1 <0.5 NA <3.5 <0.722 0.177 NA NA <1.15 <0.020 NA <0.423 NA 0.0310no target Targetheptachlor <0.2 NA 0.447 NA <1 <0.5 <0.3 <3.5 <0.722 0.773 DL 0.285 <0.426 0.0627 NA <0.423 0.108 0.0262 0.212 0.084 Referencealdrin <0.2 NA <0.3 NA <1 <0.5 <0.5 <3.5 <0.722 0.263 NA 0.0710 0.964 0.0593 NA <0.423 <0.012 < 0.1 no target Targetheptachlor epoxide <0.4 NA <0.3 NA <1 <0.5 <0.4 <3.5 <0.722 ND DL NA <0.426 0.0487 NA <0.423 0.294 < 0.1 no target Targetoxychlordane <0.4 <0.4 0.372 NA <1 <0.5 NA <3.5 <0.722 4.03 NA NA <1.15 <0.044 NA 2.11 NA 0.361 0.362 0.072 Referencegamma-chlordane 1.04 1.59 1.09 NA 1.25 0.927 0.654 16.9 1.76 11.4 NA 1.56 0.984 1.09 NA 0.750 NA 0.776 1.14 0.17 Certified2,4'-DDE <0.4 <0.7 0.234 NA NA <1.0 NA <3.5 <0.722 0.947 DL 1.68 <0.439 <0.118 NA 0.181 NA 0.258 0.336 0.044 Certified

endosulfan I <0.4 NA <0.3 NA NA <1.0 <0.4 <3.5 <0.722 ND NA 0.350 <1.14 <0.103 NA 41.8 <0.1 < 0.1 no target Target

cis-chlordane (alpha-chlordane 1.32 1.52 1.78 NA 0.938 1.03 1.48 10.1 1.04 12.4 1.36 0.898 1.12 1.02 2.16 1.12 2.97 1.02 1.36 0.10 Certified

trans-nonachlor 1.32 1.53 1.25 NA 0.538 0.798 1.12 10.7 1.12 12.8 1.17 1.59 1.07 1.49 2.19 0.800 1.22 0.946 1.30 0.14 Certifieddieldrin 0.595 NA 0.593 NA 0.324 <0.5 0.470 6.25 0.649 8.32 NA NA <1.12 0.185 NA 16.7 NA 0.444 0.62 0.13 Reference4,4'-DDE 4.36 3.96 3.96 NA 3.47 2.55 4.09 56.1 5.83 41.6 3.92 2.19 4.27 3.63 5.71 2.95 3.76 3.32 4.15 0.38 Certified2,4'-DDD 1.02 1.34 0.972 NA 0.801 1.39 0.721 <3.5 <0.722 12.6 1.11 0.490 0.870 0.745 NA 0.951 1.16 1.35 1.09 0.16 Referenceendrin <0.4 NA <0.3 NA <1 <0.5 <0.5 <3.5 <0.722 3.47 NA 0.375 NA <0.112 NA <4.23 NA < 0.09no target Target

endosulfan II <0.4 NA <0.3 NA NA <2.0 <0.7 <3.5 <0.722 20.3 NA NA <3.70 <0.577 NA <4.23 <0.1 < 0.1 no target Target4,4'-DDD 3.29 <0.6 3.23 NA 1.61 2.34 2.33 27.5 2.87 31.5 NA 1.90 5.07 2.27 4.80 2.25 3.26 2.69 3.34 0.22 Certified2,4'-DDT 0.894 3.91 1.01 NA 1.17 <1.0 <0.7 <3.5 <0.722 6.14 NA 1.98 <0.422 <1.42 NA <4.23 1.02 0.629 0.894 0.057 Referencecis-nonachlor 0.605 0.840 0.429 NA <1 <0.5 NA 5.79 0.600 9.20 NA 0.893 0.510 0.222 NA 0.349 NA 0.594 0.64 0.16 Reference4,4'-DDT 0.406 <0.5 4.41 NA 0.258 <1.0 NA 3.36 0.351 2.24 DL 2.09 0.465 <0.255 0.343 <4.23 0.359 0.251 0.396 0.096 Referencemirex <0.3 NA <0.3 NA <1 <1.5 <0.5 <3.5 <0.722 0.793 DL NA <0.429 0.0797 NA <0.423 <0.157 0.0361no target Targetendosulfan sulfate <0.3 NA <0.3 NA NA <2.0 NA <3.5 <0.722 ND NA NA <1.14 0.0370 NA <4.23 <0.1 < 0.11no target Targetchlorpyrifos <0.3 NA NA NA NA <1.0 NA NA NA 0.950 NA NA NA NA NA <0.423 NA < 0.1 no target Target

*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 7. SRM 1974b: Laboratory mean three replicates and target values - PCBs

 ng/g wet basis (reported to three significant figures) Certificate Values

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20 conc 95%CL type

PCB 8 0.352 0.390 0.365 <2.9 NA 0.235 <0.7 4.11 0.426 8.57 NA NA NA 0.323 NA <0.134 0.410 0.388 0.37 0.11 ReferencePCB 18 0.868 1.00 1.02 <1.3 NA 0.446 0.716 9.55 0.988 11.7 0.897 0.638 1.07 0.586 NA 0.933 0.853 0.796 0.84 0.13 CertifiedPCB 28 3.44 3.23 3.82 1.99 NA 2.82 3.40 27.2 2.83 41.5 NA NA 2.55 4.14 NA 8.34 3.31 3.03 3.43 0.25 CertifiedPCB 31 2.84 2.76 2.59 1.55 NA 2.71 NA 20.0 2.08 18.7 NA NA 5.04 3.01 NA NA NA 3.24 2.88 0.23 CertifiedPCB 44 3.73 3.75 3.99 2.65 NA 3.54 3.73 29.2 3.03 39.0 4.01 2.94 3.75 5.58 9.11 4.26 3.84 3.35 3.85 0.20 CertifiedPCB 49 5.71 5.28 5.96 4.32 NA 3.54 NA 20.8 2.15 71.4 5.42 3.58 4.98 4.13 10.3 4.96 NA 5.38 5.66 0.23 CertifiedPCB 52 6.42 6.50 6.73 4.33 NA 5.69 5.84 42.3 4.41 73.7 6.13 3.89 6.51 5.31 13.4 6.83 6.64 5.76 6.26 0.37 CertifiedPCB 66 6.52 6.29 7.16 3.56 NA 5.61 6.58 68.4 7.13 64.9 NA 8.18 7.15 7.18 13.1 6.70 6.33 5.31 6.37 0.37 CertifiedPCB 95 6.15 6.29 5.14 5.17 NA 5.65 NA 44.1 4.58 67.9 NA 2.77 5.85 5.54 NA 6.61 NA 4.94 6.04 0.36 CertifiedPCB 99 5.92 5.67 6.17 3.68 NA 5.20 NA 36.9 3.84 71.6 6.11 3.25 6.15 6.57 NA 6.09 NA 5.50 5.92 0.27 CertifiedPCB 101 11.2 10.3 11.4 7.86 NA 10.5 8.67 84.2 8.75 114 10.5 5.38 11.1 10.2 16.5 13.4 13.4 9.83 10.7 1.1 CertifiedPCB 105 4.13 4.01 3.61 <3.4 NA 3.64 3.92 32.8 3.41 44.3 NA NA 4.73 4.24 5.92 4.61 3.65 3.21 4.00 0.18 CertifiedPCB 118 10.3 9.36 9.79 8.45 NA 9.76 9.80 83.9 8.72 122 NA 6.05 10.6 11.1 14.1 12.3 10.4 10.3 10.3 0.4 CertifiedPCB 128 1.78 1.79 1.43 1.73 NA 1.63 1.71 18.0 1.87 20.6 NA 1.13 1.90 1.64 2.37 1.77 2.15 1.35 1.79 0.12 CertifiedPCB 138 9.57 9.30 6.59 6.97 NA 11.4 9.00 87.6 9.11 127 NA NA 13.4 12.0 14.4 12.2 13.6 10.4 9.2 1.4 Certified

PCB 149 7.17 6.63 6.41 5.44 NA 6.20 NA 46.9 4.87 71.1 NA 4.95 7.08 7.29 NA 6.47 NA 4.20 7.01 0.28 CertifiedPCB 153 12.3 14.0 11.5 7.90 NA 10.5 11.4 80.2 8.34 164 NA NA 15.6 11.5 19.2 11.7 11.2 15.5 12.3 0.8 CertifiedPCB 156 0.753 0.700 0.571 0.935 NA 0.561 NA 10.2 1.05 21.8 7.75 NA 0.792 0.841 NA 0.720 NA 0.822 0.718 0.080 Certified

PCB 170 0.274 0.210 <0.3 <1.1 NA <0.2 <0.5 1.69 0.175 5.89 NA NA <0.426 0.207 0.473 0.356 0.464 0.320 0.269 0.034 Certified

PCB 180 1.09 1.15 0.936 <0.87 NA 1.04 1.27 10.2 1.06 33.4 1.09 1.20 1.15 1.12 1.77 1.12 1.24 1.23 1.17 0.10 CertifiedPCB 187 2.89 2.71 2.34 2.00 NA 2.56 3.60 23.4 2.43 32.1 NA NA 2.76 2.57 3.74 2.66 2.41 2.50 2.94 0.15 CertifiedPCB 194 <0.2 <0.2 <0.3 <0.60 NA <0.2 NA 0.454 0.0473 1.01 DL 0.110 <0.431 0.0555 NA <0.134 NA 0.0640no target Target

PCB 195 <0.2 <0.2 <0.3 <0.46 NA <0.2 <0.5 <3.57 <0.722 1.14 NA NA <0.432 0.0130 NA <0.134 <0.12 < 0.11no target TargetPCB 206 <0.2 <0.1 <0.3 <0.51 NA <0.2 <0.5 <3.57 <0.722 0.583 DL 0.0763 <0.428 0.0115 NA <0.134 <0.098 0.0361no target TargetPCB 209 <0.2 <0.1 <0.3 <0.51 NA <0.2 <0.5 <3.57 <0.722 0.383 DL 0.0323 <0.427 0.0110 NA <0.134 <0.1 < 0.1 no target Target

*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 8. Marine Sediment XII (QA03SED12): Laboratory means of three replicates and exercise assigned values - Water and PAHs 

 (reported to three significant figures) Exercise Assigned

Laboratory No. 1a 1b 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20 Value s %RSD 95% CL

Water (percent) 45.4 NA 45.1 44.0 45.7 49.0 54.6 45.0 43.9 43.7 45.2 44.4 43.3 44.3 45.5 43.9 45.0 44.9 43.7 44.7 44.7 45.5 2.7 5.9 1.5TOC (percent) NA NA NA NA 3.21 NA NA NA NA 1.82 NA 2.74 NA NA NA NA NA NA 2.40 NA 3.02 2.59 0.71 27.2 0.88PAHs ng/g dry basis (reported to three significant figures) Exercise Assigned

Laboratory No. 1a 1b 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20 Value s %RSD 95% CL

naphthalene 121 109.0 118 49.5 137 64.4 151 75.1 102 23.3 31.7 142 50.4 158 NA 120 NA 62.4 81.0 211 109 117 39 33.6 22

2-methylnaphthalene 79.2 75.0 82.5 35.9 83.0 NA 96.3 58.0 70.2 19.1 31.87 101 DL 83.3 110 106 NA 49.4 55.6 158 78.5 80.6 29.3 36.4 16.21-methylnaphthalene 49.0 48.1 50.8 26.8 61.2 NA 50.0 43.1 40.9 13.1 ND 69.5 DL 55.6 82.0 61.8 NA 38.1 39.1 102 50.0 54.2 16.5 30.5 9.6

biphenyl 29.2 27.0 21.8 17.2 55.4 NA 34.3 28.4 27.3 8.45 ND 25.5 DL 28.0 19.9 30.0 NA 19.2 20.1 66.5 32.0 28.2 9.3 32.8 5.3

2,6-dimethylnaphthalene 35.2 25.3 22.4 27.6 NA 96.7 21.0 25.0 48.0 16.3 ND 52.7 DL 43.9 NA 61.3 NA 37.2 38.5 73.3 42.5 39.7 19.9 50.2 12.0

acenaphthylene 29.6 13.9 15.7 33.1 25.8 131.0 59.0 12.8 48.5 62.3 41.6 73.5 100 93.8 63.8 20.0 NA 48.6 64.8 74.3 99.0 52.0 34.5 66.4 18.4

acenaphthene 34.7 36.8 37.0 26.0 46.2 38.9 38.3 33.0 33.9 15.8 32.0 49.3 57.3 74.3 45.8 38.1 NA 23.9 31.0 49.9 39.7 37.1 7.4 20.0 4.1

1,6,7-trimethylnaphthalene 25.7 NA 29.3 24.4 NA NA 31.7 NA NA NA ND 39.1 DL NA NA 35.1 NA 23.2 31.4 53.3 17.6 28.6 6.6 23.1 5.1

fluorene 65.5 50.6 84.4 41.5 86.3 62.4 52.7 60.1 55.3 27.2 49.7 87.3 97.9 79.9 308 58.0 NA 37.8 57.8 68.2 54.3 62.6 15.2 24.3 8.1

phenanthrene 539 471 488 418 505 513 618 315 490 357 424 475 634 563 46.0 593 NA 394 403 733 561 505 100 19.7 53anthracene 172 95.0 105 104 121 267 161 63.5 133 139 96.3 268 296 154 856 138 NA 96.2 94.8 168 215 147 60 40.9 32

1-methylphenanthrene 69.4 NA 65.5 61.6 NA 72.6 51.7 82.4 73.3 46.1 ND 86.7 NA 77.7 NA 92.2 NA 53.1 42.8 93.1 65.3 70.5 15.2 21.6 8.8fluoranthene 1094 967 993 984 1069 1079 1263 613 1117 796 1062 1053 1523 1197 215 1283 NA 881 958 1507 1197 1070 203 18.9 112pyrene 1129 960 980 1050 1174 1103 1267 626 1150 802 1047 1123 1563 1237 14.0 1383 NA 899 827 1530 1137 1099 216 19.6 115benz[a]anthracene 378 410 364 369 443 486 508 250 352 493 419 652 770 454 14.9 575 NA 348 336 546 556 442 105 23.7 54chrysene 547 477 NA NA 584 875 1130 410 678 677 805 871 NA 840 NA NA NA NA NA NA NA 640 170 26.6 142

triphenylene 141 122 NA NA 170 NA NA NA NA NA ND NA NA NA NA NA NA NA NA NA NA 144 24 16.6 60

benzo[b ]fluoranthene 1089 585 696 NA 855 1087 1320 262 1270 1293 1001 1643 NA 1040 NA 1210 NA 832 748 1098 NA 999 358 35.8 207benzo[j ]fluoranthene 281 275 283 NA NA NA NA NA NA NA ND NA NA NA NA NA NA NA NA NA NA 280 4 1.5 11benzo[k ]fluoranthene 406 285 290 475 453 795 NA 217 422 391 1005 449 499 759 NA NA NA NA NA NA 531 392 98 25.0 70

benzo[e]pyrene 590 461 549 660 650 NA 743 298 506 606 ND 769 746 700 1834 933 NA 612 494 902 938 657 186 28.3 107

benzo[a]pyrene 636 653 659 610 525 707 1327 361 640 610 691 1137 1110 659 225.2 865 NA 586 474 906 849 718 238 33.2 123

perylene 184 182 NA 185 295 NA 286 132 105 343 ND 182 225 170 2067 301 NA 181 132 274 234 211 60 28.6 36

indeno[1,2,3-cd]pyrene 608 697 578 555 577 752 766 335 405 692 623 1143 760 699 374 881 NA 540 481 820 942 680 214 31.5 118

dibenz[a,h]anthracene 112 142 59.2 111 99.1 181 203 48.2 125 239 194 277 136 173 NA NA NA 123 NA NA 168 137 66 48.3 44

benzo[ghi]perylene 488 603 478 524 592 657 931 313 290 545 683 938 243 624 219 823 NA 470 414 817 821 608 200 32.9 103

chrysene+triphenylene 697 715 1240 1010 715 592 1090 901 817 185 22.6 154

benzo[b]+[j]fluoranthene 912 1448

benzo[j]+[k]fluoranthene 1310 1045 671 536 1151 943 327 34.7 406benzo[b]+[a]fluoranthene 1357dibenz[a,h]+[a,c]anthracene 206 111 137

Note: Bolded values were not used in the calculation of the exercise assigned value.
Table 9. Marine Sediment XII (QA03SED12): Laboratory means of three replicates and exercise assigned values - Pesticides

 ng/g dry basis (reported to three significant figures) Exercise Assigned

Laboratory No. 1a 1b 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20 Value s %RSD 95% CL

alpha-HCH (a-BHC) <1 NA <0.3 NA NA <1.0 <1.40 NA <0.5 0.360 ND 0.310 NA <0.217 0.137 <0.573 0.230 DL 6.51 NA <0.45 <2

hexachlorobenzene 0.300 0.420 <0.3 NA NA 7.2 <1.50 NA <1.0 0.384 ND 0.510 0.484 0.476 NA NA 1.01 0.260 <0.709 0.242 0.194 0.315 0.123 39.0 0.153

gamma-HCH (g-BHC,lindane) <1 NA <0.3 NA NA <1.0 <1.40 NA <0.5 <1.66 ND NA DL <0.285 0.123 <0.562 0.341 DL <0.709 2.60 <0.52 <3

beta-HCH (b-BHC) <1 NA <0.3 NA NA <1.0 <1.40 NA <1.0 <1.66 ND 0.163 NA <0.309 NA <0.579 0.156 DL <0.709 NA <0.65 <2heptachlor <1 NA <0.3 NA NA <1.0 <1.50 NA <1.0 <1.66 ND NA DL 0.586 0.857 <0.563 0.225 DL <0.709 0.352 <0.56 <2

aldrin <1 NA <0.3 NA NA <1.0 <1.50 NA <1.0 <1.66 ND 1.03 NA <0.155 0.028 <0.569 0.126 DL <0.709 0.155 <0.43 <2

heptachlor epoxide <1 NA <0.3 NA NA <1.0 <1.40 NA <1.0 <1.66 ND NA DL <0.128 NA <0.563 0.205 DL <0.709 0.269 0.198 <2oxychlordane <1 <0.3 <0.3 NA NA <1.0 <1.40 NA <1.0 <1.66 ND 0.190 NA <0.134 NA 10.4 <0.053 DL <7.09 NA 0.391 <2gamma-chlordane 0.450 <0.5 <0.3 NA NA 1.25 <1.40 NA <1.0 1.54 ND NA NA <0.227 0.104 0.483 0.744 DL 0.291 NA 0.510 0.753 0.466 62.0 0.431

2,4'-DDE <1 <0.9 0.588 NA NA <4.6 <6.48 NA <1.5 <1.66 ND 0.610 8.84 <0.446 10.1 1.25 0.912 DL <0.709 NA 0.548 0.782 0.299 38.3 0.371endosulfan I <1 NA <0.3 NA NA <1.0 <1.40 NA <1.5 <1.66 ND NA NA NA NA <1.52 <0.101 DL <7.09 0.174 <0.52 <2cis-chlordane (alpha-chlordane 0.775 <0.6 0.776 NA NA <1.0 <1.40 NA <1.0 0.317 ND 1.30 0.561 <0.6 0.066 0.386 0.701 0.420 0.285 5.63 0.469 0.639 0.326 51.0 0.273

trans-nonachlor 0.290 <0.4 <0.3 NA NA <1.0 <1.65 NA <1.0 <1.66 ND NA 0.390 <0.191 1.51 <0.566 0.466 DL 0.148 1.16 0.178 0.271 0.144 53.1 0.229dieldrin 0.576 NA 0.881 NA NA <1.0 <1.40 NA <1.0 1.91 ND 1.16 NA <0.964 NA <1.50 0.627 1.31 <0.709 NA 0.390 0.978 0.523 53.5 0.4844,4'-DDE 6.53 3.30 3.37 NA NA 4.7 11.2 NA 5.70 15.3 ND 5.69 8.84 2.38 4.52 9.83 7.25 6.93 4.80 7.45 7.64 7.30 3.28 44.8 1.98

2,4'-DDD 5.37 3.47 3.76 NA NA E6.2 5.42 NA 5.75 <1.66 ND 11.0 DL <0.239 2.80 9.73 5.49 8.55 4.79 NA 12.9 6.93 3.12 45.0 2.10endrin <1 NA <0.3 NA NA <2.0 <1.40 NA <1.0 <1.66 ND 0.783 NA <0.947 0.200 NA <0.320 DL <7.09 NA <0.83 <2

endosulfan II <1 NA <0.3 NA NA NA <1.40 NA <2 <1.66 ND 16.9 NA NA NA <1.55 <0.549 DL <7.09 < 0.1 <0.52 <24,4'-DDD 13.4 5.28 12.4 NA NA 14 15.7 NA 16.9 14.5 ND 19.4 NA 16.0 8.85 NA 18.5 17.6 12.6 11.0 17.0 15.3 2.8 18.1 1.9

2,4'-DDT 4.72 13.8 5.36 NA NA 3.00 4.19 NA 4.06 <1.66 ND 5.10 NA 6.23 0.607 8.51 4.90 7.88 4.08 4.67 3.41 5.09 1.61 31.7 0.93

cis-nonachlor 0.490 <0.2 <0.3 NA NA <1.0 <1.40 NA <1 1.81 ND 2.23 NA <0.196 5.15 <0.576 <0.342 DL <0.709 NA 0.986 1.38 0.79 57.1 1.254,4'-DDT 13.7 20.4 11.3 NA NA 14 16.6 NA 17.5 17.9 ND 17.2 DL 40.2 13.0 27.2 25.2 30.9 25.5 10.9 12.5 18.6 6.3 34.0 3.7

mirex <1 NA <0.3 NA NA <1.0 <1.50 NA <2 <1.66 ND NA DL <0.397 NA 5.62 0.105 DL <0.709 0.239 <0.62 <2endosulfan sulfate <1 NA <0.3 NA NA NA <1.40 NA <2 <1.66 ND NA NA NA NA <0.572 0.104 DL <7.09 4.25 <0.84 <2chlorpyrifos <1 NA NA NA NA NA NA NA <2 NA ND NA NA NA NA NA NA 1.31 <0.709 9.54 <0.52 <2

Note: Bolded values were not used in the calculation of the exercise assigned value.
Table 10. Marine Sediment XII (QA03SED12): Laboratory means of three replicates and exercise assigned values - PCBs

 ng/g dry basis (reported to three significant figures) Exercise Assigned

Laboratory No. 1a 1b 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20 Value s %RSD 95% CL

PCB 8 0.902 0.823 1.01 0.826 NA NA <1.50 NA 1.13 1.51 ND 3.25 NA <0.424 2.77 NA 1.01 2.24 <0.185 1.97 1.02 1.43 0.77 53.8 0.55

PCB 18 3.47 2.46 3.09 3.84 NA NA 2.26 NA 2.96 3.73 ND 4.28 0.906 <0.485 2.49 4.60 1.54 4.53 2.50 1.54 2.89 3.12 1.01 32.2 0.58PCB 28 4.91 2.77 3.64 3.54 NA NA 4.61 NA 4.44 4.33 ND 6.23 NA <0.182 NA 5.95 4.85 4.96 7.22 5.82 4.33 4.75 1.19 25.0 0.75

PCB 31 5.11 2.70 4.66 2.96 NA NA NA NA 4.63 4.99 ND 4.09 NA <0.258 NA 6.64 2.78 NA NA NA 6.50 4.51 1.41 31.4 1.01PCB 44 6.73 6.40 7.84 7.40 NA NA 9.64 NA 9.33 10.1 ND 13.5 9.26 <0.689 9.11 11.0 5.20 11.8 7.88 10.6 9.74 9.09 2.30 25.3 1.39PCB 49 5.05 4.40 5.22 7.03 NA NA NA NA 7.50 5.05 ND 9.55 6.31 <0.285 5.83 8.01 2.75 7.31 5.07 NA 7.55 6.21 1.91 30.7 1.21PCB 52 13.5 12.3 12.9 11.6 NA NA 16.7 NA 16.1 14.3 ND 26.6 15.2 17.5 12.8 20.6 8.97 18.2 14.6 20.4 18.9 16.1 4.6 28.3 2.8PCB 66 5.87 5.23 7.64 6.09 NA NA 9.13 NA 9.22 11.6 ND 9.86 NA 8.59 14.3 12.3 5.49 8.06 8.39 10.2 9.28 8.46 2.22 26.3 1.34

PCB 95 18.4 19.7 8.43 20.9 NA NA NA NA 27.2 19.3 ND 44.7 NA 27.3 17.6 35.6 13.5 NA 21.7 NA 27.9 23.4 10.1 43.3 6.8

PCB 99 3.77 7.59 <0.3 8.91 NA NA NA NA 13.7 9.72 ND 21.7 14.0 14.2 9.13 16.6 7.03 NA 10.4 NA 15.2 11.5 5.3 46.4 3.8

PCB 101 24.9 23.3 25.2 24.8 NA NA 37.5 NA 37.4 37.2 ND 57.5 36.7 34.0 22.2 42.5 13.1 36.7 35.7 48.5 45.0 34.9 11.7 33.5 6.8PCB 105 8.56 7.39 6.94 17.4 NA NA 14.2 NA 12.6 12.3 ND 21.9 NA 10.0 NA 16.7 6.22 11.0 11.4 9.50 12.0 12.2 4.5 37.2 2.7

PCB 118 22.9 15.4 17.4 21.8 NA NA 32.8 NA 33.1 28.5 ND 49.7 NA 32.5 22.3 40.6 14.8 27.2 27.6 19.4 34.9 27.6 10.0 36.4 6.1

PCB 128 4.66 5.25 4.8 6.34 NA NA 9.39 NA 9.14 7.85 ND 10.1 NA 6.53 8.25 11.8 3.69 9.97 8.17 6.12 8.30 7.65 2.50 32.7 1.51

PCB 138 34.0 22.5 18.9 31.0 NA NA 47.2 NA 59.6 43.6 ND 80.4 NA 37.4 NA 70.5 23.1 43.3 41.4 48.2 50.2 36.7 11.3 30.9 7.6

PCB 149 20.7 20.7 20.4 20.4 NA NA NA NA 33.8 25.2 ND 41.3 NA 26.3 26.9 43.5 17.3 NA 24.4 NA 24.6 26.6 8.9 33.6 6.0

PCB 153 39.0 31.3 22.7 27.1 NA NA 40.9 NA 40.5 28.8 ND 73.2 NA 43.0 NA 70.6 17.1 55.6 29.9 24.3 67.7 41.5 19.2 46.3 11.6PCB 156 2.46 3.14 2.64 4.71 NA NA NA NA 5.52 7.01 ND 14.1 5.31 <0.344 NA 7.51 2.67 NA 4.55 NA 4.13 4.43 1.80 40.7 1.29

PCB 170 9.18 6.79 5.41 8.86 NA NA 13.7 NA 11.4 10.2 ND 16.4 NA 13.4 NA 16.2 4.54 10.1 9.70 13.4 4.34 9.11 3.75 41.2 2.52

PCB 180 14.7 13.7 12.4 13.8 NA NA 24.7 NA 22.8 26.4 ND 28.1 26.4 28.9 27.8 28.7 10.0 19.4 16.0 16.0 20.9 19.1 6.2 32.4 3.7PCB 187 9.02 7.24 6.70 7.93 NA NA 13.8 NA 12.4 13.1 ND 19.7 NA 11.0 NA 16.4 4.90 11.0 9.93 14.2 13.5 10.8 3.5 32.1 2.1

PCB 194 2.16 2.63 2.22 2.64 NA NA NA NA 5.23 4.32 ND 8.06 5.16 5.06 5.77 7.47 2.40 NA 2.70 NA 2.57 3.86 2.16 55.9 1.45PCB 195 1.58 1.19 2.23 1.03 NA NA 2.09 NA 1.97 1.98 ND 3.68 NA 1.55 NA 2.34 0.959 2.14 1.31 1.27 3.13 1.79 0.63 35.3 0.40

PCB 206 2.27 1.190 0.865 1.42 NA NA 3.58 NA 3.45 4.26 ND 2.94 3.42 NA 5.43 3.90 0.926 4.06 1.65 2.21 2.89 2.57 1.25 48.5 0.75

PCB 209 1.12 0.549 0.398 0.915 NA NA 2.12 NA 2.37 3.74 ND 2.63 2.07 NA 1.30 2.06 0.373 3.37 1.09 1.05 0.935 1.62 1.10 67.5 0.63

Note: Bolded values were not used in the calculation of the exercise assigned value.
Table 11. SRM 1941b: Laboratory mean three replicates and target values - water, TOC, and PAHs

Laboratory No. 1a 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20

Water (percent) 2.21 2.29 NA NA NA NA NA NA 2.58 NA 0.00 NA <1 NA 49.5 NA NA NA NA 2.20TOC (percent) NA NA NA NA NA NA NA NA 3.09 NA 4.24 NA NA NA NA NA NA 4.20 NA NA

1941a 1944 1944 1944 1944

 ng/g dry basis (reported to three significant figures) Certificate Values

Laboratory No. 1a 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20 conc 95%CL type

naphthalene 874 919 357 NA 478 1910 1217 634 157 195 792 NA 870 NA 896 NA 755 917 1253 1010 848 95 Certified2-methylnaphthalene 284 325 116 NA NA 1011 925 265 62 149 250 NA 303 NA 329 NA 415 621 420 289 276 53 Reference1-methylnaphthalene 121 142 59.6 NA NA 441 582 102 32 ND 119 NA 143 NA 126 NA 256 425 189 123 127 14 Referencebiphenyl 70.0 67.0 38.1 NA NA 264 716 63.7 19.4 ND 54.6 NA 74.5 NA 72.3 NA 132 170 132 83.4 74.0 8.0 Reference2,6-dimethylnaphthalene 74.0 64.5 60.6 NA 96.9 309 331 98.6 29.9 ND 101 NA 107 NA 124 NA 414 660 159 89.3 75.9 4.5 Referenceacenaphthylene 56.8 39.4 39.1 NA 71.7 855 335 62.6 43.3 481 72.3 NA 87.3 NA 46.8 NA 500 1061 105 71.4 53.3 6.4 Referenceacenaphthene 35.9 40.2 21.7 NA 21.8 377 507 32.3 13.2 221 42.9 NA 45.2 NA 37.0 NA 219 363 45.2 39.3 38.4 5.2 Reference1,6,7-trimethylnaphthalene 22.7 36.1 25.7 NA NA 343 NA NA NA ND 34.1 NA NA NA 34.9 NA 279 573 59.3 22.4 25.5 5.1 Referencefluorene 85.6 125 50.7 NA 55.7 488 804 67.5 28.5 397 99.4 NA 65.6 NA 76.1 NA 258 528 83.8 78.4 85 15 Certifiedphenanthrene 433 423 298 NA 334 5160 4787 339 195 3428 356 NA 493 NA 453 NA 3263 6070 544 459 406 44 Certifiedanthracene 182 175 132 NA 158 1423 1657 149 95.1 655 254 NA 163 NA 203 NA 718 1443 242 213 184 18 Certified1-methylphenanthrene 71.8 70.5 50.6 NA 40.9 1036 1570 63.9 34.4 ND 79.2 NA 70.9 NA 78.4 NA 830 1520 88.8 59.0 73.2 5.9 Certifiedfluoranthene 638 664 513 NA 500 6713 7543 504 379 6656 584 NA 943 NA 712 NA 5709 13033 786 757 651 50 Certifiedpyrene 565 527 467 NA 403 5943 8103 402 318 6572 499 NA 705 NA 604 NA 6147 8967 644 610 581 39 Certifiedbenz[a]anthracene 326 323 237 NA 257 3943 4323 258 265 3310 323 NA 423 NA 390 NA 2970 4897 388 347 335 25 Certifiedchrysene 312 NA NA NA 332 6193 4850 250 275 4280 285 NA 572 NA NA NA NA NA NA NA 291 31 Certifiedtriphenylene 111 NA NA NA NA NA NA NA NA ND NA NA NA NA NA NA NA NA NA NA 108 5 Certified

benzo[b ]fluoranthene 463 460 NA NA 364 4100 3883 460 484 2949 588 NA 724 NA 520 NA 2720 4240 574 NA 453 21 Certifiedbenzo[j ]fluoranthene 221 173 NA NA NA NA NA NA NA ND NA NA NA NA NA NA NA NA NA NA 217 5 Referencebenzo[k ]fluoranthene 226 165 226 NA 336 NA 2510 158 146 3358 176 NA 605 NA NA NA NA NA NA 208 225 18 Certified

benzo[e]pyrene 313 335 292 NA NA 2607 3017 176 212 ND 262 NA 538 NA 398 NA 2293 3070 416 409 325 25 Certifiedbenzo[a]pyrene 362 368 232 NA 246 5063 4067 378 248 2795 361 NA 496 NA 360 NA 2558 3580 393 383 358 17 Certifiedperylene 412 NA 273 NA NA 909 1153 155 199 ND 354 NA 304 NA 492 NA 642 799 537 451 397 45 Certifiedindeno[1,2,3-cd]pyrene 360 531 240 NA 268 2520 2933 211 278 1875 352 NA 528 NA 380 NA 1854 1777 377 415 341 57 Certifieddibenz[a,h]anthracene 56.3 32.9 50.3 NA 64.7 693 465 66.2 93.8 713 77.3 NA 101 NA NA NA 524 NA NA 65.4 53 10 Certifiedbenzo[ghi]perylene 327 304 225 NA 240 3447 2990 155 245 2205 277 NA 466 NA 304 NA 1791 1253 290 325 307 45 Certifiedchrysene+triphenylene 458 339 490 4007 6180 506 459 400 36 Targetbenzo[b]+[j]fluoranthene 405 498benzo[j]+[k]fluoranthene 4260 494 2686 3393 496 442 23 Targetbenzo[b]+[a]fluoranthenedibenz[a,h]+[a,c]anthracene 82.9 424 117
Table 12. SRM 1941b: Laboratory mean three replicates and target values - pesticides

 ng/g dry basis (reported to three significant figures) 1941a 1944 1944 1944 1944

Laboratory No. 1a 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20 conc 95%CL type

alpha-HCH (a-BHC) <1 <0.3 NA NA <1.0 <2.00 NA <0.5 <0.95 ND 0.423 NA <0.0716 NA <0.437 0.077 NA <0.647 NA <0.45 no target Target

hexachlorobenzene 5.63 6.27 NA NA 7.07 6.72 NA 6.26 3.15 ND 8.10 NA 32.5 NA NA 9.34 5.84 5.99 5.57 7.53 5.83 0.38 Certifiedgamma-HCH (g-BHC,lindane) <1 <0.3 NA NA <1.0 <2.00 NA <0.5 <0.95 ND NA NA <0.0942 NA <0.428 0.141 NA <0.647 0.179 <0.65 no target Targetbeta-HCH (b-BHC) <1 <0.3 NA NA <1.0 <2.00 NA <0.5 <0.95 ND NA NA <0.102 NA <0.457 0.057 NA <0.647 NA 0.250 no target Targetheptachlor <1 <0.3 NA NA <1.0 <2.10 NA <0.5 <0.95 ND 0.117 NA <0.079 NA <0.429 0.065 NA <0.647 0.646 0.142 no target Targetaldrin <1 <0.3 NA NA <1.0 <2.10 NA <0.5 <0.95 ND 0.083 NA <0.0512 NA 0.524 0.035 NA <0.647 0.351 <0.43 no target Targetheptachlor epoxide <1 <0.3 NA NA <1.0 <2.50 NA <0.5 <0.95 ND 0.087 NA <0.0422 NA <0.429 0.219 NA <0.647 0.146 0.425 no target Targetoxychlordane <1 <0.3 NA NA <1.0 <2.00 NA <0.5 <0.95 ND NA NA 1.91 NA 6.72 <0.053 NA <6.47 NA 0.708 no target Targetgamma-chlordane 0.586 0.53 NA NA E0.72 18.4 NA 0.622 0.672 ND 3.10 NA 12.2 NA 0.611 0.717 NA 30.0 NA 0.425 0.566 0.093 Certified

2,4'-DDE <1 0.470 NA NA <1.6 16.8 NA <1.0 <0.95 ND 0.150 NA 8.10 NA 0.557 0.308 NA 12.4 NA 0.239 0.38 0.12 Referenceendosulfan I <1 <0.3 NA NA <1.0 <2.00 NA <1.0 <0.95 ND NA NA NA NA <1.16 <0.101 NA <6.47 0.062 <0.52 no target Targetcis-chlordane (alpha-chlordane 0.869 0.870 NA NA E0.61 15.6 NA 0.570 0.355 ND 0.930 NA 9.92 NA 0.514 0.592 17.843 26.2 1.29 0.653 0.85 0.11 Certified

trans-nonachlor 0.441 0.300 NA NA E0.19 9.20 NA <0.5 0.15 ND 0.157 NA 5.39 NA <0.431 0.377 11.66 15.1 0.324 0.327 0.438 0.073 Certified

dieldrin <1 0.730 NA NA <1.0 12.5 NA <0.5 0.37 ND 0.710 NA 1.41 NA <1.14 0.547 NA <0.647 NA 0.631 no target Target4,4'-DDE 3.32 3.06 NA NA E1.3 62.5 NA 2.34 2.30 ND 2.41 NA 44.3 NA 4.25 2.75 NA 105 3.43 2.63 3.22 0.28 Certified2,4'-DDD <1 0.680 NA NA <1.0 34.2 NA <1.0 <0.95 ND 2.86 NA 26.6 NA 1.81 0.376 NA 41.0 NA 2.50 no target Targetendrin <1 <0.3 NA NA <2.0 <2.00 NA <0.5 <0.95 ND 0.323 NA <0.319 NA NA <0.320 NA <6.47 NA <0.83 no target Targetendosulfan II <1 <0.3 NA NA NA <2.00 NA <2 <0.95 ND 5.77 NA NA NA <1.18 <0.549 NA <6.47 < 0.1 <0.52 no target Target4,4'-DDD 4.73 4.19 NA NA 2.23 88.8 NA 3.38 1.75 ND 2.91 NA 80.5 NA NA 3.05 NA 205 4.66 3.37 4.66 0.46 Certified2,4'-DDT <1 <0.3 NA NA <2.0 3.06 NA <1.0 <0.95 ND 0.097 NA <0.0697 NA <0.425 <0.166 NA <6.47 < 0.144 <0.64 no target Target

cis-nonachlor <1 0.480 NA NA E0.44 3.97 NA <0.5 0.47 ND 0.297 NA 1.85 NA <0.439 0.213 NA 6.66 NA 0.370 0.378 0.053 Certified

4,4'-DDT 1.15 1.32 NA NA <2.0 142 NA <1.0 0.46 ND 0.813 NA 107 NA <0.427 1.26 158.68 297 1.42 1.05 1.12 0.42 Referencemirex <1 <0.3 NA NA <1.0 <2.10 NA <1.0 <0.95 ND NA NA <0.131 NA 2.63 0.073 NA <0.647 0.129 <0.62 no target Targetendosulfan sulfate <1 <0.3 NA NA NA <24.0 NA <2 <0.95 ND NA NA NA NA <0.436 0.135 NA <6.47 0.359 <0.84 no target Targetchlorpyrifos <1 NA NA NA NA NA NA <1.0 NA ND NA NA NA NA NA NA NA <0.647 1.36 0.860 no target Target
Table 13. SRM 1941b: Laboratory mean three replicates and target values - PCBs

 ng/g dry basis (reported to three significant figures) 1941a 1944 1944 1944 1944

Laboratory No. 1a 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20 conc 95%CL type

PCB 8 1.58 1.26 1.31 NA NA 23.6 NA 1.64 1.16 ND 2.36 NA 16.6 NA NA 2.10 20.5 29.4 0.832 1.87 1.65 0.19 CertifiedPCB 18 2.26 2.55 3.09 NA NA 49.6 NA 2.10 1.76 ND 2.11 NA 41.5 NA 2.99 1.61 47.6 61.9 1.04 2.98 2.39 0.29 CertifiedPCB 28 4.45 4.63 3.08 NA NA 83.5 NA 3.99 3.05 ND 5.01 NA 55.6 NA 5.31 8.25 77.4 203 7.21 4.52 4.52 0.57 CertifiedPCB 31 3.45 3.70 2.36 NA NA NA NA 3.43 3.76 ND 2.40 NA 53.7 NA 5.05 4.14 NA NA NA 3.80 3.18 0.41 CertifiedPCB 44 3.84 4.01 2.93 NA NA 55.9 NA 3.75 3.53 ND 3.61 NA 34.9 NA 4.23 5.22 66.1 97.0 4.61 3.61 3.85 0.20 CertifiedPCB 49 4.31 4.08 3.50 NA NA NA NA 3.92 3.00 ND 4.54 NA 36.0 NA 4.14 3.32 50.8 57.3 NA 4.39 4.34 0.28 CertifiedPCB 52 5.35 5.79 4.38 NA NA 64.2 NA 5.13 3.28 ND 6.30 NA 47.7 NA 5.93 5.48 86.2 112 6.25 6.15 5.24 0.28 CertifiedPCB 66 4.93 5.88 3.88 NA NA 53.7 NA 4.89 4.09 ND 5.09 NA 42.3 NA 6.24 6.46 60.3 86.3 4.63 5.33 4.96 0.53 CertifiedPCB 95 3.77 3.70 3.48 NA NA NA NA 3.99 4.25 ND 4.27 NA 30.2 NA 4.29 3.23 NA 63.0 NA 4.64 3.93 0.62 CertifiedPCB 99 2.88 0.780 2.12 NA NA NA NA 2.84 2.14 ND 4.13 NA 19.0 NA 3.24 2.97 NA 34.9 NA 2.50 2.90 0.36 CertifiedPCB 101 5.36 5.03 4.51 NA NA 57.3 NA 5.20 4.43 ND 6.10 NA 42.6 NA 6.25 3.34 95.3 96.0 5.95 5.25 5.11 0.34 CertifiedPCB 105 1.38 1.36 <2.1 NA NA 18.8 NA 1.51 0.808 ND 1.44 NA 17.2 NA 2.11 1.53 28.7 32.8 0.544 1.16 1.43 0.10 CertifiedPCB 118 4.27 4.26 3.90 NA NA 47.0 NA 4.21 3.16 ND 3.62 NA 37.5 NA 5.21 4.56 66.1 76.3 3.34 3.85 4.23 0.19 CertifiedPCB 128 0.702 0.640 1.34 NA NA 6.94 NA 0.672 0.379 ND 0.610 NA 6.63 NA 0.854 0.689 18.3 14.9 0.18 0.588 0.696 0.044 Certified

PCB 138 3.70 2.86 3.13 NA NA 52.9 NA 5.23 2.83 ND 5.95 NA 26.8 NA 6.35 4.92 73.1 81.5 1.81 3.95 3.6 0.28 CertifiedPCB 149 4.37 4.29 3.66 NA NA NA NA 4.23 2.98 ND 4.28 NA 28.3 NA 5.03 5.55 NA 65.1 NA 3.92 4.35 0.26 CertifiedPCB 153 5.31 5.40 6.78 NA NA 52.7 NA 5.00 2.73 ND 6.20 NA 53.9 NA 7.78 5.03 98.2 75.4 4.04 5.74 5.47 0.32 CertifiedPCB 156 0.521 0.380 0.562 NA NA NA NA 0.396 0.761 ND 3.05 NA 2.83 NA 0.600 0.520 NA 7.73 NA 0.500 0.507 0.090 Certified

PCB 170 1.29 1.14 1.40 NA NA 17.0 NA 1.26 0.693 ND 23.1 NA 12.6 NA 1.47 1.14 21.6 18.4 0.507 1.62 1.35 0.09 CertifiedPCB 180 3.44 2.98 2.58 NA NA 37.6 NA 3.07 2.25 ND 3.95 NA 35.8 NA 3.40 3.33 41.2 36.6 2.97 2.77 3.24 0.51 CertifiedPCB 187 2.26 2.01 2.14 NA NA 20.9 NA 2.14 1.74 ND 5.74 NA 13.0 NA 2.22 1.91 25.8 25.1 2.29 2.58 2.17 0.22 CertifiedPCB 194 1.09 0.820 0.674 NA NA NA NA 0.890 0.826 ND 1.64 NA 9.92 NA 1.30 1.16 NA 5.85 NA 0.824 1.04 0.06 CertifiedPCB 195 <1 0.760 0.271 NA NA 3.36 NA 0.245 0.240 ND 1.37 NA 2.57 NA <0.434 0.369 3.63 2.97 0.466 0.827 0.645 0.060 Certified

PCB 206 <2 2.15 1.75 NA NA 7.38 NA 2.47 1.61 ND 2.40 NA NA NA 2.69 2.71 9.44 3.75 1.19 2.26 2.42 0.19 CertifiedPCB 209 4.71 4.42 2.80 NA NA 6.09 NA 4.92 3.44 ND 5.16 NA NA NA 4.71 5.45 12.2 2.85 5.74 3.88 4.86 0.45 Certified
Table 14. Mussel Tissue XI (QA03TIS11): z scores (25% by laboratory) - PAHs and Water

 (z=+1 is 25% higher than the exercise assigned value; z=-1 is 25% lower than the exercise assigned value)

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20

Water (percent) 0.0 -0.1 0.0 0.0 0.0 0.0 0.0 -0.1 0.0 0.0 0.0 -0.3 0.0 0.0 0.1PAHs

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20

naphthalene -0.5 2.9 0.0 0.2 -1.4 139.0 8.5 26.9 0.5 -1.7 -1.8 6.02-methylnaphthalene 1.6 1.6 5.3 1.3 -1.0 58.6 1.5 55.9 -0.9 -1.1 -0.8 3.5 1.61-methylnaphthalene 1.0 0.6 4.1 -1.5 47.2 0.5 53.9 -1.2 79.0 -1.8 -0.9 3.2 0.4biphenyl -0.2 0.6 1.6 45.6 0.3 40.8 -0.1 -1.9 4.62,6-dimethylnaphthalene 0.1 -1.0 0.5 0.7 1.0 47.4 0.5 64.9 -1.3 0.1 0.1 2.8 -0.3 -0.7acenaphthylene -0.3 -0.7 51.5 0.8 142.5 3.1 -0.8 -0.2 6.2 2.0acenaphthene -1.2 2.8 24.3 -1.6 56.4 0.3 -1.4 -1.5 1.3 -0.51,6,7-trimethylnaphthalene 0.4 2.4 74.2 -1.6 0.6 -0.3 3.7 2.1 -1.2fluorene -0.9 -1.4 1.8 0.7 50.2 -0.6 -1.2 -2.0 2.4 -1.3phenanthrene 0.0 0.3 0.6 -0.9 -0.5 7.9 54.2 1.1 41.8 -0.3 -0.2 0.4 -1.0 0.4 0.5 0.1anthracene -0.1 3.1 69.6 2.4 103.1 0.3 0.1 -0.5 2.71-methylphenanthrene 0.6 1.0 -0.3 -0.6 0.9 32.2 -0.8 48.3 0.7 -1.3 -0.7 -0.3 0.0fluoranthene -0.1 0.2 0.7 -0.7 -0.5 0.5 31.7 -0.9 42.9 -0.7 1.9 0.5 -1.0 0.0 0.3 0.1pyrene 0.3 0.0 0.7 -0.5 -0.3 0.7 33.4 -0.7 47.7 -0.5 0.2 0.8 -0.8 -0.7 0.1 0.0benz[a ]anthracene -0.6 0.0 1.4 -1.1 0.4 0.4 41.4 0.0 52.9 -0.4 2.2 -1.0 1.8 0.7 0.1

chrysene -0.6 -0.5 1.1 2.5 50.1 0.7 60.0 0.5triphenylene 0.0 0.0benzo[b ]fluoranthene -0.2 0.1 -0.8 -0.2 1.0 53.9 1.1 62.9 0.5 -1.0 0.8 -0.1benzo[j ]fluoranthene -0.4 -0.4 -1.0 1.8

benzo[k ]fluoranthene -0.1 0.0 -0.5 -1.3 3.1 28.8 -1.1 28.1 0.2 2.6 -1.3

benzo[e ]pyrene -0.3 0.2 -0.5 -0.5 -1.2 1.1 34.2 -0.7 38.7 -0.2 -2.6 0.6 -0.6 0.0 0.3 0.8

benzo[a ]pyrene -1.1 -0.7 10.9 0.2 46.0 2.2 0.2 -1.7 2.3 -1.3perylene -1.0 0.8 0.4 41.6 -0.5 0.5 -1.6 1.9 -0.5indeno[1,2,3-cd ]pyrene -1.3 0.6 -1.0 0.5 27.8 -1.2 32.3 0.1 0.5 -1.7 3.7 -1.3dibenz[a,h ]anthracene 1.0 1.8 -1.6 42.0 12.6 -1.2 0.0benzo[ghi]perylene -1.3 0.9 -0.2 -0.2 27.2 -1.3 37.2 -2.6 0.8 -1.6 2.9 -1.2

chrysene/triphenylene 1.1 -0.6 -0.3 1.6 0.7 0.8 0.3benzo[b +j ]fluoranthene -0.5 0.5

benzo[b +a ]fluoranthene 0.0

benzo[j +k ]fluoranthene 0.2 0.2 -0.4

dibenz[a,h

+a,c ]anthracene -1.7 1.7

*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 15. Mussel Tissue XI (QA03TIS11): z scores (25% by laboratory) - Pesticides 

(A z-score (25%) = +1 if the laboratory’s submitted mean value is 25% higher than the exercise assigned value.)

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20

alpha-HCH (a-BHC)hexachlorobenzenegamma-HCH (g-BHC,lindane)aldrinheptachlor epoxideoxychlordane 0.5 41.7 206.1 -0.5endosulfan Icis-chlordane (alpha-chlordane) 0.1 1.3 0.6 -0.2 -0.8 1.5 33.5 -0.7 46.9 0.6 -1.1 0.1 0.0 0.3 -1.0 4.8 -1.4

trans-nonachlor 0.1 1.2 -0.2 -1.3 -1.0 -0.1 31.0 -0.9 48.1 -0.1 0.5 -0.2 2.0 0.3 -1.3 0.6 -1.5dieldrin 0.3 0.4 0.0 47.2 0.5 81.7 -1.4 -0.74,4'-DDE 0.1 0.5 0.8 -0.1 -1.0 0.3 67.4 2.3 50.9 0.4 -1.6 1.2 0.0 0.5 -0.3 0.4 -1.1endrinendosulfan II4,4'-DDD -0.1 1.7 -0.2 -2.0 -0.8 -0.3 43.3 0.2 44.1 -1.5 3.9 -1.2 0.6 -0.6 1.4 -1.02,4'-DDT -1.1 1.2 45.4 5.5 1.3 -1.4cis-nonachlor 0.0 2.5 -1.0 72.1 2.6 78.1 2.1 0.2 -2.4 -1.4 0.14,4'-DDT -0.4 1.5 23.5 42.9 0.1 39.3 4.0 1.3 -1.2 1.2 -0.3 -2.1mirexendosulfan sulfatechlorpyrifos

*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 16. Mussel Tissue XI (QA03TIS11): z scores (25% by laboratory) - PCBs 

(A z-score (25%) = +1 if the laboratory’s submitted mean value is 25% higher than the exercise assigned value.)

Laboratory No. 1a 1b 1c 2 4 7 8 9 9 rev* 11 12 14 15 16 17 18 19 20

PCB 8 -1.6 -1.3 -1.0 -1.7 26.9 -1.3 262.8 -1.2 5.5 1.0 0.2PCB 18 0.5 0.9 1.1 -1.3 -0.4 38.3 -0.3 61.5 -0.4 -1.2 1.3 -1.0 1.2 -0.1 -0.1 -0.4PCB 28 0.2 0.1 0.8 -0.8 -0.3 0.2 35.5 -0.5 55.0 -0.6 0.9 0.2 4.0 -0.3 -0.5PCB 31 0.6 -0.2 0.6 -1.3 0.2 20.3 -1.9 23.8 3.1 -0.1 0.1PCB 44 -0.1 0.1 0.4 -0.6 0.0 -0.2 35.9 -0.5 45.1 0.0 -1.1 0.1 2.0 0.2 0.1 0.0 -0.7PCB 49 1.4 0.3 1.9 -0.4 -0.5 14.7 -2.4 60.0 0.0 -1.1 0.1 -0.8 0.1 -0.6 -0.2PCB 52 0.2 0.6 1.0 -0.6 -0.1 -0.1 26.1 -1.4 55.4 -0.1 -1.4 0.6 -0.1 0.5 0.0 0.5 -0.5PCB 66 -1.0 0.0 0.4 -1.4 -0.2 0.3 45.6 0.3 42.7 0.5 0.6 0.8 0.2 -0.5 0.0 -1.0PCB 95 -1.3 0.5 0.0 0.8 0.3 32.9 -0.8 55.0 -1.5 0.3 0.2 -0.1 -0.8PCB 99 0.3 -0.2 1.7 -1.0 -0.2 20.7 -1.8 54.3 -0.2 -1.9 0.2 0.4 -0.5 -0.5PCB 101 0.2 0.0 0.9 -0.6 -0.1 -0.6 31.6 -0.9 50.9 -0.3 -2.0 0.3 -0.1 0.1 0.3 0.3 -0.5PCB 105 0.4 0.0 0.1 -0.1 0.2 36.4 -0.5 51.2 0.7 0.2 0.3 -0.1 -0.2 -1.5PCB 118 0.5 -0.3 -0.5 -0.3 0.1 -0.4 32.4 -0.8 52.6 -1.8 0.3 0.4 0.0 0.2 0.3 -0.3PCB 128 0.6 0.2 0.0 0.0 0.2 0.0 43.2 0.1 54.4 -1.4 0.4 -0.2 0.1 0.0 1.2 -1.2PCB 138 0.4 -0.5 -1.7 -0.9 0.6 -0.3 32.6 -0.8 53.2 1.1 0.4 0.3 -0.1 1.3 -0.4PCB 149 0.1 0.1 0.5 0.0 0.2 28.4 -1.2 51.3 -1.1 0.4 0.4 -0.6 -1.6PCB 170 -0.3 -1.5 33.7 -0.7 120.9 -1.5 1.0 0.5 3.3PCB 180 1.1 0.0 0.1 -0.2 -1.0 35.9 -0.5 191.9 -0.9 1.1 0.0 0.2 0.5 0.9 0.2 -1.4PCB 187 0.3 0.2 -0.1 -0.5 0.2 0.5 36.7 -0.4 54.2 0.2 0.1 0.4 -0.4 -0.5 -0.6PCB 194PCB 195PCB 206PCB 209

*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 17. Marine Sediment XII (QA03SED12): z scores (25% by laboratory) - PAHs, Water, and TOC 

(A z-score (25%) = +1 if the laboratory’s submitted mean value is 25% higher than the exercise assigned value.)

Laboratory No. 1a 1b 1c 2 3 1-b 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20

Water (percent) 0.0 0.0 -0.1 0.0 0.3 0.8 0.0 -0.1 -0.2 0.0 -0.1 -0.2 -0.1 0.0 -0.1 0.0 0.0 -0.2 -0.1 -0.1TOC (percent) 1.0 -1.2 0.2 -0.3 0.7PAHs

Laboratory No. 1a 1b 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20

naphthalene 0.1 -0.3 0.0 -2.3 0.7 -1.8 1.1 -1.4 -0.5 -3.2 -2.9 0.9 -2.3 1.4 0.1 -1.9 -1.2 3.2 -0.32-methylnaphthalene -0.1 -0.3 0.1 -2.2 0.1 0.8 -1.1 -0.5 -3.0 -2.4 1.0 0.1 1.4 1.3 -1.5 -1.2 3.9 -0.11-methylnaphthalene -0.4 -0.5 -0.3 -2.0 0.5 -0.3 -0.8 -1.0 -3.0 1.1 0.1 2.0 0.6 -1.2 -1.1 3.5 -0.3biphenyl 0.1 -0.2 -0.9 -1.6 3.8 0.9 0.0 -0.1 -2.8 -0.4 0.0 -1.2 0.2 -1.3 -1.2 5.4 0.52,6-dimethylnaphthalene -0.5 -1.5 -1.7 -1.2 5.7 -1.9 -1.5 0.8 -2.4 1.3 0.4 2.2 -0.2 -0.1 3.4 0.3acenaphthylene -1.7 -2.9 -2.8 -1.4 -2.0 6.1 0.5 -3.0 -0.3 0.8 -0.8 1.7 3.7 3.2 0.9 -2.5 -0.3 1.0 1.7 3.6acenaphthene -0.3 0.0 0.0 -1.2 1.0 0.2 0.1 -0.4 -0.3 -2.3 -0.6 1.3 2.2 4.0 0.9 0.1 -1.4 -0.7 1.4 0.31,6,7-trimethylnaphthalene -0.4 0.1 -0.6 0.4 1.5 0.9 -0.8 0.4 3.5 -1.5fluorene 0.2 -0.8 1.4 -1.3 1.5 0.0 -0.6 -0.2 -0.5 -2.3 -0.8 1.6 2.3 1.1 15.7 -0.3 -1.6 -0.3 0.4 -0.5phenanthrene 0.3 -0.3 -0.1 -0.7 0.0 0.1 0.9 -1.5 -0.1 -1.2 -0.6 -0.2 1.0 0.5 -3.6 0.7 -0.9 -0.8 1.8 0.4anthracene 0.7 -1.4 -1.1 -1.2 -0.7 3.3 0.4 -2.3 -0.4 -0.2 -1.4 3.3 4.1 0.2 19.3 -0.3 -1.4 -1.4 0.6 1.81-methylphenanthrene -0.1 -0.3 -0.5 0.1 -1.1 0.7 0.2 -1.4 0.9 0.4 1.2 -1.0 -1.6 1.3 -0.3fluoranthene 0.1 -0.4 -0.3 -0.3 0.0 0.0 0.7 -1.7 0.2 -1.0 0.0 -0.1 1.7 0.5 -3.2 0.8 -0.7 -0.4 1.6 0.5pyrene 0.1 -0.5 -0.4 -0.2 0.3 0.0 0.6 -1.7 0.2 -1.1 -0.2 0.1 1.7 0.5 -3.9 1.0 -0.7 -1.0 1.6 0.1benz[a ]anthracene -0.6 -0.3 -0.7 -0.7 0.0 0.4 0.6 -1.7 -0.8 0.5 -0.2 1.9 3.0 0.1 -3.9 1.2 -0.9 -1.0 0.9 1.0chrysene -0.6 -1.0 -0.3 1.5 3.1 -1.4 0.2 0.2 1.0 1.4 1.3triphenylene -0.1 -0.6 0.7benzo[b ]fluoranthene 0.4 -1.7 -1.2 -0.6 0.4 1.3 -3.0 1.1 1.2 0.0 2.6 0.2 0.8 -0.7 -1.0 0.4benzo[j ]fluoranthene 0.0 -0.1 0.1

benzo[k ]fluoranthene 0.1 -1.1 -1.0 0.8 0.6 4.1 -1.8 0.3 0.0 6.3 0.6 1.1 3.7 1.4benzo[e ]pyrene -0.4 -1.2 -0.7 0.0 0.0 0.5 -2.2 -0.9 -0.3 0.7 0.5 0.3 7.2 1.7 -0.3 -1.0 1.5 1.7benzo[a ]pyrene -0.5 -0.4 -0.3 -0.6 -1.1 -0.1 3.4 -2.0 -0.4 -0.6 -0.1 2.3 2.2 -0.3 -2.7 0.8 -0.7 -1.4 1.0 0.7perylene -0.5 -0.5 -0.5 1.6 1.4 -1.5 -2.0 2.5 -0.5 0.3 -0.8 35.2 1.7 -0.6 -1.5 1.2 0.4indeno[1,2,3-cd ]pyrene -0.4 0.1 -0.6 -0.7 -0.6 0.4 0.5 -2.0 -1.6 0.1 -0.3 2.7 0.5 0.1 -1.8 1.2 -0.8 -1.2 0.8 1.5dibenz[a,h ]anthracene -0.7 0.1 -2.3 -0.8 -1.1 1.3 1.9 -2.6 -0.4 3.0 1.7 4.1 0.0 1.1 -0.4 0.9benzo[ghi ]perylene -0.8 0.0 -0.9 -0.6 -0.1 0.3 2.1 -1.9 -2.1 -0.4 0.5 2.2 -2.4 0.1 -2.6 1.4 -0.9 -1.3 1.4 1.4chrysene+triphenylene -0.6 -0.5 2.1 0.9 -0.5 -1.1 1.3 0.4

benzo[j ]+[k ]fluoranthene 1.6 0.4 -1.2 -1.7 0.9
Table 18. Marine Sediment XII (QA03SED12): z scores (25%) by laboratory - Pesticides 

(A z-score (25%) = +1 if the laboratory’s submitted mean value is 25% higher than the exercise assigned value.)

Laboratory No. 1a 1b 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20

alpha-HCH (a-BHC)hexachlorobenzene -0.2 1.3 87.4 0.9 2.5 2.1 2.0 8.8 -0.7 -0.9 -1.5gamma-HCH (g-BHC,lindane)aldrinheptachlor epoxideoxychlordaneendosulfan Icis-chlordane (alpha-chlordane 0.9 0.9 -2.0 4.1 -0.5 -3.6 -1.6 0.4 -1.4 -2.2 31.2 -1.1

trans-nonachlor 0.3 1.8 18.3 2.9 -1.8 13.1 -1.4

dieldrin -1.6 -0.4 3.8 0.7 -1.4 1.4 -2.44,4'-DDE -0.4 -2.2 -2.2 -1.4 2.1 -0.9 4.4 -0.9 0.8 -2.7 -1.5 1.4 0.0 -0.2 -1.4 0.1 0.2endrinendosulfan II4,4'-DDD -0.5 -2.6 -0.8 -0.3 0.1 0.4 -0.2 1.1 0.2 -1.7 0.8 0.6 -0.7 -1.1 0.42,4'-DDT -0.3 6.9 0.2 -1.6 -0.7 -0.8 0.0 0.9 -3.5 2.7 -0.1 2.2 -0.8 -0.3 -1.3cis-nonachlor -2.6 1.2 2.5 10.9 -1.14,4'-DDT -1.1 0.4 -1.6 -1.0 -0.4 -0.2 -0.2 -0.3 4.6 -1.2 1.8 1.4 2.6 1.5 -1.7 -1.3mirexendosulfan sulfatechlorpyrifos
Table 19. Marine Sediment XII (QA03SED12): z scores (25% by laboratory) - PCBs 

(A z-score (25%) = +1 if the laboratory’s submitted mean value is 25% higher than the exercise assigned value.)

Laboratory No. 1a 1b 1c 2 3 4 5 6 7 9 10 11 12 13 14 15 16 17 18 19 20

PCB 8 -1.5 -1.7 -1.2 -1.7 -0.8 0.2 5.1 3.8 -1.2 2.3 1.5 -1.1PCB 18 0.5 -0.8 0.0 0.9 -1.1 -0.2 0.8 1.5 -2.8 -0.8 1.9 -2.0 1.8 -0.8 -2.0 -0.3PCB 28 0.1 -1.7 -0.9 -1.0 -0.1 -0.3 -0.4 1.2 1.0 0.1 0.2 2.1 0.9 -0.4PCB 31 0.5 -1.6 0.1 -1.4 0.1 0.4 -0.4 1.9 -1.5 1.8PCB 44 -1.0 -1.2 -0.5 -0.7 0.2 0.1 0.5 2.0 0.1 0.0 0.8 -1.7 1.2 -0.5 0.7 0.3PCB 49 -0.7 -1.2 -0.6 0.5 0.8 -0.7 2.2 0.1 -0.2 1.2 -2.2 0.7 -0.7 0.9PCB 52 -0.7 -0.9 -0.8 -1.1 0.1 0.0 -0.5 2.6 -0.2 0.3 -0.8 1.1 -1.8 0.5 -0.4 1.1 0.7PCB 66 -1.2 -1.5 -0.4 -1.1 0.3 0.4 1.5 0.7 0.1 2.8 1.8 -1.4 -0.2 0.0 0.8 0.4PCB 95 -0.9 -0.6 -2.6 -0.4 0.7 -0.7 3.6 0.7 -1.0 2.1 -1.7 -0.3 0.8PCB 99 -2.7 -1.4 -0.9 0.8 -0.6 3.6 0.9 1.0 -0.8 1.8 -1.5 -0.4 1.3PCB 101 -1.2 -1.3 -1.1 -1.2 0.3 0.3 0.3 2.6 0.2 -0.1 -1.5 0.9 -2.5 0.2 0.1 1.6 1.1PCB 105 -1.2 -1.6 -1.7 1.7 0.7 0.1 0.0 3.2 -0.7 1.5 -2.0 -0.4 -0.3 -0.9 -0.1PCB 118 -0.7 -1.8 -1.5 -0.8 0.8 0.8 0.1 3.2 0.7 -0.8 1.9 -1.8 -0.1 0.0 -1.2 1.1PCB 128 -1.6 -1.3 -1.5 -0.7 0.9 0.8 0.1 1.3 -0.6 0.3 2.2 -2.1 1.2 0.3 -0.8 0.3PCB 138 -0.3 -1.5 -1.9 -0.6 1.1 2.5 0.8 4.8 0.1 3.7 -1.5 0.7 0.5 1.3 1.5PCB 149 -0.9 -0.9 -0.9 -0.9 1.1 -0.2 2.2 0.0 0.0 2.6 -1.4 -0.3 -0.3PCB 170 0.0 -1.0 -1.6 -0.1 2.0 1.0 0.5 3.2 1.9 3.1 -2.0 0.4 0.3 1.9 -2.1PCB 180 -0.9 -1.1 -1.4 -1.1 1.2 0.8 1.5 1.9 1.5 2.1 1.8 2.0 -1.9 0.1 -0.7 -0.6 0.4PCB 187 -0.7 -1.3 -1.5 -1.1 1.1 0.6 0.8 3.3 0.1 2.1 -2.2 0.1 -0.3 1.3 1.0PCB 194 -1.8 -1.3 -1.7 -1.3 1.4 0.5 4.4 1.4 1.2 2.0 3.8 -1.5 -1.2 -1.3PCB 195 -0.5 -1.3 1.0 -1.7 0.7 0.4 0.4 4.2 -0.5 1.2 -1.9 0.8 -1.1 -1.2 3.0PCB 206 -0.5 -2.1 -2.7 -1.8 1.6 1.4 2.6 0.6 1.3 4.4 2.1 -2.6 2.3 -1.4 -0.6 0.5PCB 209 -1.2 -2.6 -3.0 -1.7 1.2 1.8 5.2 2.5 1.1 -0.8 1.1 -3.1 4.3 -1.3 -1.4 -1.7
Table 20. p scores (15%) for water, TEO, and PAHs in Mussel Tissue XI and SRM 1974b

Laboratory No. 1a 1a 1b 1b 1c 1c 2 2 4 4 7 7 8 8 9 9 9 rev 9 rev

QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b

Water (percent) 0.01 0.01 0.01 0.02 0.00 0.00 0.00 0.02 0.02 0.02 0.02TEO (percent) 0.06 0.03 0.32 1.70 0.74 2.78 1.06 0.16 0.27 1.44 0.00naphthalene 0.11 0.23 0.39 0.23 0.33 0.04 0.58 0.52 1.00 1.38 0.83 1.272-methylnaphthalene 0.11 0.08 0.18 0.17 0.25 1.00 0.31 0.58 2.48 4.17 2.44 4.031-methylnaphthalene 0.15 0.15 0.29 0.38 0.31 0.41 0.13 1.71 1.61biphenyl 0.03 0.06 1.17 0.58 0.66 1.15 1.22 1.122,6-dimethylnaphthalene 0.12 0.31 0.21 0.12 0.23 0.66 2.03 1.99acenaphthylene 0.07 0.37 0.09 0.66 0.68acenaphthene 0.03 0.28 2.14 0.42 0.17 0.15 0.071,6,7-trimethylnaphthalene 0.16 0.07 0.30 0.91fluorene 0.12 0.08 0.44 0.24 0.37 0.34 0.35phenanthrene 0.15 0.20 0.20 0.12 0.10 2.06 0.95 0.20 0.73 0.53 0.27 2.21 1.22 2.16 1.41anthracene 0.05 0.06 0.12 0.41 1.82 0.07 0.93 0.69 0.88 0.791-methylphenanthrene 0.08 0.27 0.22 0.30 0.07 0.38 0.61 0.47fluoranthene 0.09 0.08 0.15 0.06 0.09 0.19 0.82 2.27 0.22 0.49 0.46 0.11 0.75 1.56 0.60 1.62pyrene 0.20 0.11 0.15 0.00 0.11 0.14 1.21 1.15 0.22 1.61 0.45 0.11 0.98 1.47 0.88 1.56benz[a]anthracene 0.05 0.09 0.16 0.42 0.19 0.10 1.13 1.60 1.04 0.88 0.41 0.22 2.26 1.43 2.18 1.40chrysene 0.19 0.08 0.03 0.13 0.18 0.37 1.14 4.04 0.35 0.53 0.45 0.22 0.52 0.88 0.47 0.92triphenylene 0.26 0.19 0.16 0.10benzo[b ]fluoranthene 0.07 0.14 0.10 0.14 0.15 0.30 1.00 1.43 0.43 1.09 0.53 0.13 0.80 0.66 0.64 0.69

benzo[j]fluoranthene 0.08 0.15 0.47 0.20 0.12 0.26benzo[k ]fluoranthene 0.09 0.11 0.46 0.31 0.05 0.15 0.45 0.98 0.13 0.27 0.22 1.36 0.38 1.22

benzo[e]pyrene 0.05 0.23 0.07 0.14 0.19 0.12 2.02 1.22 0.39 0.52 0.29 0.04 0.95 1.87 0.92 2.00benzo[a]pyrene 0.21 0.07 0.44 0.33 0.38 1.08 0.55 0.65 0.86 0.99

perylene 0.07 0.26 0.19 1.19indeno[1,2,3-cd]pyrene 0.20 0.14 0.21 0.21 0.23 0.57 0.40 0.23dibenz[a,h]anthracene 0.38 0.09 0.65 0.68 0.36 0.51

benzo[ghi]perylene 0.21 0.07 0.07 0.10 0.27 0.31 0.11 0.19 0.93 1.04

*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 20 (cont). p scores (15%) for water, TEO, and PAHs in Mussel Tissue XI and SRM 1974b

Laboratory No. 11 11 12 12 14 14 15 15 16 16 17 17 18 18 19 19 20 20

QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b

Water (percent) 0.03 0.03 0.04 0.00 0.04 0.01 0.01 0.02 0.06 0.91 0.08 0.07 0.01 0.01 0.07TEO (percent) 0.80 1.06 1.51 0.87 0.02 1.96 1.23 0.47 1.18 0.10 0.06 0.95 0.84naphthalene 0.64 2.07 1.10 0.54 0.56 0.93 0.99 0.37 2.66 1.922-methylnaphthalene 0.37 2.00 0.38 0.51 0.31 0.16 1.07 0.72 1.43 1.881-methylnaphthalene 0.32 2.06 0.33 0.60 1.04 0.06 0.34 0.26 1.15 0.78 0.83 2.38biphenyl 0.68 1.72 0.37 0.22 1.59 0.77 1.55 1.532,6-dimethylnaphthalene 0.41 1.47 0.46 0.61 0.18 0.31 0.83 0.50 1.22 4.30 0.31 5.14acenaphthylene 0.49 0.62 0.48 0.38 0.54 0.27 1.27 0.55 3.73 6.30 1.49acenaphthene 0.13 1.41 0.18 0.56 0.83 0.49 2.26 2.65 5.081,6,7-trimethylnaphthalene 0.25 0.88 0.43 0.10 0.30 0.18 1.20 1.55 4.10 0.08 1.89fluorene 0.63 0.61 0.02 2.28 0.11 0.17 0.34 0.96 1.15 2.75 4.04phenanthrene 0.35 1.13 0.31 0.91 0.56 0.28 0.17 0.26 0.27 0.91 0.79 0.29 0.19 0.33 0.35anthracene 1.33 0.54 0.07 0.64 0.09 1.03 1.11 1.54 1.121-methylphenanthrene 0.35 0.53 0.11 0.16 0.41 3.48 0.27 1.34 1.25 1.89fluoranthene 0.04 0.99 0.40 0.62 0.42 1.05 0.08 0.11 0.49 0.45 0.71 0.62 0.09 0.07 0.62pyrene 0.03 1.10 0.37 0.59 0.39 0.27 0.10 0.11 0.21 0.87 0.95 0.78 0.04 0.23 0.84benz[a]anthracene 0.33 0.99 0.51 0.60 0.15 0.30 0.41 0.84 0.70 1.30 0.23 0.37 0.64chrysene 0.32 0.69 0.09 0.20 0.21 0.42 0.67 0.85 0.74triphenylenebenzo[b ]fluoranthene 0.41 0.57 0.12 0.26 1.84 2.09 1.56 1.92 1.25 1.28 0.97

benzo[j]fluoranthene 1.34 1.48

benzo[k ]fluoranthene 0.57 0.84 0.37 0.90 3.07 1.50 0.26 0.22 1.85 0.74 3.35

benzo[e]pyrene 0.37 0.66 0.31 0.97 1.94 1.68 0.07 0.13 1.43 1.55 1.62 0.92 0.81 0.09 0.13benzo[a]pyrene 0.54 0.81 0.66 1.02 2.06 0.45 0.09 1.99 1.14 3.63 1.99 0.41perylene 0.64 1.13 0.16 0.63 0.35 0.10 2.25 2.41 4.18 1.99 0.94indeno[1,2,3-cd]pyrene 0.20 1.28 0.43 0.72 0.39 0.07 2.86 3.38 4.22 2.76 0.76dibenz[a,h]anthracene 0.26 0.33 0.36 0.86 0.61 0.07 3.49 4.27 2.15 4.21 0.00

benzo[ghi]perylene 0.44 0.82 2.91 3.37 0.29 0.14 1.93 1.61 4.01 2.17 0.75
Table 21. p scores (15%) for Pesticides in Mussel Tissue XI and SRM 1974b

Laboratory No. 1a 1a 1b 1b 1c 1c 2 2 4 4 7 7 8 8 9 9 9 rev 9 rev

QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b

alpha-HCH (a-BHC)hexachlorobenzenegamma-HCH (g-BHC,lindane)beta-HCH (b-BHC)heptachlor 1.31 0.36aldrinheptachlor epoxideoxychlordane 1.16 0.69gamma-chlordane 0.04 0.21 0.07 0.19 0.54 0.19 3.25 0.77 1.02 0.06 0.30 2.30 0.79 0.65 1.09 0.762,4'-DDE 1.20 0.34endosulfan Icis-chlordane (alpha-chlordane 0.11 0.28 0.06 0.18 0.47 0.32 4.20 0.99 0.44 0.31 0.40 0.27 0.55 1.16 0.70 1.17

trans-nonachlor 0.23 0.25 0.09 0.16 0.90 0.83 1.71 1.29 0.44 0.09 0.35 0.27 0.22 1.46 0.39 1.67dieldrin 0.08 0.07 0.10 0.14 4.70 1.99 0.51 1.92 0.564,4'-DDE 0.12 0.27 0.05 0.26 0.54 0.38 0.70 0.38 0.22 0.03 0.26 0.15 0.73 0.44 0.70 0.592,4'-DDD 0.07 0.22 0.17 0.10 0.31 0.35 2.26 0.10 0.17 0.32 2.34endrinendosulfan II4,4'-DDD 0.14 0.14 0.41 0.33 3.01 0.25 0.15 0.28 3.05 1.52 1.63 1.65 1.822,4'-DDT 0.10 0.05 0.20 0.32 0.30 0.43 2.56cis-nonachlor 0.10 0.08 0.33 0.14 1.93 0.80 2.67 0.64 2.61 0.60

4,4'-DDT 0.04 0.17 0.36 0.31 2.78 3.87 1.54 2.24 1.73 2.44mirexendosulfan sulfatechlorpyrifos*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 21 (cont). p scores (15%) for Pesticides in Mussel Tissue XI and SRM 1974b

Laboratory No. 11 11 12 12 14 14 15 15 16 16 17 17 18 18 19 19 20 20

QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b

alpha-HCH (a-BHC) 1.02 1.50 1.50 0.36 0.27 0.20hexachlorobenzene 1.04 2.37 2.90 0.86 0.72 2.50 3.87gamma-HCH (g-BHC,lindane) 1.36 4.89 0.83 4.92 0.43 0.69 1.15 2.13 1.47 0.49 1.69beta-HCH (b-BHC) 4.43 7.63 2.22 1.07 0.21heptachlor 0.64 0.18 3.24 0.33 0.44 0.71 1.44 0.48 2.20aldrin 0.69 1.72 2.48 1.46 0.47 0.12 0.07 4.74heptachlor epoxide 0.60 0.44 2.12 1.15oxychlordane 0.51 0.76 0.98 1.33 0.07 0.05gamma-chlordane 0.49 0.96 1.40 4.68 0.19 0.13 0.39 1.18 0.22 0.66 0.26 1.04 0.522,4'-DDE 1.20 0.72 0.59 0.53 1.68 0.41 0.16endosulfan I 2.71 1.39 1.62 2.50cis-chlordane (alpha-chlordane 0.32 0.81 0.25 0.67 0.99 0.68 0.24 0.10 0.52 1.22 0.23 0.15 1.53 1.14 0.45 0.36 1.04 0.16

trans-nonachlor 0.26 0.78 0.34 0.53 1.26 0.75 0.16 0.19 0.48 0.75 0.21 0.17 0.52 0.53 0.76 0.27 0.99 0.45dieldrin 0.74 0.99 1.39 1.20 1.68 0.56 0.26

4,4'-DDE 0.37 0.58 0.22 0.78 0.10 0.10 0.39 0.08 0.36 0.71 0.22 0.27 0.71 0.60 0.33 0.28 0.88 0.332,4'-DDD 0.34 0.65 0.28 0.15 0.26 0.91 0.59 0.59 0.32 0.92 0.34 2.80 2.25 0.19 0.81 0.22 0.40endrin 0.73 1.55 2.60 2.28endosulfan II 0.39 0.694,4'-DDD 0.50 0.82 0.68 1.10 0.26 0.19 0.17 0.84 0.22 0.30 1.26 1.11 0.26 1.90 0.73 0.742,4'-DDT 0.68 0.87 0.16 1.01 0.07 0.51 1.18 0.64cis-nonachlor 0.45 0.74 1.49 1.30 0.17 0.06 1.59 1.97 0.97 1.33 1.17 0.304,4'-DDT 0.62 0.71 0.61 4.50 0.40 0.66 0.28 0.78 0.31 3.24 0.70 1.56mirex 0.81 0.26 0.97 1.20 0.96 1.14

endosulfan sulfate 1.28 1.62chlorpyrifos 0.24 1.28
Table 22. p scores (15%) for PCBs in Mussel Tissue XI and SRM 1974b

Laboratory No. 1a 1a 1b 1b 1c 1c 2 2 4 4 7 7 8 8 9 9 9 rev 9 rev

QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b

PCB 8 0.08 0.15 0.23 0.21 1.29 0.58 1.07 0.72 2.17 2.21 2.36 2.15PCB 18 0.06 0.17 0.10 0.15 0.31 0.31 0.09 0.71 0.14 0.28 0.66 1.25 0.75 1.14PCB 28 0.15 0.13 0.10 0.07 0.10 0.15 0.98 1.35 0.20 0.11 0.13 0.10 0.22 1.20 0.36 1.40PCB 31 0.22 0.26 0.03 0.15 0.43 0.45 1.11 1.28 0.23 0.22 0.43 0.35 0.58 0.54PCB 44 0.17 0.19 0.10 0.08 0.20 0.29 0.52 0.67 0.26 0.24 0.17 0.25 1.64 0.59 1.51 0.68PCB 49 0.04 0.07 0.15 0.08 0.23 0.23 0.56 1.07 0.25 0.25 1.53 1.19 1.72 1.06PCB 52 0.12 0.05 0.05 0.07 0.20 0.21 0.69 0.67 0.13 0.29 0.11 0.12 2.07 1.69 2.18 1.87PCB 66 0.04 0.07 0.06 0.06 0.19 0.13 0.04 1.00 0.17 0.20 0.15 0.13 1.69 2.04 1.77 2.17PCB 95 0.18 0.06 0.10 0.08 0.23 0.18 0.96 0.83 0.29 0.26 0.77 0.59 0.80 0.77PCB 99 0.23 0.07 0.03 0.05 0.21 0.21 0.43 0.87 0.30 0.30 1.16 0.90 1.32 1.10PCB 101 0.05 0.25 0.03 0.04 0.15 0.22 0.20 1.25 0.11 0.41 0.13 0.11 0.52 0.66 0.60 0.84PCB 105 0.13 0.21 0.05 0.04 0.19 0.28 0.33 0.26 0.27 0.16 1.30 0.98 1.17 1.18PCB 118 0.06 0.25 0.06 0.04 0.08 0.32 0.60 1.56 0.21 0.32 0.15 0.18 0.84 0.86 0.94 1.03PCB 128 0.17 0.09 0.13 0.02 0.25 0.34 1.49 3.92 0.33 0.46 0.27 0.20 0.82 0.77 0.73 0.78PCB 138 0.06 0.02 0.05 0.03 0.08 0.37 0.44 0.82 0.27 0.44 0.29 0.22 0.57 0.91 0.69 1.09PCB 149 0.11 0.05 0.09 0.12 0.28 0.31 1.23 2.24 0.19 0.33 0.73 0.72 0.88 0.92PCB 153 0.07 0.21 0.04 0.05 0.16 0.29 0.48 0.84 0.24 0.39 0.05 0.03 0.68 0.98 0.83 1.18PCB 156 0.06 0.29 0.10 0.08 0.28 0.43 0.00 0.25 0.13 0.48 0.57 0.60 0.61 0.43PCB 170 0.12 0.17 0.36 0.67 3.16 0.67 3.34 0.61PCB 180 0.04 0.12 0.09 0.03 0.34 0.39 0.26 0.66 0.07 0.32 1.00 0.95 0.87 0.86PCB 187 0.15 0.05 0.11 0.03 0.22 0.36 0.23 0.98 0.22 0.35 0.14 0.84 1.34 1.53 1.40 1.64PCB 194 1.52 1.51PCB 195PCB 206PCB 209*Lab 9 rev values are calculated on a wet mass basis as requested. The original submission (Lab 9) was calculated on a dry mass basis.
Table 22 (cont). p scores (15%) for PCBs in Mussel Tissue XI and SRM 1974b

Laboratory No. 11 11 12 12 14 14 15 15 16 16 17 17 18 18 19 19 20 20

QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b QA03TIS11 1974b

PCB 8 2.25 1.84 0.22 0.26 1.14 1.32 0.55 1.60 0.28PCB 18 0.39 0.74 0.62 1.29 0.16 1.59 0.10 0.22 0.59 0.32 0.20 1.07 0.78 0.32 0.90 0.73 0.34PCB 28 0.45 0.75 0.22 0.42 1.09 0.51 0.15 0.35 0.94 0.80 1.08 0.39 0.22PCB 31 0.33 0.58 0.82 0.11 0.56 0.53 0.34 0.17PCB 44 0.33 0.68 0.46 0.95 0.70 0.48 0.12 0.04 0.46 0.61 0.17 0.06 0.68 0.73 0.55 0.45 0.47 0.34PCB 49 0.42 0.84 0.45 0.92 0.98 0.29 0.07 0.04 1.66 0.71 0.07 0.07 0.73 0.95 0.63 0.56PCB 52 0.37 0.74 0.42 0.88 0.71 0.41 0.08 0.03 0.89 0.96 0.21 0.02 0.70 0.56 0.25 0.02 0.61 0.10PCB 66 0.45 0.66 0.79 0.13 0.37 0.17 0.21 0.61 0.35 0.19 0.66 0.68 0.21 0.24 0.79 0.18PCB 95 0.32 0.69 0.15 2.19 0.10 0.04 1.05 0.19 0.75 0.64 0.49 0.23PCB 99 0.35 0.68 0.49 0.95 0.58 0.44 0.07 0.10 1.06 0.26 0.69 0.45 0.74 0.34PCB 101 0.32 0.70 0.55 0.84 0.68 0.41 0.11 0.03 1.03 0.20 0.18 0.02 0.71 0.56 0.36 0.08 0.56 0.00PCB 105 0.50 0.94 0.08 0.10 0.45 0.33 1.38 1.51 0.67 0.75 0.33 0.31 0.48 0.58PCB 118 0.47 0.74 0.60 0.38 0.18 0.10 0.52 0.51 0.24 0.06 0.66 0.71 0.73 0.25 0.57 0.19PCB 128 0.55 0.86 0.45 0.54 0.13 0.15 0.67 0.20 0.57 0.24 0.87 0.59 0.60 0.38 0.66 0.65PCB 138 0.49 0.74 0.03 0.12 0.66 0.20 0.19 0.03 0.61 0.66 0.53 0.34 0.78 0.12PCB 149 0.34 0.64 0.77 0.49 0.09 0.12 1.04 0.12 0.82 0.73 0.56 0.08PCB 153 0.50 0.73 0.10 0.11 0.72 0.12 0.70 0.86 0.77 0.75 0.48 0.06 0.47 0.15PCB 156 0.53 0.78 0.29 1.89 0.33 0.28 0.30 0.28 0.35 0.63 0.77 1.03PCB 170 1.01 0.75 0.55 0.23 0.62 0.35 3.10 0.71 0.55 0.21 0.39PCB 180 0.54 0.84 0.56 0.94 2.27 0.36 0.32 0.09 0.53 0.42 0.29 0.19 2.05 0.99 0.46 0.05 1.00 0.73PCB 187 0.46 0.72 0.34 0.04 0.60 0.31 0.31 0.18 0.46 0.64 0.41 0.08 0.86 0.36PCB 194 0.41 0.97 2.86 0.46 1.33 0.59 1.03 0.24PCB 195 0.61 0.82 4.06 2.90PCB 206 0.87 0.54 3.46 2.14 2.56 3.69 0.01 1.14PCB 209 0.82 0.96 2.97 2.61 2.52 3.43
Table 23. p scores (15%) for water, TOC, and PAHs in Marine Sediment XII and SRM 1941b

Laboratory No. 1a 1a 1b 1b 1c 1c 2 2 3 3 4 4 5 5 6 6 7 7

QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941a QA03SED12 1941b QA03SED12 1944 QA03SED12 1944 QA03SED12 1941b

Water 0.01 0.06 0.13 0.07 0.08 0.40 0.00 0.04 0.06TOC 0.04naphthalene 0.14 0.06 0.04 0.09 0.18 0.17 0.82 0.47 0.80 1.82 0.49 0.50 0.48 1.09 0.23 0.12 0.792-methylnaphthalene 0.07 0.28 0.26 0.18 0.55 0.30 0.60 0.50 1.71 0.36 0.33 1.05 0.25 0.10 0.071-methylnaphthalene 0.12 0.36 0.24 0.13 0.58 0.42 0.37 0.41 1.90 0.13 0.29 0.90 0.43 0.12 0.02biphenyl 0.16 0.19 0.13 0.06 0.31 0.33 0.40 0.52 2.44 0.30 0.28 1.51 0.29 0.15 0.072,6-dimethylnaphthalene 0.09 0.18 0.29 0.13 0.48 0.31 0.42 0.60 0.37 0.76 0.32 1.55 1.37 0.55 0.15 0.14acenaphthylene 0.31 0.24 0.54 0.31 0.17 0.26 2.89 2.44 1.12 0.92 0.90 0.11 0.80 1.78 1.07 0.14 0.29acenaphthene 0.09 0.41 0.52 0.29 0.50 0.31 0.36 0.68 0.77 1.86 2.32 0.86 0.36 1.34 0.45 0.28 0.111,6,7-trimethylnaphthalene 0.14 0.31 0.30 0.19 0.36 1.62 0.80 0.57fluorene 0.07 0.28 1.03 0.07 0.54 0.15 0.35 1.24 0.99 0.65 0.80 1.35 0.22 0.71 0.92 0.14 0.15phenanthrene 0.09 0.15 0.46 0.15 0.36 0.03 0.14 0.69 0.87 0.59 0.92 0.29 0.16 1.09 0.07 0.11 0.11anthracene 0.10 0.22 0.41 0.11 0.42 0.21 0.31 0.74 1.00 0.63 0.50 0.73 0.33 1.19 0.23 0.26 0.061-methylphenanthrene 0.06 0.06 0.44 0.22 0.78 0.30 2.31 1.42 0.43 0.93 0.37 0.18 0.46fluoranthene 0.06 0.35 0.26 0.15 0.23 0.15 0.34 0.68 0.75 0.45 0.86 0.22 0.13 1.16 0.14 0.12 0.47pyrene 0.08 0.12 0.22 0.15 0.32 0.11 0.42 0.68 0.65 0.44 0.90 0.74 1.29 0.99 0.12 0.06 0.48benz[a]anthracene 0.07 0.20 0.28 0.16 0.42 0.03 0.40 0.78 0.56 0.25 0.81 0.86 0.27 0.80 0.44 0.12 0.36chrysene 0.05 0.27 0.43 0.14 0.12 0.30 0.42 0.80 0.68 0.57 0.87 0.27 0.46 1.20 0.50 0.30 0.14triphenylene 0.40 0.16 0.14 0.14 0.79benzo[b ]fluoranthene 0.12 0.10 0.10 0.36 0.19 0.15 0.41 1.15 0.45 0.53 1.05 0.44 0.50 1.67 0.77 0.19 0.55benzo[j ]fluoranthene 0.20 0.05 0.18 0.37 0.18 0.32benzo[k ]fluoranthene 0.14 0.15 0.13 0.35 0.25 0.65 2.82 2.13 0.37 0.82 1.35 0.85 0.98 0.79 0.62 0.37 0.36

benzo[e]pyrene 0.14 0.14 0.12 0.32 0.17 0.14 0.64 0.87 0.40 0.21 0.12 1.24 0.69 0.08 0.65benzo[a]pyrene 0.06 0.09 0.18 0.22 0.44 0.40 0.62 0.80 0.35 0.50 0.76 0.75 1.50 0.97 0.67 0.31 0.52perylene 0.25 0.16 0.10 0.20 0.50 1.04 0.69 0.49 0.39 1.95 0.78 1.65 0.42indeno[1,2,3-cd]pyrene 0.09 0.15 0.41 1.17 0.26 0.59 0.36 1.36 0.74 0.25 0.76 0.03 0.26 0.94 0.35 0.21 0.17dibenz[a,h]anthracene 0.25 0.08 0.92 0.21 0.38 0.77 0.70 1.96 0.92 0.76 0.41 0.44 0.46 0.95 0.32 2.67 2.43

benzo[ghi]perylene 0.07 0.11 0.13 0.29 0.32 0.38 0.48 1.51 0.49 0.69 1.08 0.23 0.25 1.12 0.27 0.59 0.16
Table 23 (cont). p scores (15%) for water, TOC, and PAHs in Marine Sediment XII and SRM 1941b

Laboratory No. 9 9 10 10 11 11 12 12 13 13 14 14 15 15 16 16 17 17

QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1944

Water 0.11 0.73 0.05 0.10 0.09 0.09 0.01 0.06 0.01 0.02 0.21TOC 0.44 0.18 0.81 0.18naphthalene 3.09 4.92 0.68 0.13 0.21 1.15 0.41 3.05 0.13 0.31 0.15 0.29 0.532-methylnaphthalene 3.20 4.27 1.96 0.29 0.10 1.05 0.78 0.53 0.48 0.50 0.14 0.33 0.34

1-methylnaphthalene 2.61 3.98 0.05 0.93 0.99 0.77 0.76 0.27 0.12 1.58 0.96biphenyl 1.60 3.43 0.84 0.57 0.64 0.89 0.67 0.24 0.05 1.81 0.662,6-dimethylnaphthalene 2.18 2.59 0.76 0.42 0.14 0.47 0.25 0.03 1.12 0.70acenaphthylene 0.55 1.52 0.41 0.63 0.39 0.41 0.20 3.30 0.80 0.71 0.38 0.14 4.30 3.13acenaphthene 1.30 2.80 0.95 0.54 0.94 0.57 0.94 4.80 0.77 0.81 0.54 0.04 0.98 0.681,6,7-trimethylnaphthalene 0.82 1.26 0.32 0.08 0.70 0.25fluorene 1.04 1.80 1.10 0.52 1.14 0.21 0.63 4.07 0.38 1.20 1.20 0.09 0.84 0.58phenanthrene 0.89 1.15 0.79 0.32 0.30 0.25 0.27 1.12 0.45 0.26 0.68 0.12 0.68 1.56anthracene 0.89 1.72 2.06 0.31 0.29 0.13 0.17 2.43 0.68 1.56 0.41 0.07 1.47 0.191-methylphenanthrene 0.95 0.69 0.34 0.78 0.85 0.44 0.37 0.11 1.51 1.65fluoranthene 0.56 0.97 0.58 0.25 0.29 0.65 0.22 0.25 0.66 1.36 0.47 0.11 1.48 2.01pyrene 0.58 0.97 0.62 0.22 0.34 0.57 0.23 0.08 0.57 0.88 0.40 0.12 1.77 2.11benz[a]anthracene 0.57 1.17 1.06 0.29 0.17 0.21 0.19 0.86 1.34 1.90 0.46 0.17 1.38 1.90chrysene 0.40 0.94 0.68 0.24 0.34 1.03 0.30 0.57 0.52 0.24 1.31 1.97triphenylenebenzo[b ]fluoranthene 0.49 1.67 0.53 0.36 0.69 0.24 1.41 0.79 0.40 0.18 1.36 1.66benzo[j]fluoranthene 1.08 1.37

benzo[k ]fluoranthene 0.29 0.94 0.81 0.49 0.48 0.84 0.18 0.91 1.23 0.42 0.12

benzo[e]pyrene 0.35 1.18 0.62 0.69 0.16 0.70 0.53 0.82 0.48 0.17 0.84 1.40benzo[a]pyrene 0.25 1.30 1.16 0.34 0.59 0.70 0.10 1.41 0.78 4.26 0.38 0.20 1.29 1.66perylene 5.31 1.41 0.37 1.07 0.19 0.71 0.82 0.59 0.35 0.07 0.98 1.14indeno[1,2,3-cd]pyrene 0.30 1.10 0.63 0.43 0.43 0.72 0.15 2.43 1.71 0.79 0.37 0.09 1.24 1.06dibenz[a,h]anthracene 0.46 1.07 3.83 0.67 0.47 0.84 0.82 3.35 0.43 0.11 0.15 0.67 0.97

benzo[ghi]perylene 0.35 2.76 0.63 0.32 0.58 0.74 1.45 1.54 0.80 1.33 0.33 0.18 0.41 0.99
Table 23 (cont). p scores (15%) for water, TOC, and PAHs in Marine Sediment XII and SRM 1941b

Laboratory No. 18 18 19 19 20 20

QA03SED12 1944 QA03SED12 1941b QA03SED12 1941b

Water 0.53 0.09 0.23TOC 1.74 0.67naphthalene 0.47 0.38 1.95 0.75 0.562-methylnaphthalene 0.37 0.23 2.02 0.68 0.341-methylnaphthalene 0.43 0.15 1.89 0.80 0.25biphenyl 0.73 0.30 2.12 1.31 0.442,6-dimethylnaphthalene 0.91 0.41 1.30 1.06 0.07acenaphthylene 2.35 1.40 2.04 1.08 0.74acenaphthene 1.51 0.75 2.19 1.50 0.021,6,7-trimethylnaphthalene 2.77 1.13 0.84 0.17 0.22fluorene 2.65 0.95 1.81 0.07 1.26phenanthrene 0.55 0.12 0.49 0.59 0.22anthracene 0.66 0.27 1.45 0.16 0.881-methylphenanthrene 0.72 0.37 0.71 0.18 1.06fluoranthene 0.56 0.31 0.03 0.52 0.35pyrene 0.54 0.06 0.23 0.25 0.09benz[a]anthracene 0.51 0.09 0.54 0.31 0.39chrysene 0.29 0.05 1.26triphenylenebenzo[b ]fluoranthene 0.48 0.44 0.85 0.80 1.27

benzo[j ]fluoranthenebenzo[

k ]fluoranthene 0.29 0.19 0.54

benzo[e]pyrene 0.21 0.13 0.58 0.34 0.79benzo[a]pyrene 0.59 0.12 0.68 0.44 0.51perylene 0.50 0.10 0.68 1.41 0.41indeno[1,2,3-cd]pyrene 0.39 0.31 0.28 0.39 0.61dibenz[a,h]anthracene 0.45 0.15 0.55

benzo[ghi]perylene 0.43 0.35 0.89 3.77 0.56
Table 24. p scores (15%) for Pesticides in Marine Sediment XII and SRM 1941b

Laboratory No. 1a 1a 1b 1b 1c 1c 2 2 3 3 4 4 5 5 6 6 7 7

QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941a QA03SED12 1941b QA03SED12 1944 QA03SED12 1944 QA03SED12 1941b

alpha-HCH (a-BHC)hexachlorobenzene 0.19 0.11 0.29 0.01 0.98 3.09 0.71 0.37gamma-HCH (g-BHC,lindane)beta-HCH (b-BHC)heptachloraldrinheptachlor epoxideoxychlordanegamma-chlordane 0.74 0.16 0.41 1.89 0.47 0.642,4'-DDE 1.01 0.19 0.65

endosulfan Icis-chlordane (alpha-chlordane) 0.52 0.13 0.33 0.31 0.53 0.54trans-nonachlor 0.27 0.18 0.36 0.65dieldrin 0.15 0.64 0.54 1.714,4'-DDE 0.07 0.20 0.27 0.14 0.49 0.03 0.36 0.47 0.10 0.162,4'-DDD 0.04 0.16 0.50 0.58 1.08 0.65 0.06endrinendosulfan II4,4'-DDD 0.13 0.18 0.68 0.18 0.11 1.26 0.96 1.09 0.43 0.08 0.152,4'-DDT 0.07 0.16 0.29 0.14 0.22 2.58 0.63 0.41cis-nonachlor 0.15 1.15 0.464,4'-DDT 0.32 0.32 0.42 0.40 0.09 0.95 1.72 0.45 0.52mirexendosulfan sulfatechlorpyrifos
Table 24 (cont). p scores (15%) for Pesticides in Marine Sediment XII and SRM 1941b

Laboratory No. 9 9 10 10 11 11 12 12 13 13 14 14 15 15 16 16 17 17

QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1944

alpha-HCH (a-BHC) 2.02 2.64 1.43 0.90 0.09 1.28hexachlorobenzene 2.59 2.26 1.58 0.60 0.12 1.40 9.81 1.55 0.15 1.36gamma-HCH (g-BHC,lindane) 1.76 1.63 0.48beta-HCH (b-BHC) 1.89 0.68 0.71heptachlor 0.33 2.55 2.02 0.57 1.87

aldrin 2.25 1.22 3.00 0.63 7.64 1.89heptachlor epoxide 1.18 2.85 0.98

oxychlordane 1.40 0.60 0.80gamma-chlordane 1.01 2.43 1.15 0.23 3.70 0.03 0.20 0.95 0.802,4'-DDE 0.66 1.18 0.08 5.34 0.56 0.16 0.25 0.36 0.34endosulfan Icis-chlordane (alpha-chlordane) 2.14 4.38 1.17 0.29 0.02 5.04 2.63 0.06 0.34 2.02 1.05 2.81 1.11

trans-nonachlor 2.93 2.34 1.66 4.38 1.51 3.33 0.79 1.27dieldrin 0.79 3.43 1.31 1.05 2.19 0.51 4.854,4'-DDE 0.66 0.04 0.84 0.96 0.08 5.31 5.19 0.91 0.56 0.32 0.25 0.37 1.04

2,4'-DDD 0.98 0.71 1.74 0.15 0.22 1.01 0.32 0.33 1.04endrin 2.21 1.40 2.52endosulfan II 0.72 2.524,4'-DDD 2.64 2.80 1.36 0.68 2.44 5.42 0.25 0.71 0.32 0.722,4'-DDT 0.74 1.05 2.13 1.32 0.90 0.32 2.16cis-nonachlor 1.10 6.49 1.01 0.26 2.85 0.444,4'-DDT 1.10 1.80 0.99 0.47 3.50 5.77 0.60 1.50 0.77 1.24 0.77 0.52mirex 0.15 0.75 1.04 0.51endosulfan sulfate 2.43 0.83chlorpyrifos 4.85
Table 24 (cont). p scores (15%) for Pesticides in Marine Sediment XII and SRM 1941b

Laboratory No. 18 18 19 19 20 20

QA03SED12 1944 QA03SED12 1941b QA03SED12 1941b

alpha-HCH (a-BHC) 0.74hexachlorobenzene 0.55 0.94 1.43 0.26gamma-HCH (g-BHC,lindane) 1.05 0.62beta-HCH (b-BHC)heptachlor 2.23 1.67aldrin 1.75 4.69heptachlor epoxide 2.90 4.11 2.40oxychlordane 0.70gamma-chlordane 0.28 0.50 1.242,4'-DDE 0.36 0.80endosulfan I 1.82 0.92cis-chlordane (alpha-chlordane) 0.55 0.84 2.68 1.37trans-nonachlor 1.32 0.69 1.90 1.08 1.10dieldrin 0.754,4'-DDE 0.06 0.62 0.15 1.39 0.932,4'-DDD 0.37 0.24 1.02endrinendosulfan II4,4'-DDD 0.43 1.65 0.60 1.71 1.642,4'-DDT 0.53 0.73 0.94cis-nonachlor 0.72 0.764,4'-DDT 0.07 3.34 0.53 1.68 1.87mirex 3.25 3.05endosulfan sulfate 1.61 1.04chlorpyrifos 0.53 1.14
Table 25. p scores (15%) for PCBs in Marine Sediment XII and SRM 1941b

Laboratory No. 1a 1a 1b 1b 1c 1c 2 2 3 3 4 4 5 5 6 6 7 7

QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941a QA03SED12 1941b QA03SED12 1944 QA03SED12 1944 QA03SED12 1941b

PCB 8 0.08 0.32 0.23 0.05 0.88 1.37 2.92 0.34 0.56 0.81 0.68PCB 18 0.15 0.18 0.62 0.06 0.87 0.70 0.72 0.70 1.02 0.39 0.54 0.58PCB 28 0.10 0.17 0.32 0.07 0.50 0.46 1.09 0.88 1.08 0.36 0.76 0.68PCB 31 0.07 0.23 0.22 0.15 0.40 0.44 1.37 0.07 0.67 0.72PCB 44 0.10 0.14 0.48 0.05 0.21 0.16 0.95 0.59 1.15 0.43 0.64 0.82PCB 49 0.13 0.18 0.37 0.24 0.76 0.08 1.08 0.70 0.64 0.71PCB 52 0.17 0.09 0.43 0.10 0.40 0.03 0.90 0.34 0.58 0.41 0.55 0.72PCB 66 0.07 0.12 0.32 0.07 1.05 0.23 0.89 0.76 1.02 0.41 0.80 0.79PCB 95 0.09 0.19 0.22 0.26 0.19 0.09 0.86 0.46 0.65 0.95PCB 99 0.19 0.19 0.30 0.13 0.61 1.05 0.31 0.81 0.82PCB 101 0.15 0.11 0.22 0.12 0.25 0.44 1.06 0.08 0.34 0.38 0.89 0.73PCB 105 0.04 0.24 0.37 0.20 0.40 0.78 0.73 0.48 1.07 0.56PCB 118 0.20 0.09 0.27 0.05 0.34 0.18 1.19 0.32 0.29 0.41 0.90 0.89PCB 128 0.07 0.12 0.21 0.20 0.48 1.18 1.03 0.35 0.41 0.87 0.95PCB 138 0.10 0.29 0.24 0.11 0.09 0.11 0.99 1.25 0.24 0.41 0.92 0.73PCB 149 0.32 0.10 0.24 0.04 0.29 0.09 0.89 0.28 0.79 0.81PCB 153 0.05 0.20 0.26 0.04 0.44 0.25 1.14 0.22 0.20 0.39 0.84 0.71PCB 156 0.76 0.11 0.31 0.48 0.58 0.45 1.15 0.99 0.96 0.73PCB 170 0.05 0.21 0.41 0.07 0.77 0.11 1.32 0.44 0.03 0.65 0.94 0.75PCB 180 0.25 0.17 0.50 0.01 0.54 0.01 1.17 0.13 0.19 0.57 0.99 0.69PCB 187 0.07 0.28 0.48 0.03 0.41 0.01 1.23 0.19 0.11 0.74 0.82 0.55PCB 194 0.16 0.09 0.65 0.51 0.70 0.31 1.38 0.47 0.81 1.25PCB 195 0.27 0.77 0.62 0.19 1.37 0.20 0.39 0.74 1.32PCB 206 0.18 0.72 0.06 1.36 0.19 1.04 1.08 0.63 0.66 0.97 0.59PCB 209 0.24 0.12 0.62 0.06 1.90 0.03 1.68 0.73 0.43 0.25 0.59 0.79
Table 25 (cont). p scores (15%) for PCBs in Marine Sediment XII and SRM 1941b

Laboratory No. 9 9 10 10 11 11 12 12 13 13 14 14 15 15 16 16 17 17

QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1941b QA03SED12 1944

PCB 8 1.54 4.83 1.18 1.16 5.42 2.40 1.99 0.69 3.02 4.33PCB 18 1.47 0.64 0.87 0.89 0.63 5.55 0.71 0.90 0.10 2.76 0.21 1.78 1.45PCB 28 0.41 2.43 0.79 0.61 5.31 0.22 0.23 2.07 0.20 1.44 1.46PCB 31 1.64 2.56 0.85 0.85 4.65 0.72 0.15 2.11 0.47PCB 44 0.88 4.03 1.87 0.62 0.27 4.88 0.41 0.54 0.10 2.14 0.23 1.04 1.70

PCB 49 1.70 1.09 0.68 0.62 0.14 4.65 0.44 0.43 0.07 3.01 0.29 1.46 1.57PCB 52 0.82 1.72 1.38 0.84 0.31 2.46 5.08 0.51 0.57 0.11 2.25 1.37 0.94 1.44PCB 66 0.80 1.54 0.74 0.60 4.75 5.32 1.32 0.36 0.07 1.50 0.35 1.41 1.21PCB 95 0.60 2.34 0.37 0.71 1.68 5.02 0.39 0.58 0.25 2.34 0.99PCB 99 0.35 1.97 1.35 0.44 0.37 2.86 4.96 0.48 0.45 0.05 2.50 1.01PCB 101 0.35 1.74 0.50 0.62 0.38 1.75 4.57 0.56 0.56 0.20 4.92 3.35 0.93 2.38PCB 105 0.50 1.55 1.68 0.90 3.14 4.59 0.45 0.20 2.19 0.40 1.07 3.32PCB 118 0.32 3.06 0.20 0.63 3.11 4.29 0.48 0.42 0.22 2.14 0.34 0.88 3.17PCB 128 1.09 0.71 0.83 1.91 2.73 4.37 0.69 0.54 0.17 2.16 0.46 0.97 5.55PCB 138 0.64 1.25 0.09 0.38 2.95 4.22 0.58 0.15 2.09 0.63 1.17 2.78PCB 149 0.85 2.65 0.39 0.52 3.16 4.44 0.65 0.54 0.12 2.03 1.72PCB 153 0.49 1.21 0.23 0.48 1.97 4.50 0.53 0.11 1.92 0.41 1.24 1.70PCB 156 0.85 0.61 0.80 0.68 0.32 4.09 0.47 0.15 1.87 0.65PCB 170 0.91 0.74 0.70 0.68 1.75 4.58 0.47 0.34 1.62 1.68 0.92 0.52PCB 180 0.69 1.83 1.22 0.36 0.15 1.86 4.74 1.29 0.76 0.06 0.36 0.37 1.18 1.43PCB 187 1.48 2.58 0.63 0.98 2.61 4.46 0.66 0.06 0.96 0.69 1.13 0.67PCB 194 0.60 1.31 1.23 1.50 0.13 1.72 4.73 1.58 0.62 0.51 1.14 0.09PCB 195 0.25 3.64 1.17 1.98 3.41 4.63 0.37 1.12 0.34 0.96 2.03PCB 206 1.32 0.94 0.96 1.11 0.09 1.27 0.06 0.48 1.15 0.43 3.65 0.71PCB 209 1.14 1.73 1.41 1.02 0.12 1.41 0.16 0.03 2.06 0.16 3.14 3.86
Table 25 (cont). p scores (15%) for PCBs in Marine Sediment XII and SRM 1941b

Laboratory No. 18 18 19 19 20 20

QA03SED12 1944 QA03SED12 1941b QA03SED12 1941b

PCB 8 1.45 1.75 0.65 0.53PCB 18 0.52 0.56 0.56 1.00 0.74PCB 28 0.37 0.81 1.77 0.63 0.51PCB 31 0.84PCB 44 0.63 0.55 0.88 0.31 0.38PCB 49 0.59 0.60 0.56PCB 52 0.87 0.73 0.02 0.09 0.36PCB 66 0.69 0.99 0.30 1.50 0.62PCB 95 0.85 0.85 0.71PCB 99 0.89 0.66 0.30PCB 101 0.80 0.80 0.63 0.15 0.17PCB 105 0.68 0.70 0.57 0.51 0.69PCB 118 0.76 0.72 0.58 0.43 0.32PCB 128 2.01 0.92 0.80 0.66 0.69PCB 138 0.88 0.63 0.47 0.59 0.31PCB 149 0.87 0.71 0.39PCB 153 0.80 0.69 0.32 0.37 0.45PCB 156 1.07 1.29 0.47PCB 170 0.92 0.76 0.25 0.64 1.84PCB 180 0.82 0.34 0.42 0.56 0.64PCB 187 1.03 0.43 0.19 1.97 0.61PCB 194 0.16 0.69 0.92PCB 195 1.64 1.34 0.51 0.55 0.84PCB 206 0.63 0.45 0.18 0.44 0.80PCB 209 0.99 0.71 1.20 0.77 1.48
 

Table 26. Comparison to Previous Exercise Assigned Values for the PAHs (ng/g dry basis)

PAHs Mussel Tissue Marine Sediment

QA92TIS4 QA98TIS9 QA03TIS11 QA98SED8 QA03SED12

14 labs 20 labs 20 labs 29 labs 20 labs

naphthalene 25.1 (5.7) 25.7 (6.2) 24.4 (9.5) 107 (29) 117 (39)

2-methylnaphthalene 40.5 (10.3) 33.1 (12.2) 25.2 (8.7) 77.4 (19.1) 80.6 (29.3)

1-methylnaphthalene 24.3 (4.8) 23.3 (8.5) 18.3 (9.6) 50.7 (13.2) 54.2 (16.5)

biphenyl 22.9 (14.5) 12.2 (1.0) 11.8 (3.8) 36.6 (12.9) 28.2 (9.3)

2,6-dimethylnaphthalene 65.8 (31.9) 38.8 (13.3) 30.8 (5.8) 51.2 (15.4) 39.7 (19.9)

acenaphthylene 8.69 (3.20) 7.87 (3.16) 6.49 (1.9) 50.2 (27.0) 52.0 (34.5)

acenaphthene 9.07 (1.59) 9.46 (1.42) 11.7 (5.7) 38.2 (7.3) 37.1 (7.4)

1,6,7-trimethylnaphthalene 41.8 (14.6) 31.3 (13.6) 27.8 (9.3) 27.2 (8.9) 28.6 (6.6)

fluorene 22.2 (4.6) 21.4 (1.9) 25.2 (10.3) 67.9 (18.4) 62.6 (15.2)

phenanthrene 144 (25) 126 (22) 120 (15) 604 (127) 505 (100)

anthracene 17.5 (10.1) 11.3 (4.3) 10.4 (0.2) 183 (57) 147 (60)

1-methylphenanthrene 67.8 (7.4) 60.2 (13.6) 49.1 (9.6) 87.3 (23.3) 70.5 (15.2)

fluoranthene 395 (80) 322 (56) 313 (43) 1293 (374) 1070 (203)

pyrene 282 (48) 224 (63) 227 (30) 1367 (383) 1099 (216)

benz[a]anthracene 79.4 (16.3) 77.5 (15.3) 71.3 (13.9) 551 (109) 442 (105)

chrysene 142 (27) 640 (170)

triphenylene 69.4 (na) 144 (24)

chrysene+triphenylene 227 (52) 196 (44) 181 (31) 944 (246) 817 (185)

benzo[b ]fluoranthene 81.3 (13.6) 999 (358)

benzo[j]fluoranthene 37.5 (11.5) 280 (4)

benzo[k ]fluoranthene 38.1 (14.3) 392 (98)

benzo[b+j+k ]fluoranthene 158 (26) 146 (31) 2110 (635)

benzo[e]pyrene 114 (22) 99.5 (23.7) 98.8 (16.4) 805 (186) 657 (186)

benzo[a]pyrene 29.4 (5.7) 25.9 (3.5) 30.7 (11.9) 832 (210) 718 (238)

perylene 11.3 (3.0) 8.13 (1.58) 10.2 (2.9) 248 (52) 211 (60)

indeno[1,2,3-cd]pyrene 20.0 (7.1) 18.0 (4.4) 22.7 (9.3) 710 (219) 680 (214)

dibenz[a,h]anthracene 4.22 (1.52) 137 (66)

dibenz[a,h]+[a,c]anthracene 7.56 (6.89) 4.36 (2.53) 10.4 (na) 161 (43)

benzo[ghi]perylene 26.0 (9.7) 21.2 (5.2) 24.3 (9.2) 683 (229) 608 (200)
 

Table 27. Comparison to Previous Exercise Assigned Values for the Pesticides (ng/g dry basis)

Pesticides Mussel Tissue Marine Sediment

QA92TIS4 QA98TIS9 QA03TIS11 QA98SED8 QA03SED12

14 labs 20 labs 20 labs 29 labs 20 labs

alpha-HCH (a-BHC) 1.62 (0.81) <10 <2 <2

hexachlorobenzene 0.43 (0.49) 1.08 (0.91) <10 <3 0.315 (0.123)

gamma-HCH (g-BHC,lindane 3.53 (4.24) 1.26 (0.86) <10 <2 <3

beta-HCH (b-BHC) <10 <2 <2

heptachlor 1.33 (1.54) <5 2.92 (2.34) <2 <2

aldrin 2.51 (2.30) <3 <10 <2 <2

heptachlor epoxide 4.43 (5.10) 2.25 (0.33) <10 <2 <2

oxychlordane 3.48 (1.73) 3.67 (na) <2 <2

gamma-chlordane 12.3 (2.9) 13.2 (5.7) 1.65 (0.41) 0.753 (0.466)

2,4'-DDE 15.8 (12.9) <5 2.51 (na) <2 0.782 (0.299)

endosulfan I <2 <10 <2 <2

cis-chlordane (alpha-chlordan 16.3 (5.5) 14.7 (3.7) 13.3 (2.9) 1.76 (0.83) 0.639 (0.326)

trans-nonachlor 13.0 (4.2) 13.6 (2.1) 12.5 (3.1) 0.489 (0.259)0.271 (0.144)

dieldrin 10.3 (7.5) 5.49 (1.27) 4.63 (0.56) <2 0.978 (0.523)

4,4'-DDE 45.2 (4.2) 34.0 (8.0) 32.1 (6.2) 6.88 (2.00) 7.30 (3.28)

2,4'-DDD 11.3 (5.1) 11.5 (4.0) 10.3 (1.9) 7.15 (2.19) 6.93 (3.12)

endrin <2 <10 <2 <2

endosulfan II 2.73 (0.54) <10 <2 <2

4,4'-DDD 25.6 (9.7) 29.3 (7.6) 28.3 (10.9) 17.3 (6.3) 15.3 (2.8)

2,4'-DDT 6.31 (4.35) 7.51 (2.53) 8.02 (2.91) 5.14 (1.49) 5.09 (1.61)

cis-nonachlor 6.27 (1.93) 4.83 (2.01) 1.73 (1.01) 1.38 (0.79)

4,4'-DDT 10.3 (4.3) 9.30 (1.63) 10.1 (3.5) 19.4 (4.3) 18.6 (6.3)

mirex 1.32 (1.04) 1.75 (0.25) <10 <2 <2

endosulfan sulfate <10 <2

chlorpyrifos <10 <2
 

Table 28. Comparison to Previous Exercise Assigned Values for the PCBs (ng/g dry basis) and water content (%)

PCBs and Water Mussel Tissue Marine Sediment

QA92TIS4 QA98TIS9 QA03TIS11 QA98SED8 QA03SED12

14 labs 20 labs 20 labs 29 labs 20 labs

PCB 8 3.32 (2.37) 4.18 (2.32) 4.85 (2.91) 2.04 (1.51) 1.43 (0.77)

PCB 18 11.0 (5.4) 12.9 (4.5) 8.84 (2.06) 3.61 (1.42) 3.12 (1.01)

PCB 28 37.2 (16.8) 41.4 (9.6) 33.4 (4.6) 4.95 (1.68) 4.75 (1.19)

PCB 31 28.0 (4.5) 4.51 (1.41)

PCB 44 31.7 (11.9) 40.3 (8.7) 37.8 (21.8) 7.90 (3.04) 9.09 (2.30)

PCB 49 44.8 (10.3) 6.21 (1.91)

PCB 52 55.9 (11.2) 61.8 (10.8) 52.3 (8.1) 15.6 (6.3) 16.1 (4.6)

PCB 66 55.7 (13.8) 58.8 (9.1) 8.85 (3.51) 8.46 (2.22)

PCB 95 39.1 (9.9) 47.2 (7.8) 20.2 (7.7) 23.4 (10.1)

PCB 66/95 79.3 (22.1) 80.6 (23.5) 16.7(10.5)

PCB 99 48.5 (8.8) 11.5 (5.3)

PCB 101 96.3 (15.0) 92.2 (20.1) 88.3 (9.6) 33.3 (13.6) 34.9 (11.7)

PCB 105 37.9 (7.0) 36.2 (7.7) 33.4 (4.8) 11.9 (3.9) 12.2 (4.5)

PCB 118 92.1 (16.5) 96.1 (20.7) 82.0 (7.0) 29.7 (11.9) 27.6 (10.0)

PCB 128 12.8 (3.3) 16.1 (4.5) 13.3 (2.3) 8.22 (3.20) 7.65 (2.50)

PCB 138 84.7 (18.8) 36.7 (11.3)

PCB 138/163/164 106 (18) 102 (25) 44.9 (17.5)

PCB 149 54.1 (7.2) 26.6 (8.9)

PCB 153 114 (21) 113 (24) 102 (15) 50.6 (25.1) 41.5 (19.2)

PCB 156 5.79 (0.97) 4.43 (1.80)

PCB 170 1.90 (0.38) 3.01 (1.13) 1.98 (1.13) 12.6 (5.2) 9.11 (3.75)

PCB 180 9.16 (2.32) 15.5 (11.0) 7.95 (1.60) 21.7 (11.1) 19.1 (6.2)

PCB 187 24.3 (5.5) 27.5 (6.1) 22.8 (2.2) 11.5 (4.9) 10.8 (3.5)

PCB 194 <10 3.86 (2.16)

PCB 195 1.06 (1.03) 1.04 (0.55) <10 2.61 (1.22) 1.79 (0.63)

PCB 206 4.23 (7.11) <2 <10 3.30 (1.20) 2.57 (1.25)

PCB 209 0.84 (0.86) <2 <10 2.33 (1.23) 1.62 (1.10)

% water 91.8 (0.3) 91.4 (1.0) 91.5 (0.9)
 

Appendix A: Description, Storage, Use, and Reporting Instructions for 

Mussel Tissue XI (QA03TIS11) 
 

NIST Intercomparison Exercise Program for 

Organic Contaminants in the Marine Environment 

NIST QA Program

Intercomparison Exercise: Mussel Tissue XI 

Description of Materials and Instructions

Intercomparison Exercise Materials:

QA03TIS11 (Mussel Tissue XI)

Each of the three jars contains approximately 15 g (wet basis) of Mussel Tissue XI. This cryogenically 

homogenized fresh material was prepared from mussels collected from an urban area. This material 

has not been enriched or spiked and still contains its endogenous water. Each 2-oz clear glass jar has a 

Teflon-lined screw cap and is labeled with an individual jar number as well as the above name. 

In addition, three concurrent analyses of SRM 1974b, Organics in Mussel Tissue (Mytilus edulis), are 

recommended. Three jars of this material are enclosed and the appropriate tables from the draft 

Certificate of Analysis are attached to these instructions. 

Storage of Materials:

Mussel Tissue Material. The tissue material should be stored in the dark at temperatures of -20  ̊C or 

lower. If allowed to thaw or if stored for extended periods at temperatures higher than -40  ̊C, it will 

lose its powder-like form. If this happens, use the contents from the entire jar for analysis. This 

material has been stored at NIST at -80  ̊C and was shipped to you on dry ice. If only a portion of the 

contents of a jar is used, the jar should be tightly closed immediately after removal of a subsample to 

preserve the integrity of the remaining material for later analysis. 

Instructions for Use: 

You are to analyze Mussel Tissue XI and SRM 1974b, using your laboratory's and/or program's 

analytical protocols, for the concentrations (mass/mass [wet basis]) of the 26 polycyclic aromatic 

hydrocarbon (PAH) compounds, 25 chlorinated pesticides, and 25 polychlorinated biphenyl (PCB) 

congeners1

 of interest in the current NIST Intercomparison Exercise Program for Organic Contaminants 

in the Marine Environment. These compounds are listed in Table 1. 

 

1

If your laboratory is not analyzing samples for all three chemical classes, you are expected to submit results 

only for those compounds currently being determined in your laboratory. 
 

The percentage of water and of total extractable organics (or lipid) in Mussel Tissue XI and SRM 

1974b should also be determined. You should have received sufficient material so that you can 

perform separate determinations for the water content if you do not dry your tissue samples prior to 

analysis. 

The amount of material used for each analysis should correspond to the amount (wet basis) of marine 

tissue that you would typically analyze as prescribed in your protocols. It is best if the Mussel Tissue 

XI and the SRM 1974b samples are not allowed to thaw prior to the taking of samples for analysis; 

however, if the material has been even partially thawed, you should use the contents of the entire jar as 

a single sample as it is difficult to take representative samples from a jar once the material has thawed. 

After removing the material for analysis from the jars, the samples should be used without delay. 

You should analyze three samples of Mussel Tissue XI and at least one, and more if possible, of SRM 

1974b in three different batches/sets/strings/catalogs using your protocol for tissue samples. 

Specifically, we are asking that you analyze one sample of Mussel Tissue XI and one sample of SRM 

1974b with one batch of laboratory samples; analyze a second sample of each material with another 

batch; and the third sample with yet another batch. This will allow a more realistic assessment of 

laboratory precision over a longer term than the assessment obtained when a laboratory places all three 

samples in the same extraction and cleanup batch and the resulting extracts are analyzed using the same 

calibration curve, etc. 

Reporting of Results: 

Please report one result, as if three figures were significant, for each of the requested analytes in each of 

the three replicates of the Mussel Tissue XI and of SRM 1974b. Report results in units of ng/g wet

basis. Report the date of measurement of each sample in the requested m/d/y format. Also, report the 

results of your percentage water determinations of Mussel Tissue XI. 

We recognize that the reported concentrations for some of the requested determinands will probably 

include concentrations of compounds reported to coelute with the determinand of interest with methods 

commonly in use in environmental laboratories. Please note at the bottom of your table of reported 

results if any coelution qualifiers are applicable to your data. Please note that any changes you make to 

the column or row headings within the tables will not be seen by the coordinators because only the 

table entries and comments at the bottom of the tables are automatically transferred to the exercise 

database. 

We prefer that concentration values be reported for each analyte determined. If the measured 

concentration is below your typical reporting concentration for an analyte in a particular matrix, you 

can report the number and list the appropriate detection limit, quantification limit, etc. at the bottom of 

the data table. However, if you need to report non-numerical data please use the following 

conventions: 

NA "Not analyzed", "not determined" 

<"value" "Less than specified concentration", e.g., <8 ng/g 

Other "Other"; add note of explanation at end of data table, e.g., interference 
 

DL "Below detection limit" may be used, however, <"value" is preferable 

Do not use negative numbers or parentheses to indicate "less than detection limits". 

The attached file is an EXCEL file, TIS11.xls. If you have any software/hardware conversion problems, 

please contact Michele Schantz. The data file templates also include places for you to list the 

surrogate/internal standards and type of calibration curve used, and to provide a brief description of the 

analyses. Please do not add spaces before entering numbers in the table cells and enter them as 

"numbers" not as "labels". Please do not insert any columns or rows within the table in the data file. If 

you wish to include additional data and/or other information or comments, you may add it to the bottom 

of the data table in the diskette file or send it in hard copy. A printout of the data file format is shown 

in Table 2. 

Submit your results by July 11, 2003 as an attached file via e-mail to: 

E-mail: michele.schantz@nist.gov 

Further Information:

If you need further information, please contact Michele at the following address or phone numbers: 

Michele M. Schantz 

NIST 

100 Bureau Drive Stop 8392 

 Gaithersburg, MD 20899-8392 

Phone: (301)975-3106 

FAX: (301)977-0685 
 

Table 1: Analytes of Interest in NIST Intercomparison Exercise Program for Organic 

Contaminants in the Marine Environment 

Chlorinated Pesticides 

hexachlorobenzene 2,4'-DDE 

alpha-HCH (alpha-BHC) 4,4'-DDE 

beta-HCH (beta-BHC) 2,4'-DDD 

gamma-HCH (gamma-BHC, Lindane) 4,4'-DDD 

heptachlor 2,4'-DDT 

heptachlor epoxide 4,4'-DDT 

cis-chlordane (alpha-chlordane) chlorpyrifos 

trans-chlordane (gamma-chlordane) aldrin 

oxychlordane dieldrin 

cis-nonachlor endrin 

trans-nonachlor endosulfan I 

mirex endosulfan II 

endosulfan sulfate 

Polychlorinated Biphenyl Congeners

 PCB No. Compound Name

 8 2,4'-dichlorobiphenyl 

 18 2,2',5-trichlorobiphenyl 

 28 2,4,4'-trichlorobiphenyl 

 31 2,4',5-trichlorobiphenyl 

 44 2,2',3,5'-tetrachlorobiphenyl 

 49 2,2',4,5'-tetrachlorobiphenyl 

 52 2,2',5,5'-tetrachlorobiphenyl 

 66 2,3',4,4'-tetrachlorobiphenyl 

 95 2,2',3,5',6-pentachlorobiphenyl 

 99 2,2',4,4',5-pentachlorobiphenyl 

 101 2,2',4,5,5'-pentachlorobiphenyl 

 105 2,3,3',4,4'-pentachlorobiphenyl 

 118 2,3',4,4',5-pentachlorobiphenyl 

 128 2,2',3,3',4,4'-hexachlorobiphenyl 

 138 2,2',3,4,4',5'-hexachlorobiphenyl 

 149 2,2',3,4',5',6-hexachlorobiphenyl 

 153 2,2',4,4',5,5'-hexachlorobiphenyl 

 156 2,3,3',4,4',5-hexachlorobiphenyl 

 170 2,2',3,3',4,4',5-heptachlorobiphenyl 

 180 2,2',3,4,4',5,5'-heptachlorobiphenyl 

 187 2,2',3,4',5,5',6-heptachlorobiphenyl 

 194 2,2',3,3',4,4',5,5'-octachlorobiphenyl 

 195 2,2',3,3',4,4',5,6-octachlorobiphenyl 

 206 2,2',3,3',4,4',5,5',6-nonachlorobiphenyl 

 209 decachlorobiphenyl 
 

Table 1. (continued) 

Polycyclic aromatic hydrocarbons (PAH)

naphthalene pyrene 

2-methylnaphthalene benz[a]anthracene 

1-methylnaphthalene chrysene 

biphenyl triphenylene 

2,6-dimethylnaphthalene benzo[b]fluoranthene 

acenaphthylene benzo[j]fluoranthene 

acenaphthene benzo[k]fluoranthene 

1,6,7-trimethylnaphthalene benzo[e]pyrene 

fluorene benzo[a]pyrene 

phenanthrene perylene 

anthracene indeno[1,2,3-cd]pyrene 

1-methylphenanthrene dibenz[a,h]anthracene 

fluoranthene benzo[ghi]perylene 

 
 

Table 2. Diskette Data File Format (File: TIS11.*)

NIST Intercomparison Exercise Program for Organics in the Marine Environment

NIST QA Program

Sample: QA03TIS11 - Mussel Tissue XI

Please fill in all blanks; Use requested units of concentration; Report results as if 3 figures were significant

DO NOT INSERT ROWS OR COLUMNS WITHIN THIS TABLE. DO NOT MOVE CELLS.

 - If necessary, add additional data/information at the end of the table.

 - Use one of the following if no concentration is reported for an analyte:

 NA = Not analyzed/determined; <"conc" = <detection limit conc.; Other = other, explain in a note at end of table

 (DL = "below detection limit" may be used, but <"conc", e.g., <8, is preferable.)

 Do not use parentheses or negative numbers to indicate "less than detection limit".

Reporting Date (m/d/y): _______________________

Laboratory: _______________________

Submitted by: _______________________

BRIEF DESCRIPTION OF PROCEDURES USED:

Approximate amount of sample extracted: Mussel XI ___________ g, wet basis; SRM 1974b ___________ g, wet basis

Method used for determining percentage water: ______________________________________________________________________

Method used for determining percentage total organic ______________________________________________________________________

extractables (lipid): ______________________________________________________________________

Were "wet" or "dry" samples extracted? Mussel XI ___________ SRM 1974b ___________

Extraction method: ____________________________________________________________________________________________

Extraction solvent: ____________________________________________________________________________________________

Extraction time: ____________________________________________________________________________________________

Extraction - other: ____________________________________________________________________________________________

____________________________________________________________________________________________

Sample extract cleanup method: ____________________________________________________________________________________________

____________________________________________________________________________________________

____________________________________________________________________________________________

____________________________________________________________________________________________

____________________________________________________________________________________________

Analytical method used (e.g., GC-FID, GC-ECD):

Analyt. Instr. Column Phase Col. Length, m Col. i.d., mm Col. film thickness, μm

PAH __________________ ________________________________________________________________________

 Pesticides __________________ ________________________________________________________________________

 PCB Congeners __________________ ________________________________________________________________________

Method of quantitation (IS = internal standard, ES = external standard):

 PAH __________________

 Pesticides __________________

 PCB Congeners __________________

IF internal standard method was used, please complete the following section:

 Identity of internal standards/surrogates used that were:

 Added PRIOR to extraction of sample:

 PAH ________________________________________________________________________

 Pesticides ________________________________________________________________________

 PCB Congeners ________________________________________________________________________

 Added after extraction/cleanup and JUST PRIOR to chromatographic analysis:

PAH ________________________________________________________________________

Pesticides ________________________________________________________________________

 PCB Congeners ________________________________________________________________________

 Any others? Added at what point in analyses: __________________________________________________________

PAH ________________________________________________________________________

Pesticides ________________________________________________________________________

 PCB Congeners ________________________________________________________________________

 IS/surrogate standards used for quantitation calculations were: 

________ those added prior to extraction

________ those added after extraction/cleanup and just prior to chromatographic analysis

 If the IS/surrogates added after extraction/cleanup extraction were used for quantitation, 

 were results corrected for percent recovery? __________________

 Percent recovery range: PAH __________________

Pesticides __________________

PCB Congeners __________________
 

Calibration Curve

Analytes outside of calibration 

Points Conc. Range curve calibration range

 PAH __________________ __________________ __________________________________

 Pesticides __________________ __________________ __________________________________

 PCB Congeners __________________ __________________ __________________________________

Were PCB congeners separated from pesticides prior to GC? __________________

Please note any differences in procedures used for SRM 19 74b analyses from those for Mussel TIssue XI described above:

_____________________________________________________________________________________________________________________

_____________________________________________________________________________________________________________________

_____________________________________________________________________________________________________________________

_____________________________________________________________________________________________________________________

_____________________________________________________________________________________________________________________

RESULTS:

PERCENT WATER (List each result if determined more than once. Enter results as a number, for example 90.0. DO NOT change format of cell to percent.)

Mussel TIssue XI Mussel TIssue XI Mussel TIssue XI SRM 1974b SRM 1974b SRM 1974b

(percent) (percent) (percent) (percent) (percent) (percent)

Water __________ __________ __________ 

PAH ANALYSES Mussel TIssue XI Mussel TIssue XI Mussel TIssue XI SRM 1974b SRM 1974b SRM 1974b

Batch A Batch B Batch C Batch A Batch B Batch C

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

Analyst (Initials) __________ __________ __________ __________ __________ __________ 

Date(s) of measurements (m/d/y) __________ __________ __________ __________ __________ __________ 

Sample Jar number __________ __________ __________ 

Mussel TIssue XI Mussel TIssue XI Mussel TIssue XI SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

naphthalene __________ __________ __________ __________ __________ __________ 

2-methylnaphthalene __________ __________ __________ __________ __________ __________ 

1-methylnaphthalene __________ __________ __________ __________ __________ __________ 

biphenyl __________ __________ __________ __________ __________ __________ 

2,6-dimethylnaphthalene __________ __________ __________ __________ __________ __________ 

acenaphthylene __________ __________ __________ __________ __________ __________ 

acenaphthene __________ __________ __________ __________ __________ __________ 

1,6,7-trimethylnaphthalene __________ __________ __________ __________ __________ __________ 

fluorene __________ __________ __________ __________ __________ __________ 

phenanthrene __________ __________ __________ __________ __________ __________ 

anthracene __________ __________ __________ __________ __________ __________ 

1-methylphenanthrene __________ __________ __________ __________ __________ __________ 

fluoranthene __________ __________ __________ __________ __________ __________ 

pyrene __________ __________ __________ __________ __________ __________ 

benz[a]anthracene __________ __________ __________ __________ __________ __________ 

chrysene __________ __________ __________ __________ __________ __________ 

triphenylene __________ __________ __________ __________ __________ __________ 

benzo[b ]fluoranthene __________ __________ __________ __________ __________ __________ 

benzo[j]fluoranthene __________ __________ __________ __________ __________ __________ 

benzo[k ]fluoranthene __________ __________ __________ __________ __________ __________ 

benzo[e]pyrene __________ __________ __________ __________ __________ __________ 

benzo[a]pyrene __________ __________ __________ __________ __________ __________ 

perylene __________ __________ __________ __________ __________ __________ 

indeno[1,2,3-cd]pyrene __________ __________ __________ __________ __________ __________ 

dibenz[a,h]anthracene __________ __________ __________ __________ __________ __________ 

benzo[ghi]perylene __________ __________ __________ __________ __________ __________ 
 

PESTICIDE ANALYSES Mussel TIssue XI Mussel TIssue XI Mussel TIssue XI SRM 1974b SRM 1974b SRM 1974b

Batch A Batch B Batch C Batch A Batch B Batch C

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

Analyst (Initials) __________ __________ __________ __________ __________ __________ 

Date(s) of measurements (m/d/y) __________ __________ __________ __________ __________ __________ 

Sample Jar number __________ __________ __________ 

Mussel TIssue XI Mussel TIssue XI Mussel TIssue XI SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

alpha-HCH (a-BHC) __________ __________ __________ __________ __________ __________ 

hexachlorobenzene __________ __________ __________ __________ __________ __________ 

gamma-HCH (g-BHC,lindane) __________ __________ __________ __________ __________ __________ 

beta-HCH (b-BHC) __________ __________ __________ __________ __________ __________ 

heptachlor __________ __________ __________ __________ __________ __________ 

aldrin __________ __________ __________ __________ __________ __________ 

heptachlor epoxide __________ __________ __________ __________ __________ __________ 

oxychlordane __________ __________ __________ __________ __________ __________ 

gamma-chlordane __________ __________ __________ __________ __________ __________ 

2,4'-DDE __________ __________ __________ __________ __________ __________ 

endosulfan I __________ __________ __________ __________ __________ __________ 

cis-chlordane (alpha-chlordane) __________ __________ __________ __________ __________ __________ 

trans-nonachlor __________ __________ __________ __________ __________ __________ 

dieldrin __________ __________ __________ __________ __________ __________ 

4,4'-DDE __________ __________ __________ __________ __________ __________ 

2,4'-DDD __________ __________ __________ __________ __________ __________ 

endrin __________ __________ __________ __________ __________ __________ 

endosulfan II __________ __________ __________ __________ __________ __________ 

4,4'-DDD __________ __________ __________ __________ __________ __________ 

2,4'-DDT __________ __________ __________ __________ __________ __________ 

cis-nonachlor __________ __________ __________ __________ __________ __________ 

4,4'-DDT __________ __________ __________ __________ __________ __________ 

mirex __________ __________ __________ __________ __________ __________ 

endosulfan sulfate __________ __________ __________ __________ __________ __________ 

chlorpyrifos __________ __________ __________ __________ __________ __________ 

PCB CONGENER ANALYSES Mussel TIssue XI Mussel TIssue XI Mussel TIssue XI SRM 1974b SRM 1974b SRM 1974b

Batch A Batch B Batch C Batch A Batch B Batch C

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

Analyst (Initials) __________ __________ __________ __________ __________ __________ 

Date(s) of measurements (m/d/y) __________ __________ __________ __________ __________ __________ 

Sample Jar number __________ __________ __________ 

Mussel TIssue XI Mussel TIssue XI Mussel TIssue XI SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

PCB 8 __________ __________ __________ __________ __________ __________ 

PCB 18 __________ __________ __________ __________ __________ __________ 

PCB 28 __________ __________ __________ __________ __________ __________ 

PCB 31 __________ __________ __________ __________ __________ __________ 

PCB 44 __________ __________ __________ __________ __________ __________ 

PCB 49 __________ __________ __________ __________ __________ __________ 

PCB 52 __________ __________ __________ __________ __________ __________ 

PCB 66 __________ __________ __________ __________ __________ __________ 

PCB 95 __________ __________ __________ __________ __________ __________ 

PCB 99 __________ __________ __________ __________ __________ __________ 

PCB 101 __________ __________ __________ __________ __________ __________ 

PCB 105 __________ __________ __________ __________ __________ __________ 

PCB 118 __________ __________ __________ __________ __________ __________ 

PCB 128 __________ __________ __________ __________ __________ __________ 

PCB 138 __________ __________ __________ __________ __________ __________ 

PCB 149 __________ __________ __________ __________ __________ __________ 

PCB 153 __________ __________ __________ __________ __________ __________ 

PCB 156 __________ __________ __________ __________ __________ __________ 

PCB 170 __________ __________ __________ __________ __________ __________ 

PCB 180 __________ __________ __________ __________ __________ __________ 

PCB 187 __________ __________ __________ __________ __________ __________ 

PCB 194 __________ __________ __________ __________ __________ __________ 

PCB 195 __________ __________ __________ __________ __________ __________ 

PCB 206 __________ __________ __________ __________ __________ __________ 

PCB 209 __________ __________ __________ __________ __________ __________ 

(percent) (percent) (percent) (percent) (percent) (percent)

total extractable organics (lipid) __________ __________ __________ __________ __________ __________ 

(Any additional data/information should be added here.)
 

Draft Certificate Table 1. Certified Concentrations for Selected PAHs in SRM 1974b 

mass fractions in μg/kga

 

 wet-mass basis dry-mass basis 

 

Naphthalened,e,f,g,h,i,j 2.43 ± 0.12b

 24.0 ± 1.2b

Fluorened,e,f,g,h,i,j 0.494 ± 0.036b 4.88 ± 0.36b

Phenanthrened,e,f,g,h,i ,j 2.58 ± 0.11b

 25.5 ± 1.1b

Anthracened,e,f,g,h,i,j 0.527 ± 0.071c

 5.20 ± 0.71c

1-Methylphenanthrened,e,f,g,h,i,j 0.98 ± 0.13c

 9.66 ± 1.3c

2-Methylphenathrened,e,f,g 1.28 ± 0.31b 24.0 ± 1.2b

3-Methylphenanthrened,e,g 1.27 ± 0.04c

 12.5 ± 0.4c

Fluoranthened,e,f,g,h,i,j 17.1 ± 0.7b 169 ± 7b

Pyrened,e,f,g,h,i,j 18.04 ± 0.6b 178 ± 6b

Benz[a]anthracened,e,f,g,h,i,j 4.74 ± 0.53b

 46.8 ± 5.2b

Chrysened,g,h 6.3 ± 1.0b 62.2 ± 9.9b

Triphenylened,g,h 4.33 ± 0.72b

 42.7 ± 7.1b

Benzo[b]fluoranthenee,f,g,h,i,j 6.46 ± 0.59b

 63.8 ± 5.8b

Benzo[j]fluoranthenee,f,g,h,i 2.99 ± 0.29b

 29.5 ± 2.9b

Benzo[k]fluoranthened,e,f,g,h,i,j 3.16 ± 0.18b

 31.2 ± 1.8b

Benzo[a]fluoranthened,e,f,g 0.634 ± 0.074b

 6.26 ± 0.73b

Benzo[e]pyrened,e,f,g,h,i,j 10.3 ± 1.1b 102 ± 11b

Benzo[a]pyrened,e,f,g,h,i,j 2.80 ± 0.38b

 27.6 ± 3.8b

Perylened,e,f,g,h,i,j 0.99 ± 0.14b 9.8 ± 1.4b

Benzo[ghi]perylened,e,f,g,h,i,j 3.12 ± 0.33b

 30.8 ± 3.3b

Indeno[1,2,3-cd]pyrened,e,f,g,h,i,j 2.14 ± 0.11b

 21.1 ± 1.1b

Dibenz[a,h]anthracenee,f,g,h,i 0.327 ± 0.031c 3.23 ± 0.31c

a

 Concentrations reported on both wet- and dry-mass basis; material as received contains 89.87 % ± 0.05 % (95 % confidence 

level) water. b

 Certified values are weighted means of the results from three to seven analytical methods [17]. The uncertainty listed with 

each value is an expanded uncertainty about the mean, with coverage factor 2 (approximately 95% confidence), calculated by 

combining a between-method variance incorporating inter-method bias with a pooled within-source variance following the 

ISO/NIST Guide to the Expression of Uncertainty in Measurements [2]. c

 The certified value is an unweighted mean of the results from three to seven analytical methods. The uncertainty listed with 

the value is an expanded uncertainty about the mean, with coverage factor 2, calculated by combining a between-method 

variance [18] with a pooled, within method variance following the ISO/NIST Guide to the Expression of Uncertainty in 

Measurement [2]. Note for anthracene and 1-methylphenanthrene the within method variance for the interlaboratory study was 

not used for the calculation of the expanded uncertainty. d

 GC/MS (Ia) on a relatively non-polar proprietary phase after PFE with 50% hexane/50% acetone mixture. e

 GC/MS (Ib) on 50% phenyl-substituted methylpolysiloxane phase; same extracts analyzed as in GC/MS (Ia). f

 GC/MS (II) on 50% phenyl-substituted methylpolysiloxane phase after PFE with DCM. g

 GC/MS (III) on a relatively non-polar proprietary phase and 50% phenyl-substituted methylpolysiloxane phase after Soxhlet 

extraction with DCM. h

 GC/MS (IV) on a relatively non-polar proprietary phase after Soxhlet extraction with DCM. i

 GC/MS (V) on 50% phenyl-substituted methylpolysiloxane phase after PFE with DCM. 

j

 2000 Interlaboratory Comparison Study [10] with 16 laboratories submitting data.
 

Draft Certificate Table 2. Certified Concentrations for Selected PCB Congenersa in SRM 1974b 

 mass fractions in μg/kgb

 wet-mass basis dry mass basis 

 PCB 18 (2,2',5-Trichlorobiphenyl)e,f,g,h,i,j,k,l 0.84 ± 0.13c 8.30 ± 1.3c

 PCB 28 (2,4,4'-Trichlorobiphenyl)e,f,g,h,j.k.l 3.43 ± 0.25c 33.9 ± 2.5c

 PCB 31 (2,4',5-Trichlorobiphenyl)e,f,g,h,i,j,k,l 2.88 ± 0.23c 28.4 ± 2.3c

 PCB 44 (2,2'3,5'-Tetrachlorobiphenyl)e,f,g,h,i,j,k,l 3.85 ± 0.20c 38.0 ± 2.0c

 PCB 49 (2,2'4,5'-Tetrachlorobiphenyl)e,f,g,h,i,j,k,l 5.66 ± 0.23c 55.9 ± 2.3c

 PCB 52 (2,2',5,5'-Tetrachlorobiphenyl)e,f,g,h,i,j,k,l 6.26 ± 0.37c 61.8 ± 3.7c

 PCB 66 (2,3',4,4'-Tetrachlorobiphenyl)e,f,g,h,j,k,l 6.37 ± 0.37c

 62.9 ± 3.7c

 PCB 70 (2,3’,4’,5-Tetrachlorobiphenyl)e,f,h,i 6.01 ± 0.22d 59.3 ± 2.2d

 PCB 74 (2,4,4’,5-Tetrachlorobiphenyl)e,f,h,i 3.55 ± 0.23c 35.0 ± 2.3c

 PCB 82 (2,2’,3,3’,4-Pentachlorobiphenyl)e,f,g,i 1.16 ± 0.14c 11.5 ± 1.4c

 PCB 87 (2,2',3,4,5'-Pentachlorobiphenyl)e,f,i 4.33 ± 0.36d 42.7 ± 3.6d

 PCB 95 (2,2',3,5',6-Pentachlorobiphenyl)e,f,g,h,j,k,l 6.04 ± 0.36c 59.6 ± 3.6c

 PCB 99 (2,2',4,4',5-Pentachlorobiphenyl)e,f,g,h,i,j,k,l 5.92 ± 0.27c 58.4 ± 2.7c

 PCB 101 (2,2',4,5,5'-Pentachlorobiphenyl)e,f,h,i,j,k,l 10.7 ± 1.1c 106 ± 11c

 PCB 105 (2,3,3',4,4'-Pentachlorobiphenyl)e,f,g,h,i,j,k,l 4.00 ± 0.18c 39.5 ± 1.8c

 PCB 107 (2,3,3’,4,5’-Pentachlorobiphenyl)e,f,g,h,i 1.03 ± 0.12c 10.2 ± 1.2c

 PCB 110 (2,3,3',4',6-Pentachlorobiphenyl)e,f,h 10.0 ± 0.7c 99.1 ± 7.1c

 PCB 118 (2,3',4,4',5-Pentachlorobiphenyl)e,f,g,h,i,j,k,l 10.3 ± 0.4c 102 ± 4c

 PCB 128 (2,2',3,3',4,4'-Hexachlorobiphenyl)e,f,g,h,i,j,k,l 1.79 ± 0.12c 17.7 ± 1.2c

 PCB 132 (2,2’,3,3’,4,6’-Hexachlorobiphenyl)e,f,g,h,i 2.43 ± 0.25c 24.0 ± 2.5c

 PCB 138 (2,2',3,4,4',5'-Hexachlorobiphenyl)e,f,h,j,k,l 9.2 ± 1.4c 91 ± 14c

 PCB 146 (2,2’,3,4’,5,5’-Hexachlorobiphenyl)e,f,g,h 1.92 ± 0.16c 19.0 ± 1.6c

 PCB 149 (2,2',3,4',5',6-Hexachlorobiphenyl)e,f,h,i,j,k,l 7.01 ± 0.28c

 69.2 ± 2.8c

 PCB 151 (2,2’,3,5,5’,6-Hexachlorobiphenyl)e,f,g,i 1.86 ± 0.16c 18.4 ± 1.6c

 PCB 153 (2,2',4,4',5,5'-Hexachlorobiphenyl)e,f,g,h,i,j,k,l 12.3 ± 0.8c 121 ± 8c

 PCB 156 (2,3,3',4,4',5-Hexachlorobiphenyl)e,f,h,j,k,l 0.718± 0.080c 7.09 ± 0.79c

 PCB 158 (2,3,3’,4,4’,6-Hexachlorobiphenyl)e,g,h,i 0.999± 0.096c 9.86 ± 0.95c

 PCB 170 (2,2',3,3',4,4',5-Heptachlorobiphenyl)e,f,h,j,k,l 0.269± 0.034c 2.66 ± 0.34c

 PCB 180 (2,2',3,4,4',5,5'-Heptachlorobiphenyl)e,f,g,h,i,j,k,l 1.17 ± 0.10c 11.5 ± 1.0c

 PCB 183 (2,2',3,4,4',5',6-Heptachlorobiphenyl)e,f,g,h,i 1.25 ± 0.03c 12.3 ± 0.3c

 PCB 187 (2,2',3,4',5,5',6-Heptachlorobiphenyl)e,f,g,h,i,j,k,l 2.94 ± 0.15c 29.0 ± 1.5c

a

 PCB congeners are numbered according to the scheme proposed by Ballschmiter and Zell [19] and later revised by Schulte and Malisch [20] to conform 

with IUPAC rules; for the specific congeners mentioned in this SRM, only PCB 107 is different in the numbering systems. Under the Ballschmiter and 

Zell numbering system, the IUPAC PCB 107 is listed as PCB 108. 

b

 Concentrations reported on both wet- and dry-mass basis; material as received contains 89.87 % ± 0.05 % (95 % confidence level) water. c

 Certified values are weighted means of the results from three to eight analytical methods [17]. The uncertainty listed with each value is an expanded 

uncertainty about the mean, with coverage factor 2 (approximately 95% confidence), calculated by combining a between-method variance incorporating 

inter-method bias with a pooled within-source variance following the ISO/NIST Guide to the Expression of Uncertainty in Measurements [2]. d

 The certified value is an unweighted mean of the results from three analytical methods. The uncertainty listed with the value is an expanded uncertainty 

about the mean, with coverage factor 2, calculated by combining a between-method variance [18] with a pooled, within method variance following the 

ISO/NIST Guide to the Expression of Uncertainty in Measurement [2]. e GC/MS (Ia) on a relatively non-polar proprietary phase after PFE with 50% hexane/50% acetone mixture. f. GC/MS (Ib) on 50 % phenyl-substituted methylpolysiloxane phase; same extracts analyzed as in GC/MS (Ia). g

 GC-ECD (Ia) on 5 % phenyl-substituted methylpolysiloxane phase after PFE with DCM. h

 GC-ECD (Ib) on a relatively non-polar proprietary phase; same extracts as GC-ECD (Ia). i

 GC-ECD (II) on a 5% phenyl-substituted methylpolysiloxane phase after Soxhlet extraction with DCM. 

j GC/MS (II) on a relatively non-polar proprietary phase after Soxhlet extraction with DCM. k

 GC-ECD (III) on a 5% phenyl-substituted methylpolysiloxane phase and a relatively non-polar proprietary phase after PFE with DCM. l

 2000 Interlaboratory Comparison Study [10] with 16 laboratories submitting data. 
 

Draft Certificate Table 3. Certified Concentrations for Selected Chlorinated Pesticides in SRM 1974b 

 mass fractions in μg/kga,b

 wet-mass basis dry-mass basis 

 

 cis-Chlordanec,d,e,f,g,h,i,j 1.36 ± 0.10 13.4 ± 1.0 

 trans-Chlordanec,d,e,f,g,h,i,j 1.14 ± 0.17 11.3 ± 1.7 

 trans-Nonachlorc,d,e,f,g,h,i,j 1.30 ± 0.14 12.8 ± 1.4 

 2,4’-DDEc,d,h,i,j 0.336 ± 0.044 3.32 ± 0.43 

 4,4’-DDEc,d,e,f,g,h,i,j 4.15 ± 0.38 41.0 ± 3.8 

 2,4’-DDDc,d,e,f,h,i,j 1.09 ± 0.16 10.8 ± 1.6 

 4,4’-DDDc,d,e,f,g,h,i,j 3.34 ± 0.22 33.0 ± 2.2 

a Concentrations reported on both wet- and dry-mass basis; material as received contains 89.87 % ± 0.05 % (95 % confidence level) 

water. b

 Certified values are weighted means of the results from five to eight analytical methods [17]. The uncertainty listed with each value is 

an expanded uncertainty about the mean, with coverage factor 2 (approximately 95% confidence), calculated by combining a betweensource variance incorporating inter-method bias with a pooled within-source variance following the ISO/NIST Guide to the Expression 

of Uncertainty in Measurements [2]. c GC/MS (Ia) on a relatively non-polar proprietary phase after PFE with 50% hexane/50% acetone mixture. d

 GC/MS (Ib) on 50 % phenyl-substituted methylpolysiloxane phase; same extracts analyzed as in GC/MS (Ia). e

 GC-ECD (Ia) on 5 % phenyl-substituted methylpolysiloxane phase after PFE with DCM. 

f

 GC-ECD (Ib) on a relatively non-polar proprietary phase; same extracts as GC-ECD (Ia). g

 GC-ECD (II) on a 5% phenyl-substituted methylpolysiloxane phase after Soxhlet extraction with DCM. h GC/MS (II) on a relatively non-polar proprietary phase after Soxhlet extraction with DCM. i

 GC-ECD (III) on a 5% phenyl-substituted methylpolysiloxane phase and a relatively non-polar proprietary phase after PFE with DCM. 

j

 2000 Interlaboratory Comparison Study [10] with 16 laboratories submitting data. 
 

Draft Certificate Table 4. Reference Concentrations for Selected PAHs in SRM 1974b 

mass fractions in μg/kga

 wet-mass basis dry-mass basis 

1-Methylnaphthalenee,f,g,h,i,j,k 0.614 ± 0.050b 6.06 ± 0.49b

2-Methylnaphthalenee,f,g,h,i,j,k 1.25 ± 0.09b 12.3 ± 0.9b

2,6-Dimethylnaphthalenee,f,g,h,i,j,k 0.33 ± 0.16b 3.3 ± 1.6b

2,3,5-Trimethylnaphthalenee,f,g,h,i,j,k 0.400 ± 0.032b 3.95 ± 0.32b

Biphenyle,f,g,h,i,j,k 0.61 ± 0.14b 6.0 ± 1.4b

Acenaphthylenee,f,g,h,i,j,k 0.48 ± 0.12b 4.7 ± 1.2b

Acenaphthenee,f,g,h,i,j,k 0.274 ± 0.054b 2.70 ± 0.53b

4-Methylphenanthrene and 1.60 ± 0.18b 15.8 ± 1.8b

 9-Methylphenanthreneg,h

2-Methylanthracenee,f 0.232 ± 0.004c 2.29 ± 0.04c

Cyclopenta[cd]pyreneh 0.227 ± 0.010d 2.24 ± 0.10d

Benzo[c]phenanthrenee,f,h 1.85 ± 0.21b 18.3 ± 2.1b

Benzo[b]chryseneh

 0.507 ± 0.030d 5.00 ± 0.30d

Benzo[c]chryseneg,h 0.318 ± 0.042b 3.14 ± 0.42b

Dibenz[a,c]anthracenef,g 0.212 ± 0.013c 2.09 ± 0.13c

Dibenz[a,j]anthraceneg,h 0.467 ± 0.048b 4.61 ± 0.47b 

Piceneg,h 0.75 ± 0.16b 7.4 ± 1.6b

a Concentrations reported on both wet- and dry-mass basis; material as received contains 89.87 % ± 0.05 % (95 % confidence level) 

water. b

 The reference value is a weighted mean of the results from two to seven analytical methods [17]. The uncertainty listed with each value 

is an expanded uncertainty about the mean, with coverage factor 2 (approximately 95% confidence), calculated by combining a 

between-source variance incorporating inter-method bias with a pooled within-source variance following the ISO/NIST Guide to the 

Expression of Uncertainty in Measurements [2]. c

 The reference value is an unweighted mean of the results from two analytical methods. The uncertainty listed with the value is an 

expanded uncertainty about the mean, with coverage factor 2, calculated by combining a between-method variance [18] with a pooled, 

within method variance following the ISO/NIST Guide to the Expression of Uncertainty in Measurement [2]. d

 The reference value is the mean of results obtained by NIST using one analytical technique. The expanded uncertainty, U, is calculated 

as U = kuc, where uc is intended to represent, at the level of one standard deviation, the combined standard uncertainty calculated according 

to the ISO Guide [2]. The coverage factor, k, is determined from the Student’s t-distribution corresponding to the appropriate associated 

degrees of freedom and 95 % confidence for each analyte. e

 GC/MS (Ia) on a relatively non-polar proprietary phase after PFE with 50% hexane/50% acetone mixture. f

 GC/MS (Ib) on 50% phenyl-substituted methylpolysiloxane phase; same extracts analyzed as in GC/MS (Ia). g

 GC/MS (II) on 50% phenyl-substituted methylpolysiloxane phase after PFE with DCM. h

 GC/MS (III) on a relatively non-polar proprietary phase and 50% phenyl-substituted methylpolysiloxane phase after Soxhlet extraction 

with DCM. i

 GC/MS (IV) on a relatively non-polar proprietary phase after Soxhlet extraction with DCM. 

j

 GC/MS (V) on 50% phenyl-substituted methylpolysiloxane phase after PFE with DCM. k

 2000 Interlaboratory Comparison Study [10] with 16 laboratories submitting data. 
 

Draft Certificate Table 5. Reference Concentrations for Selected PCB Congenersa and Total PCBs in SRM 1974b 

 mass fractions in μg/kg b

 wet-mass basisdry-mass basis 

PCB 8 (2,4’-Dichlorobiphenyl)f,g 0.37 ± 0.11c 3.7 ± 1.1c

 PCB 45 (2,2’,3,6-Tetrachlorobiphenyl)f,h,i,j 0.50 ± 0.18d 4.9 ± 1.8d

 PCB 56 (2,3,3’,4-Tetrachlorobiphenyl)f,h,i,k 2.82 ± 0.56d 27.8 ± 5.5d

 PCB 63 (2,3,4’,5-Tetrachlorobiphenyl)f,h,j,k 0.46 ± 0.14d

 4.5 ± 1.4d

 PCB 77 (3,3’,4,4’-Tetrachlorobiphenyl)l

 0.563 ± 0.023e 5.56 ± 0.23e

 PCB 92 (2,2’,3,5,5’-Pentachlorobiphenyl)f,h,i,k 2.76 ± 0.58d 27.2 ± 5.7d

 PCB 157(2,3,3’,4,4’,5’-Hexachlorobiphenyl)f,h,i 0.236 ± 0.024d

 2.33 ± 0.24d

 PCB 163(2,3,3’,4’,5,6-Hexachlorobiphenyl)f,h,i 2.02 ± 0.05c

 19.9 ± 0.5c

 Total PCBsm 205 ± 42 2020 ± 420 

 

 

a

 PCB congeners are numbered according to the scheme proposed by Ballschmiter and Zell [19] and later revised by Schulte and Malisch 

[20] to conform with IUPAC rules; for the specific congeners mentioned in this SRM, only PCB 107 (Table 2) is different in the

numbering systems. Under the Ballschmiter and Zell numbering system, the IUPAC PCB 107 is listed as PCB 108. b

 Concentrations reported on both wet- and dry-mass basis; material as received contains 89.87 % ± 0.05 % (95 % confidence level) 

water. c

 The reference value is an unweighted mean of the results from two to three analytical methods. The uncertainty listed with the value is 

an expanded uncertainty about the mean, with coverage factor 2, calculated by combining a between-method variance [18] with a 

pooled, within method variance following the ISO/NIST Guide to the Expression of Uncertainty in Measurement [2]. d

 The reference value is a weighted mean of the results from three to four analytical methods [17]. The uncertainty listed with each value 

is an expanded uncertainty about the mean, with coverage factor 2 (approximately 95% confidence), calculated by combining a 

between-method variance incorporating inter-method bias with a pooled within-source variance following the ISO/NIST Guide to the 

Expression of Uncertainty in Measurements [2]. e

 The reference value is the mean of results obtained by NIST using one analytical technique. The expanded uncertainty, U, is calculated 

as U = kuc, where uc is intended to represent, at the level of one standard deviation, the combined standard uncertainty calculated according 

to the ISO Guide [2]. The coverage factor, k, is determined from the Student’s t-distribution corresponding to the appropriate associated 

degrees of freedom and 95 % confidence for the analyte. f

 GC-ECD (Ib) on a relatively non-polar proprietary phase; same extracts as GC-ECD (Ia). g

 2000 Interlaboratory Comparison Study [10] with 16 laboratories submitting data.

h GC/MS (Ia) on a relatively non-polar proprietary phase after PFE with 50% hexane/50% acetone mixture. i

 GC/MS (Ib) on 50 % phenyl-substituted methylpolysiloxane phase; same extracts analyzed as in GC/MS (Ia). 

j

 GC-ECD (Ia) on 5 % phenyl-substituted methylpolysiloxane phase after PFE with DCM. 

k

 GC-ECD (II) on a 5% phenyl-substituted methylpolysiloxane phase after Soxhlet extraction with DCM. l

 GC/MS on a 5 % phenyl-substituted methylpolysiloxane phase; same extracts analyzed as in GC-ECD (I) fractionated using a PYE 

column. m Interlaboratory comparison study with four laboratories submitting data (See Preparation and Analysis for definition of total PCBs.). 

The expanded uncertainty, U, is calculated as U = kuc, where uc is intended to represent, at the level of one standard deviation, the 

combined standard uncertainty calculated according to the ISO Guide [2]. The coverage factor, k, is determined from the Student’s tdistribution corresponding to the appropriate associated degrees of freedom and 95 % confidence for the total PCBs. 
 

Draft Certificate Table 6. Reference Concentrations for Selected Chlorinated Pesticides and Total Extractable 

Organics in SRM 1974b 

mass fractions in μg/kga

 wet-mass basis dry-mass basis 

 Heptachlord,e 0.212 ± 0.084b

 2.09 ± 0.83b

 Oxychlordaned,e 0.362 ± 0.072b 3.57 ± 0.71b

 Dieldrind,e,f,g,h,i 0.62 ± 0.13c 6.1 ± 1.3c

cis-Nonachlord,e,f,g,h,i,j 0.64 ± 0.16c 6.3 ± 1.6c

 2,4’-DDTe,h,i 0.894 ± 0.057b 8.83 ± 0.56b

 4,4'-DDTd,e,f,g,h,i,j,k 0.396 ± 0.096c 3.91 ± 0.94c

 

 Percent 

 Total Extractable Organics (TEO)l

 0.64 ± 0.13 

a Concentrations reported on both wet- and dry-mass basis; material as received contains 89.87 % ± 0.05 % (95 % confidence level) 

water. b

 The reference value is an unweighted mean of the results from two to three analytical methods. The uncertainty listed with the value is 

an expanded uncertainty about the mean, with coverage factor 2, calculated by combining a between-method variance [18] with a 

pooled, within method variance following the ISO/NIST Guide to the Expression of Uncertainty in Measurement [2]. c

 The reference value is a weighted mean of the results from six to eight analytical methods [17]. The uncertainty listed with each value 

is an expanded uncertainty about the mean, with coverage factor 2 (approximately 95% confidence), calculated by combining a 

between-method variance incorporating inter-method bias with a pooled within-source variance following the ISO/NIST Guide to the 

Expression of Uncertainty in Measurements [2]. d

 GC-ECD (Ib) on a relatively non-polar proprietary phase; same extracts as GC-ECD (Ia). e

 GC-ECD (III) on a 5% phenyl-substituted methylpolysiloxane phase and a relatively non-polar proprietary phase after PFE with DCM. f

 GC/MS (Ib) on 50 % phenyl-substituted methylpolysiloxane phase; same extracts analyzed as in GC/MS (Ia). g

 GC-ECD (Ia) on 5 % phenyl-substituted methylpolysiloxane phase after PFE with DCM. 

h GC/MS (II) on a relatively non-polar proprietary phase after Soxhlet extraction with DCM. i

 2000 Interlaboratory Comparison Study [10] with 16 laboratories submitting data.

j GC/MS (Ia) on a relatively non-polar proprietary phase after PFE with 50% hexane/50% acetone mixture. k

 GC-ECD (II) on a 5% phenyl-substituted methylpolysiloxane phase after Soxhlet extraction with DCM. l

 Interlaboratory comparison study with six laboratories submitting data. The expanded uncertainty, U, is calculated as U = kuc, where uc is 

intended to represent, at the level of one standard deviation, the combined standard uncertainty calculated according to the ISO Guide [2]. 

The coverage factor, k, is determined from the Student’s t-distribution corresponding to the appropriate associated degrees of freedom and 

95 % confidence for the TEO. 
 

Appendix B: Description, Storage, Use, and Reporting Instructions for 

Marine Sediment XII (QA03SED12) 
 

NIST Intercomparison Exercise Program for 

Organic Contaminants in the Marine Environment 

NIST QA Program

Intercomparison Exercise: Marine Sediment XII 

Description of Materials and Instructions

Intercomparison Exercise Materials:

QA03SED12 (Marine Sediment XII)

Each of the three jars contains 20 g (wet basis) of Marine Sediment XII. This wetted sediment was 

prepared from material that was collected from a site near the Northwestern US coast and then freezedried, ground sieved, and radiation-sterilized. This material has not been enriched or spiked. Each 

2-oz clear glass jar has a Teflon-lined screw cap and is labeled with an individual jar number as well as 

the above name. 

In addition, three concurrent analyses of SRM 1941b, Organics in Marine Sediment, are recommended. 

This material can be obtained from the NIST Standard Reference Materials Program ($400/50 g (dry 

basis) (phone: 301/975-6776; fax: 301/948-3730). See the following link for information on ordering 

on-line: http://patapsco.nist.gov/srmcatalog/common/view_detail.cfm?srm=1941b. 

Storage of Materials:

Marine Sediment Material. This Marine Sediment XII material should be stored in the dark at 

temperatures of -15 ΕC or lower. If only a portion of the contents of a jar is used, that jar should be 

tightly closed immediately after removal of a subsample to preserve the integrity of the remaining 

material for later analysis. 

Instructions for Use: 

You are to analyze Marine Sediment XII and SRM 1941b, using your laboratory's and/or program's 

analytical protocols, for the concentrations (mass/mass [dry basis]) of the 26 polycyclic aromatic 

hydrocarbon (PAH) compounds, 25 chlorinated pesticides, and 25 polychlorinated biphenyl (PCB) 

congeners2

 of interest in the current NIST Intercomparison Exercise Program for Organic Contaminants 

in the Marine Environment. These compounds are listed in Table 1. 

 

2

If your laboratory is not analyzing samples for all three chemical classes, you are expected to submit results 

only for those compounds currently being determined in your laboratory. 
 

The percentage of water in Sediment XII should be determined so that the results can be reported on a 

dry basis. You should have received sufficient material so that you can perform separate 

determinations for the water content if you do not dry your sediment samples prior to analysis. In 

addition, the percentage of total organic carbon should be determined in Sediment XII and SRM 1941b. 

The amount of material used for each analysis should correspond to the amount (wet basis) of marine 

sediment that you would typically analyze as prescribed in your protocols. Prior to removing an aliquot 

of Sediment XII, you should thaw the sample in the jar and then stir or otherwise mix it thoroughly. 

You should analyze three samples of Marine Sediment XII and at least one, and more if possible, of 

SRM 1941b in three different batches/sets/strings/catalogs using your protocol for marine sediment 

samples. Specifically, we are asking that you analyze one sample of Sediment XII and one sample of 

SRM 1941b with one batch of laboratory samples; analyze a second sample of each material with 

another batch; and the third sample with yet another batch. This will allow a more realistic assessment 

of laboratory precision over a longer term than the assessment obtained when a laboratory places all 

three samples in the same extraction and cleanup batch and the resulting extracts are analyzed using the 

same calibration curve, etc. 

Reporting of Results: 

Please report one result, as if three figures were significant, for each of the requested analytes in each of 

the three replicates of the Marine Sediment XII and of SRM 1941b. Report results in units of ng/g dry

basis. Report the date of measurement of each sample in the requested m/d/y format. Also, report the 

results of your percentage water determinations of Marine Sediment XII. 

We recognize that the reported concentrations for some of the requested determinands will probably 

include concentrations of compounds reported to coelute with the determinand of interest with methods 

commonly in use in environmental laboratories. Please note at the bottom of your table of reported 

results if any coelution qualifiers are applicable to your data. Please note that any changes you make to 

the column or row headings within the tables will not be seen by the coordinators because only the 

table entries and comments at the bottom of the tables are automatically transferred to the exercise 

database. 

We prefer that concentration values be reported for each analyte determined. If the measured 

concentration is below your typical reporting concentration for an analyte in a particular matrix, you 

can report the number and list the appropriate detection limit, quantification limit, etc. at the bottom of 

the data table. However, if you need to report non-numerical data please use the following 

conventions: 

NA "Not analyzed", "not determined" 

<"value" "Less than specified concentration", e.g., <8 ng/g 

Other "Other"; add note of explanation at end of data table, e.g., interference 

DL "Below detection limit" may be used, however, <"value" is preferable 

Do not use negative numbers or parentheses to indicate "less than detection limits". 
 

The attached file is an EXCEL file, SED12.xls. If you have any software/hardware conversion 

problems, please contact Michele Schantz. The data file templates also include places for you to list the 

surrogate/internal standards and type of calibration curve used, and to provide a brief description of the 

analyses. Please do not add spaces before entering numbers in the table cells and enter them as 

"numbers" not as "labels". Please do not insert any columns or rows within the table in the data file. If 

you wish to include additional data and/or other information or comments, you may add it to the bottom 

of the data table in the diskette file or send it in hard copy. A printout of the data file format is shown 

in Table 2. 

Submit your results by July 11, 2003 as an attached file via e-mail to: 

E-mail: 

michele.schantz@nist.gov 

Further Information:

If you need further information, please contact Michele at the following address or phone numbers: 

Michele M. Schantz 

NIST 

100 Bureau Drive Stop 8392 

Gaithersburg, MD 20899-8392 

Phone: (301)975-3106 

FAX: (301)977-0685 
 

Table 1: Analytes of Interest in NIST Intercomparison Exercise Program for Organic 

Contaminants in the Marine Environment 

Chlorinated Pesticides 

hexachlorobenzene 2,4'-DDE 

alpha-HCH (alpha-BHC) 4,4'-DDE 

beta-HCH (beta-BHC) 2,4'-DDD 

gamma-HCH (gamma-BHC, Lindane) 4,4'-DDD 

heptachlor 2,4'-DDT 

heptachlor epoxide 4,4'-DDT 

cis-chlordane (alpha-chlordane) chlorpyrifos 

trans-chlordane (gamma-chlordane) aldrin 

oxychlordane dieldrin 

cis-nonachlor endrin 

trans-nonachlor endosulfan I 

mirex endosulfan II 

endosulfan sulfate 

Polychlorinated Biphenyl Congeners

 PCB No. Compound Name

 8 2,4'-dichlorobiphenyl 

 18 2,2',5-trichlorobiphenyl 

 28 2,4,4'-trichlorobiphenyl 

 31 2,4',5-trichlorobiphenyl 

 44 2,2',3,5'-tetrachlorobiphenyl 

 49 2,2',4,5'-tetrachlorobiphenyl 

 52 2,2',5,5'-tetrachlorobiphenyl 

 66 2,3',4,4'-tetrachlorobiphenyl 

 95 2,2',3,5',6-pentachlorobiphenyl 

 99 2,2',4,4',5-pentachlorobiphenyl 

 101 2,2',4,5,5'-pentachlorobiphenyl 

 105 2,3,3',4,4'-pentachlorobiphenyl 

 118 2,3',4,4',5-pentachlorobiphenyl 

 128 2,2',3,3',4,4'-hexachlorobiphenyl 

 138 2,2',3,4,4',5'-hexachlorobiphenyl 

 149 2,2',3,4',5',6-hexachlorobiphenyl 

 153 2,2',4,4',5,5'-hexachlorobiphenyl 

 156 2,3,3',4,4',5-hexachlorobiphenyl 

 170 2,2',3,3',4,4',5-heptachlorobiphenyl 

 180 2,2',3,4,4',5,5'-heptachlorobiphenyl 

 187 2,2',3,4',5,5',6-heptachlorobiphenyl 

 194 2,2',3,3',4,4',5,5'-octachlorobiphenyl 

 195 2,2',3,3',4,4',5,6-octachlorobiphenyl 

 206 2,2',3,3',4,4',5,5',6-nonachlorobiphenyl 

 209 decachlorobiphenyl 
 

Table 1. (continued) 

Polycyclic aromatic hydrocarbons (PAH)

naphthalene pyrene 

2-methylnaphthalene benz[a]anthracene 

1-methylnaphthalene chrysene 

biphenyl triphenylene 

2,6-dimethylnaphthalene benzo[b]fluoranthene 

acenaphthylene benzo[j]fluoranthene 

acenaphthene benzo[k]fluoranthene 

1,6,7-trimethylnaphthalene benzo[e]pyrene 

fluorene benzo[a]pyrene 

phenanthrene perylene 

anthracene

 indeno[1,2,3-cd]pyrene 

1-methylphenanthrene dibenz[a,h]anthracene 

fluoranthene benzo[ghi]perylene 

 
 

Table 2. Diskette Data File Format (File: SED12.*)

NIST Intercomparison Exercise Program for Organics in the Marine Environment

NIST QA Program

Sample: QA03SED12 - Marine Sediment XII

Please fill in all blanks; Use requested units of concentration; Report results as if 3 figures were significant

DO NOT INSERT ROWS OR COLUMNS WITHIN THIS TABLE. DO NOT MOVE CELLS.

 - If necessary, add additional data/information at the end of the table.

 - Use one of the following if no concentration is reported for an analyte:

 NA = Not analyzed/determined; <"conc" = <detection limit conc.; Other = other, explain in a note at end of table

 (DL = "below detection limit" may be used, but <"conc", e.g., <8, is preferable.)

 Do not use parentheses or negative numbers to indicate "less than detection limit".

Reporting Date (m/d/y): _______________________

Laboratory: _______________________

Submitted by: _______________________

BRIEF DESCRIPTION OF PROCEDURES USED:

Approximate amount of sample extracted: Sediment XII ___________ g, wet basis; SRM 1941b ___________ g, dry basis

Method used for determining percentage water: ______________________________________________________________________

______________________________________________________________________

______________________________________________________________________

Were "wet" or "dry" samples extracted? Sediment XII ___________ SRM 1941b ___________

Extraction method: ____________________________________________________________________________________________

Extraction solvent: ____________________________________________________________________________________________

Extraction time: ____________________________________________________________________________________________

Extraction - other: ____________________________________________________________________________________________

____________________________________________________________________________________________

Sample extract cleanup method: ____________________________________________________________________________________________

____________________________________________________________________________________________

____________________________________________________________________________________________

____________________________________________________________________________________________

____________________________________________________________________________________________

Analytical method used (e.g., GC-FID, GC-ECD):

Analyt. Instr. Column Phase Col. Length, m Col. i.d., mm Col. film thickness, μm

PAH ________________________________________________________________________

 Pesticides ________________________________________________________________________

 PCB Congeners ________________________________________________________________________

Method of quantitation (IS = internal standard, ES = external standard):

 PAH __________________

 Pesticides __________________

 PCB Congeners __________________

IF internal standard method was used, please complete the following section:

 Identity of internal standards/surrogates used that were:

 Added PRIOR to extraction of sample:

 PAH ________________________________________________________________________

 Pesticides ________________________________________________________________________

 PCB Congeners ________________________________________________________________________

 Added after extraction/cleanup and JUST PRIOR to chromatographic analysis:

PAH ________________________________________________________________________

Pesticides ________________________________________________________________________

 PCB Congeners ________________________________________________________________________

 Any others? Added at what point in analyses: __________________________________________________________

PAH ________________________________________________________________________

Pesticides ________________________________________________________________________

 PCB Congeners ________________________________________________________________________

 IS/surrogate standards used for quantitation calculations were: 

________ those added prior to extraction

________ those added after extraction/cleanup and just prior to chromatographic analysis

 If the IS/surrogates added after extraction/cleanup extraction were used for quantitation, 

 were results corrected for percent recovery? __________________

 Percent recovery range: PAH __________________

Pesticides __________________

PCB Congeners __________________
 

Calibration Curve

Analytes outside of calibration 

Points Conc. Range curve calibration range

 PAH ____________________________________ __________________________________

 Pesticides ____________________________________ __________________________________

 PCB Congeners ____________________________________ __________________________________

Were PCB congeners separated from pesticides prior to GC? __________________

Please note any differences in procedures used for SRM 1941b analyses from those for Marine Sediment XII described above:

_____________________________________________________________________________________________________________________

_____________________________________________________________________________________________________________________

_____________________________________________________________________________________________________________________

_____________________________________________________________________________________________________________________

_____________________________________________________________________________________________________________________

RESULTS:

PERCENT WATER & total organic carbon, TOC (List each result if determined more than once. Enter results as a number, for example 90.0. 

DO NOT change format of cell to percent.)

Sediment XII Sediment XII Sediment XII SRM 1941b SRM 1941b SRM 1941b

(percent) (percent) (percent) (percent) (percent) (percent)

Water __________ __________ __________ 

TOC __________ __________ __________ __________ __________ __________ 

PAH ANALYSES Sediment XII Sediment XII Sediment XII SRM 1941b SRM 1941b SRM 1941b

Batch A Batch B Batch C Batch A Batch B Batch C

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

Analyst (Initials) __________ __________ __________ __________ __________ __________ 

Date(s) of measurements (m/d/y) __________ __________ __________ __________ __________ __________ 

Sample Jar number __________ __________ __________ 

Sediment XII Sediment XII Sediment XII SRM 1941b SRM 1941b SRM 1941b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g dry wt) (ng/g dry wt) (ng/g dry wt) (ng/g dry wt) (ng/g dry wt) (ng/g dry wt)

naphthalene __________ __________ __________ __________ __________ __________ 

2-methylnaphthalene __________ __________ __________ __________ __________ __________ 

1-methylnaphthalene __________ __________ __________ __________ __________ __________ 

biphenyl __________ __________ __________ __________ __________ __________ 

2,6-dimethylnaphthalene __________ __________ __________ __________ __________ __________ 

acenaphthylene __________ __________ __________ __________ __________ __________ 

acenaphthene __________ __________ __________ __________ __________ __________ 

1,6,7-trimethylnaphthalene __________ __________ __________ __________ __________ __________ 

fluorene __________ __________ __________ __________ __________ __________ 

phenanthrene __________ __________ __________ __________ __________ __________ 

anthracene __________ __________ __________ __________ __________ __________ 

1-methylphenanthrene __________ __________ __________ __________ __________ __________ 

fluoranthene __________ __________ __________ __________ __________ __________ 

pyrene __________ __________ __________ __________ __________ __________ 

benz[a]anthracene __________ __________ __________ __________ __________ __________ 

chrysene __________ __________ __________ __________ __________ __________ 

triphenylene __________ __________ __________ __________ __________ __________ 

benzo[b ]fluoranthene __________ __________ __________ __________ __________ __________ 

benzo[j]fluoranthene __________ __________ __________ __________ __________ __________ 

benzo[k ]fluoranthene __________ __________ __________ __________ __________ __________ 

benzo[e]pyrene __________ __________ __________ __________ __________ __________ 

benzo[a]pyrene __________ __________ __________ __________ __________ __________ 

perylene __________ __________ __________ __________ __________ __________ 

indeno[1,2,3-cd]pyrene __________ __________ __________ __________ __________ __________ 

dibenz[a,h]anthracene __________ __________ __________ __________ __________ __________ 

benzo[ghi]perylene __________ __________ __________ __________ __________ __________ 
 

PESTICIDE ANALYSES Sediment XII Sediment XII Sediment XII SRM 1941b SRM 1941b SRM 1941b

Batch A Batch B Batch C Batch A Batch B Batch C

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

Analyst (Initials) __________ __________ __________ __________ __________ __________ 

Date(s) of measurements (m/d/y) __________ __________ __________ __________ __________ __________ 

Sample Jar number __________ __________ __________ 

Sediment XII Sediment XII Sediment XII SRM 1941b SRM 1941b SRM 1941b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g dry wt) (ng/g dry wt) (ng/g dry wt) (ng/g dry wt) (ng/g dry wt) (ng/g dry wt)

alpha-HCH (a-BHC) __________ __________ __________ __________ __________ __________ 

hexachlorobenzene __________ __________ __________ __________ __________ __________ 

gamma-HCH (g-BHC,lindane) __________ __________ __________ __________ __________ __________ 

beta-HCH (b-BHC) __________ __________ __________ __________ __________ __________ 

heptachlor __________ __________ __________ __________ __________ __________ 

aldrin __________ __________ __________ __________ __________ __________ 

heptachlor epoxide __________ __________ __________ __________ __________ __________ 

oxychlordane __________ __________ __________ __________ __________ __________ 

gamma-chlordane __________ __________ __________ __________ __________ __________ 

2,4'-DDE __________ __________ __________ __________ __________ __________ 

endosulfan I __________ __________ __________ __________ __________ __________ 

cis-chlordane (alpha-chlordane) __________ __________ __________ __________ __________ __________ 

trans-nonachlor __________ __________ __________ __________ __________ __________ 

dieldrin __________ __________ __________ __________ __________ __________ 

4,4'-DDE __________ __________ __________ __________ __________ __________ 

2,4'-DDD __________ __________ __________ __________ __________ __________ 

endrin __________ __________ __________ __________ __________ __________ 

endosulfan II __________ __________ __________ __________ __________ __________ 

4,4'-DDD __________ __________ __________ __________ __________ __________ 

2,4'-DDT __________ __________ __________ __________ __________ __________ 

cis-nonachlor __________ __________ __________ __________ __________ __________ 

4,4'-DDT __________ __________ __________ __________ __________ __________ 

mirex __________ __________ __________ __________ __________ __________ 

endosulfan sulfate __________ __________ __________ __________ __________ __________ 

chlorpyrifos __________ __________ __________ __________ __________ __________ 

PCB CONGENER ANALYSES Sediment XII Sediment XII Sediment XII SRM 1941b SRM 1941b SRM 1941b

Batch A Batch B Batch C Batch A Batch B Batch C

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

Analyst (Initials) __________ __________ __________ __________ __________ __________ 

Date(s) of measurements (m/d/y) __________ __________ __________ __________ __________ __________ 

Sample Jar number __________ __________ __________ 

Sediment XII Sediment XII Sediment XII SRM 1941b SRM 1941b SRM 1941b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g dry wt) (ng/g dry wt) (ng/g dry wt) (ng/g dry wt) (ng/g dry wt) (ng/g dry wt)

PCB 8 __________ __________ __________ __________ __________ __________ 

PCB 18 __________ __________ __________ __________ __________ __________ 

PCB 28 __________ __________ __________ __________ __________ __________ 

PCB 31 __________ __________ __________ __________ __________ __________ 

PCB 44 __________ __________ __________ __________ __________ __________ 

PCB 49 __________ __________ __________ __________ __________ __________ 

PCB 52 __________ __________ __________ __________ __________ __________ 

PCB 66 __________ __________ __________ __________ __________ __________ 

PCB 95 __________ __________ __________ __________ __________ __________ 

PCB 99 __________ __________ __________ __________ __________ __________ 

PCB 101 __________ __________ __________ __________ __________ __________ 

PCB 105 __________ __________ __________ __________ __________ __________ 

PCB 118 __________ __________ __________ __________ __________ __________ 

PCB 128 __________ __________ __________ __________ __________ __________ 

PCB 138 __________ __________ __________ __________ __________ __________ 

PCB 149 __________ __________ __________ __________ __________ __________ 

PCB 153 __________ __________ __________ __________ __________ __________ 

PCB 156 __________ __________ __________ __________ __________ __________ 

PCB 170 __________ __________ __________ __________ __________ __________ 

PCB 180 __________ __________ __________ __________ __________ __________ 

PCB 187 __________ __________ __________ __________ __________ __________ 

PCB 194 __________ __________ __________ __________ __________ __________ 

PCB 195 __________ __________ __________ __________ __________ __________ 

PCB 206 __________ __________ __________ __________ __________ __________ 

PCB 209 __________ __________ __________ __________ __________ __________ 

(Any additional data/information should be added here.)
 

Appendix C: Laboratory Notes Accompanying Data, 

Mussel Tissue XI 
 

Lab Additional notes for Mussel Tissue XI

1b MT XI MT XI MT XI SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt)

PCB 151 1.38 1.40 1.39 1.76 1.76 1.77

2,3,5-trimethylnaphthalene 2.91 2.81 2.68 0.566 0.483 0.487

3-methylphenanthrene 7.12 7.20 7.17 1.09 1.32 1.35

2-methylphenanthrene 8.81 8.94 9.10 1.44 1.52 1.60

9-methylphenanthrene 4.59 4.57 4.69 0.979 1.00 1.09

1-methylphenanthrene w/ 4- 4.89 5.05 4.83 1.06 0.850 0.938

benzo[ghi]fluoranthene 2.79 2.71 2.58 2.36 2.29 2.35

benzo[c]phenanthrene 2.85 2.65 2.67 1.98 1.91 1.91

benzo[ C ]chrysene w/ di[a,j]ant 0.757 0.616 0.596 0.789 0.756 0.804

dibenz[a,c]anthracene 1.82 1.75 1.73 1.75 1.85 2.06

benzo[b]chrysene 0.521 0.408 0.355 0.470 0.935 0.755

picene 0.864 0.813 0.687 0.755 0.928 0.977

benzo[a]fluoranthene 0.851 0.786 0.759 0.784 1.01 0.970

possible coelution of another compound with 2,4'-DDT in both tissue 11 and 1974b

4,4'-DDD seems to have degraded in samples, may have lost in clean-up

dibenz[a,c]anthracene not a single peak in tissue 11 or SRM 1974b on DB-17MS column

1c MT XI MT XI MT XI SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt)

PCB 29 <0.3 <0.3 <0.3 <0.3 <0.3 <0.3

PCB 45 0.545 0.527 0.443 0.466 0.589 0.427

PCB 63 0.533 0.523 0.667 0.395 0.434 0.400

PCB 74 3.26 3.34 3.18 3.26 3.34 3.18

PCB 70 5.61 5.68 5.48 5.61 5.68 5.48

PCB 56 1.34 1.13 1.13 2.90 2.71 2.73

PCB 92 2.37 2.23 2.23 2.17 2.43 2.07

PCB 87 4.39 4.47 4.23 4.39 4.47 4.23

PCB 154 <0.3 <0.3 <0.3 <0.3 <0.3 <0.3

PCB 110 6.73 6.44 6.55 9.47 9.24 8.76

PCB 151 1.72 1.66 1.56 1.72 1.66 1.56

PCB 107 0.634 0.655 0.618 0.773 0.788 0.744

PCB 146 1.25 1.21 1.16 1.53 1.50 1.40

PCB 132 1.66 1.52 1.39 1.95 1.76 1.66

PCB 163 1.15 1.12 1.12 1.74 1.67 1.56

PCB 158 0.679 0.646 0.621 0.800 0.753 0.705

PCB 183 0.994 0.956 0.927 1.14 1.10 1.02

PCB 174 <0.3 <0.3 <0.3 <0.3 <0.3 <0.3

PCB 201 <0.3 <0.3 <0.3 <0.3 <0.3 <0.3

PCB 157 <0.3 <0.3 <0.3 <0.3 <0.3 <0.3

PCB 193 <0.3 <0.3 <0.3 <0.3 <0.3 <0.3

2 PAHs: Chrysene and triphenylene co-elute

 - reported chrysene values include contribution from triphenylene

Benzo(b)fluoranthene and benzo(j)fluoranthene co-elute

 - reported benzo(b)fluoranthene values include contribution from benzo(j)fluoranthene

4 1) 'Other" o,p'-DDE coelution issues

2) Normal Method Report Limit is 5.0

8 other = interference

12 MT XI MT XI MT XI SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt)

chrysene\triphenylene 15 15.8 14.1 10.6 9.88 8.81

benzo(b+a)fluoranthene 9.78 10.4 9.18 10.9 9.57 8.06

1-methylphenanthrene/1-methylan 3.05 3.11 2.81 1.15 1.05 0.913

o,p-DDT & p,p-DDD 4.58 4.73 4.87 5.09 4.85 4.44

PCBs

8/5 0.3 0.245 0.238 0.421 0.581 0.29

28/31 5.01 4.82 4.26 5.95 6.53 4.95

95/121/88 3.84 3.75 3.35 5.56 5.61 4.4

66/80 4.65 4.44 4.09 6.29 6.2 4.89

149/139 4.74 4.68 4.27 7.13 7.11 5.57

118/106 7.78 7.62 7.02 11.9 11.9 9.68

153/132 6.23 6.16 5.76 9.93 9.53 7.78

105/127 3.1 3.07 2.75 4.67 4.57 3.62

138/160/163/158 8.22 8.07 7.27 12.6 12.3 10

187/182 1.91 1.85 1.68 2.7 2.67 2.16

128/167 1.19 1.14 1.04 1.97 1.97 1.64

170/190 DL DL DL 0.256 0.256 0.197

Anthracene, fluorene, and biphenyl were not quantified due to background interference.
 

15 Coelutions: Triphenylene coelutes with chrysene; benzo[j]fluoranthene coelutes with benzo[k]fluoranthene; 

dibenz[a.c]anthracene coelutes with dibenz[a.h]anthracene.

PCB 90 coelutes with PCB 101; PCBs 163 and 164 colelute with PCB 138; PCB 132 coleutes with PCB 153; 

PCBs 159 and 182 coleute with PCB 187.

MT XI MT XI MT XI SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt)

dibenzothiophene 1.37 1.39 1.43 0.324 0.304 0.299

retene 2.28 2.08 2.14 0.885 0.914 0.929

PCB 17 0.911 0.868 0.834 0.970 1.01 0.928

PCB 33 <1.12 0.911 0.888 <1.12 <0.881 <1.04

PCB 70 6.95 6.37 6.25 7.63 7.25 7.46

PCB 74 3.89 3.8 3.76 4.30 4.24 4.30

PCB 82 1.01 0.957 0.981 1.18 1.15 1.19

PCB 87 3.70 3.78 3.68 4.62 4.55 4.66

PCB 110 8.11 8.09 7.88 10.3 10.1 10.3

PCB 151 1.34 1.42 1.36 1.73 1.76 1.75

PCB 158 0.886 0.874 0.838 1.13 1.08 1.13

PCB 171 0.454 0.425 0.426 0.543 0.525 0.541

PCB 177 0.815 0.823 0.818 1.06 1.05 1.07

PCB 183 1.02 1.06 1.01 1.22 1.22 1.26

PCB 191 <0.431 <0.254 <0.262 <0.431 <0.338 <0.398

PCB 199 <0.850 <0.500 <0.518 <0.850 <0.668 <0.786

PCB 205 <0.431 <0.254 <0.262 <0.431 <0.339 <0.399

PCB 208 <0.431 <0.254 <0.262 <0.431 <0.338 <0.398

16 Co-eluters: PCB18/30, PCB-28/20/21/33, PCB-44/47/65, PCB-49/69, PCB-52/73/43, PCB-99/83/112, PCB-101/90/113, PCB-128/166, 

 PCB-138/164/163/129, PCB-147/149, PCB-153/168, PCB-156/157, PCB-180/193

18 * The results for Chrysene is a total result for Chrysene and Triphenylene which coelute.

*The results for Benzo(k)Fluoranthene is a total result for Benzo(k)Fluoranthene and Benzo(j)Fluoranthene which coelute.

*The results for Dibenz(a,h)anthracene is a total result for Dibenz(a,c) & (a,h)anthracene, which coelute.

*The results PCB 28 is the total result of PCB 28 and PCB 31 which coelute.

19 PAH Internal Standards

d8-naphthalene, d8-acenaphthylene, d10-acenaphthene, d10-fluorene, d10-phenanthrene, d10-anthracene, d10-fluoranthene

d10-pyrene, d12-benz(a)anthracene, d12-chrysene, d12-benzo(b)fluoranthene, d12-benzo(k)fluoranthene, d12-benzo(e)pyrene

d12-benzo(a)pyrene, d12-perylene, d12-indeno(1,2,3-cd)pyrene, d12-dibenz(a,h)anthracene, d12-benzo(g,h,i)perylene

Other (1) - Under our chromatographic conditions, chrysene and triphenylene co-elute. They are reported as the sum, 

 based upon the response factor of chrysene.

Other (2) - Under our chromatographic conditions, benzo [j] and [k] fluoranthene co-elute. They are reported as the sum, 

based upon the response factor of b[k]f.

MT XI MT XI MT XI SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt)

Chrysene+Triphenylene 18.9 19.7 19.8 12.2 11.5 11.9

Benzo(j+k)fluoranthene 6.27 5.74 6.31 5.50 6.94 6.76

Dibenzothiophene 0.950 1.16 1.04 0.309 0.651 0.448

PCB 29 0.576 0.788 0.754 0.937 0.814 0.797

PCB 50 4.31 4.5 4.68 4.8 4.84 4.8

PCB 87 3.52 3.56 3.54 4.5 4.62 4.6

PCB 104 0.281 0.406 0.33 0.293 0.417 0.43

PCB 126 0.683 0.813 0.948 1.01 1.06 1.09

PCB 154 4.56 4.62 4.66 5.94 6.17 6.19

PCB 188 1.16 1.32 1.44 1.88 1.81 1.93

PCB 201 0.35 0.355 0.426 0.496 0.481 0.495

20 PCB101 coelutes with PCB90

PCB153 coelutes with PCB132 and 168

PCB170 coelutes with PCB190

PCB 8 coelutes with PCB 5

PCB 195 coelutes with PCB208

<symbol refers to values less than our MDL

the chrysene number is the sum of chrysene and triphenylene, we cannot resolve the two

we do not analyze for benzo(j)fluoranthes because it coelutes with benzo(b)fluoranthene

Tissue MDL values are high due to limited sample volume and reporting data on a wet weight basis.

Our MDLs are based on 13.0g wet weight of mussel. Therfore MDLs reported here are approximately 2X higher than

those on 13 g wet. Additionally, sample PAH concentrations are low which is compounded by the small sample volume.
 

Appendix D: Laboratory Notes Accompanying Data, Marine 

Sediment XII 
 

Lab Additional notes for Sediment XII

1b SED XII SED XII SED XII SRM 1941b SRM 1941b SRM 1941b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g dry wt) (ng/g dry wt)

PCB 151 5.75 6.09 5.52 1.19 1.16 1.27

2,3,5-trimethylnaphthalene 24.3 26.9 26.3 29.8 30.0 29.7

3-methylphenanthrene 69.8 74.6 75.3 92.3 95.1 94.4

2-methylphenanthrene 85.3 90.6 91.2 103 107 106

9-methylphenanthrene 49.2 52.1 52.9 55.2 56.8 55.9

1-methylphenanthrene w/ 4- 69.5 74.5 75.9 77.7 78.7 77.4

benzo[ghi]fluoranthene 95.5 99.8 97.9 61.8 63.6 61.9

benzo[c]phenanthrene 82.4 86.5 93 61.1 62.1 64.5

benzo[ C ]chrysene w/ di[a,j]ant 107? 139 151 77.2 78.4 84.4

dibenz[a,c]anthracene 74.2 75.3 83.9 44.1 45.5 54.8

benzo[b]chrysene 94.1 111 119 64.7 72.2 80.5

picene 48.6? 107 119 41.2 42.1 31.4

benzo[a]fluoranthene 46.9? 116 123 69.5 74.6 73.5

possible coelution of another compound with 2,4'-DDT in both sed12 and in 1941b

4,4'-DDD seems to have degraded in samples, may have lost in clean-up

dibenz[a,c]anthracene is not a single peak in sed 12 and in 1941b on DB-17MS column

1c SED XII SED XII SED XII SRM 1941b SRM 1941b SRM 1941b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g dry wt) (ng/g dry wt)

PCB 29 <0.3 <0.3 <0.3 NA <0.3 <0.3

PCB 63 <0.3 <0.3 <0.3 NA <0.3 <0.3

PCB 74 2.90 3.04 3.05 NA 1.83 2.04

PCB 70 7.25 6.64 6.77 NA 4.15 4.24

PCB 56 3.91 3.67 3.51 NA 2.65 2.85

PCB 92 3.84 4.04 4.45 NA 0.970 0.978

PCB 87 12.5 11.3 12.3 NA 1.68 1.43

PCB 110 24.1 23.3 25.5 NA 4.70 4.40

PCB 154 <0.3 <0.3 <0.3 NA <0.3 <0.3

PCB 82 2.41 2.45 2.48 NA 0.419 0.432

PCB 151 6.08 5.65 6.14 NA 1.08 1.12

PCB 107 1.26 1.00 1.21 NA 0.461 0.476

PCB 146 3.37 3.02 3.44 NA 0.829 0.887

PCB 105 7.05 6.48 7.29 NA 1.47 1.25

PCB 163 4.90 4.56 5.35 NA 0.883 0.981

PCB 158 2.45 2.19 2.53 NA 0.362 0.322

PCB 183 3.85 3.53 3.72 NA 1.04 1.07

PCB 174 5.29 5.10 5.21 NA 1.02 1.08

PCB 201 2.39 2.17 2.36 NA 0.678 0.740

PCB 157 0.543 0.535 0.445 NA <0.3 <0.3

PCB 193 0.764 0.528 0.649 NA <0.3 <0.3

2 PAHs: Chrysene and triphenylene co-elute

 - reported chrysene values include contribution from triphenylene

Benzo(b)fluoranthene and benzo(j)fluoranthene co-elute

 - reported benzo(b)fluoranthene values include contribution from benzo(j)fluoranthene

3 SRM1941a was used , not 1941b

SEDXII was oven-"dried" at 37C for 17 hours prior to extraction

4 PAH analysis: concentrations reported below 150ng/g for NIST sediments are considered estimated values because they are

below the method reporting level based on an 8g sample weight. Concentrations reported below 125ng/g for the SRMs are

considered estimated values due to a 10g sample weight.

9 SRM 1941b, Sample 3 - Data unuseable due to lab accident.

12 SED XII SED XII SED XII

Sample 1 Sample 2 Sample 3

(ng/g dry wt)

chrysene\triphenylene 1260 1260 1200

benzo(b+a)fluoranthene 1300 1400 1370

1-methylphenanthrene/1-methylan 94.4 100 97.4

o,p-DDT & p,p-DDD 45.9 46.7 45.6

PCBs

8/5 1.07 1.22 1.2

28/31 7 7.41 7.04

95/121/88 25.2 22.8 22.7

66/80 8.21 8 7.78

149/139 36.1 33.6 34

118/106 0.667 0.619 0.594

153/132 57.7 53 53.6

105/127 14.4 13 13.1

138/160/163/158 58.1 54 55.3

187/182 13.3 12.9 12.6

128/167 10.5 9.73 9.83

170/190 13.2 12.5 12.7
 

15 Coelutions: Triphenylene coelutes with chrysene; benzo[j]fluoranthene coelutes with benzo[k]fluoranthene; 

dibenz[a.c]anthracene coelutes with dibenz[a.h]anthracene.

PCB 90 coelutes with PCB 101; PCBs 163 and 164 colelute with PCB 138; PCB 132 coleutes with PCB 153;

PCBs 159 and 182 coleute with PCB 187.

SED XII SED XII SED XII SRM 1941b SRM 1941b SRM 1941b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

Additional compounds: (ng/g dry wt) (ng/g dry wt)

dibenzothiophene 47.0 44.5 39.0 57.5 58.1 58.2

PCB 17 2.08 2.30 1.74 1.47 1.45 1.48

PCB 33 4.94 4.92 4.44 2.85 2.92 2.89

PCB 70 18.9 19.9 17.3 6.13 6.36 6.18

PCB 74 6.69 6.89 6.06 2.48 2.6 2.51

PCB 82 5.43 5.63 5.01 0.570 0.672 0.581

PCB 87 21.8 23.8 20.1 1.44 1.62 1.38

PCB 110 46.7 49.8 43.1 6.55 6.83 6.66

PCB 151 11.4 12.9 11.2 1.23 1.22 1.22

PCB 158 6.88 7.67 6.49 0.441 0.483 0.444

PCB 171 4.35 4.93 4.35 <0.403 <0.410 <0.434

PCB 177 8.50 9.92 8.65 0.906 0.913 0.912

PCB 183 8.21 9.38 8.27 0.855 0.861 0.865

PCB 191 0.590 0.684 0.59 <0.403 <0.410 <0.434

PCB 199 7.04 7.98 7.25 1.29 1.38 1.27

PCB 205 0.367 <0.570 0.366 <0.404 <0.410 <0.434

PCB 208 1.22 1.28 1.22 1.16 1.15 1.15

16 Co-eluters: PCB18/30, PCB-28/20/21/33, PCB-44/47/65, PCB-49/69, PCB-52/73/43, PCB-99/83/112, PCB-101/90/113, PCB-128/166, 

PCB-138/164/163/129, PCB-147/149, PCB-153/168, PCB-156/157, PCB-180/193

17 chrysene co-elutes with triphenylene

benzo(j)fluoranthene co-elutes with benzo(k)fluoranthene

18 * The results for Chrysene is a total result for Chrysene and Triphenylene which coelute.

*The results for Benzo(k)Fluoranthene is a total result for Benzo(k)Fluoranthene and Benzo(j)Fluoranthene which coelute.

*The results for Dibenz(a,h)anthracene is a total result for Dibenz(a,c) & (a,h)anthracene, which coelute.

*The results PCB 28 is the total result of PCB 28 and PCB 31 which coelute.

19 PAH Internal Standards

d8-naphthalene, d8-acenaphthylene, d10-acenaphthene, d10-fluorene, d10-phenanthrene, d10-anthracene, d10-fluoranthene

d10-pyrene, d12-benz(a)anthracene, d12-chrysene, d12-benzo(b)fluoranthene, d12-benzo(k)fluoranthene, d12-benzo(e)pyrene

d12-benzo(a)pyrene, d12-perylene, d12-indeno(1,2,3-cd)pyrene, d12-dibenz(a,h)anthracene, d12-benzo(g,h,i)perylene

Other (1) - Under our chromatographic conditions, chrysene and triphenylene co-elute. They are reported as the sum, 

based upon the response factor of chrysene.

Other (2) - Under our chromatographic conditions, benzo [j] and [k] fluoranthene co-elute. They are reported as the sum, 

based upon the response factor of b[k]f.

Other (3) - Under our chromatographic conditions, dibenz [a,h] and [a,c] anthracene co-elute. They are reported as the sum, 

based upon the response factor of dibenz(a,h)anthracene.

SED XII SED XII SED XII SRM 1941b SRM 1941b SRM 1941b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g dry wt) (ng/g dry wt)

chrysene+triphenylene 1040 1060 1170 505 508 504

benzo[j+k]fluoranthene 1260 923 1270 517 498 474

dibenzothiophene 39.4 44.7 50.0 58.0 66.7 63.1

dibenz[a,h+a,c]anthracene 164 136 111 120 105 125

PCB 29 0.314 0.319 0.266 0.641 1.19 1.52

PCB 50 1.93 3.09 2.29 0.908 1.37 1.2

PCB 77 60.9 66 62.9 5.09 5.88 5.55

PCB 87 14.3 13.6 13.1 0.952 1.13 1.25

PCB 126 4.77 5.65 4.73 0.658 0.777 0.96

PCB 154 18.3 15.4 14.9 3.67 3.59 3.86

PCB 188 6.21 6.96 5.64 0.378 0.472 0.42

PCB 201 3.7 3.93 2.92 0.419 0.541 0.472

20 the crysene number is the sum of chrysene and triphenylene, we cannot resolve the two

we can not separate benzo(j)fluoranthene because under our conditions it coelutes with benzo(b)fluoranthene

<symbol refers to values less than our MDL

PCB101 coelutes with PCB90

PCB153 coelutes with PCB132 and 168

PCB170 coelutes with PCB190

PCB8 coelutes with PCB5

PCB195 coelutes with PCB208

Total carbon and total organic carbon are measured independently in oven-dried sediments and soils using a LECO CR-412 

Carbon Determinator
 

Appendix E: Laboratory Methods Used, Mussel Tissue XI 
g extracted g extracted % water Extraction Extraction Extraction Extraction

Lab # Reported QA03TIS11 SRM 1974b Determination Method Solvent Time other

1a 7/12/2003 6 wet 6 wet freeze-dry PFE dichloromethane 3 cycles each 5 min

temp = 100 oC; pressure 2000 psi; 3 

static cycles / sample

1b 10/6/2003 12 wet 10 wet not analyzed Soxhlet dichloromethane overnight

1c 10/15/2003 10 wet 10 wet freeze-dry PFE dichloromethane 3 cycles each 5 min

temp = 100 oC; pressure 2000 psi; 3 

static cycles / sample

2 6/17/2003 5 wet 5 wet not analyzed Soxhlet dichloromethane 16 h (PCBs); 2 h (PAHs)4 7/3/2003 10 wet 10 wet not analyzed Soxhlet dichloromethane 12 h7 7/2/2003 5 wet 5 wet

approx 2 g dried at 70 oC 

for 48 h PFE dichloromethane 40 min

8 7/10/2003 6.008 wet 6.011 wet

105 oC until constant 

weight polytron dichloromethane 3 x 2.0 min each

filtered on glass fiber-filters (1.2 μm 

pore size) during extraction

9 7/11/2003 10 wet 10 wet EPA 160.3

SW-846 Method 3540B, 

Sonication dichloromethane:acetone (1:1) 4 x 2 min

11 7/11/2003 10.3 wet 8.2 wet drying and weighing grinding with sodium sulfate dichloromethane 3 x 3 min12 7/16/2003 5 wet 5 wet 1 g dried at 60  ̊C for 24h ultrasonic probe dichloromethane 3 x 3 min14 7/21/2003 1 wet

2 g dried at 100  ̊C for 

24h Soxhlet dichloromethane 18 h

15 8/13/2003 2.3 wet 2.3 wet 120  ̊C for 24h PFE dichloromethane 16 min temp = 100 oC; pressure 2000 psi

16 8/8/2003 1 g wet 1 g wet overnight at 100 oC PFE dichloromethane:hexane (1:1) 3 x 10 min static

17 7/10/2003 10 wet 5 wet 105  ̊C for at least 24h NOAA NS&T dichloromethane

2 x 2 min using tissuemizer 

and 1 x 30 min on shaker table

18 8/8/2003 5.29 wet 5.27 wet 105 oC oven PFE dichloromethane:acetone 15 min

19 8/22/2003 5 wet 5 wet 120 oC oven PFE dichloroemethane 3 x 5 min

sodium sulfate added prior to 

extraction

20 8/29/2003 5 wet 5 wet

105 oC until constant 

weight PFE dichloromethane 13 min

temp = 100 oC; pressure 2000 psi; 2 

static cycles / sample; reduce to 2 to 

3 mL using water bath
PCBs and Pesticides Method of 

Lab # Sample extract cleanup method Separated? quantitation

1a

gel permeation chromatography (GPC); silica solid phase extraction (SPE) column; condition and 

elute with 10 % dichloromethane in hexane no IS

1b GPC; silica SPE column; condition and elute with 10 % dichloromethane in hexane (2 x 10 mL) no IS

1c

1g florisil column; elute with 10.5 mL of dichloromethane:hexane (1:1); following analysis for PAHs 

fractionate on 1 g silica column - 1st fraction eluted with 5 mL hexane; 2nd fraction with 6 mL of 

dichloromethane:hexane (1:1) yes IS

2

PCBs - GPC (EPA 3640), florisil (EPA 3620), sulfuric acid (EPA 3665); PAHs - silica gel (EPA 

3630) no PAH - IS; PCBs- ES

4 GPC; Al/Si yes ES7 GPC and florisil no ES8 GPC; 7.3% deactivated silica gel for fractionation and clean-up yes IS9

PAH- EPA SW846 3640A (GPC); Pesticides - EPA SW846 3620B (florisil); PCBs - EPA SW846 

3620B (florisil) and 3665 (sulfuric acid) no

IS for PAH; ES for pesticides 

and PCBs

11 silica gel/ alumina and phenogel no IS12 GPC (OI analytical Envirobeads S-X3 temperature 19  ̊C) no

IS for PAH and PCBs; ES for 

pesticides

14 gravitational alumina column; gravitational florisil chromatography IS15 gravity flow column with silica and neutral alumina, followed by HPLC-SEC to elute AH/CH fraction no IS16

pesticides - GPC and multiple silica gel cleanup columns; PCBs - GPC followed by acid/base silica, 

alumina, and light acid/base silica columns IS

17

extracts concentrated; poured through 40g - 6% deactivated super B alumina column- eluted with 

dichloromethane and concentrated for HPLC/GPC fractionation no IS

18 silica gel no IS19

GPC (SDVB column w/ dichloromethane as mobile phase); 1/2 of extract- aliphatic/aromatic 

fractionation on silica SPE - aromatic fraction analyzed for PAH; other 1/2 of extract - 

PCB/pesticides fractionated on silica SPE yes IS

20

silica/alumina column chromatography, HPLC (phenogel 100 A column), reduce to 0.5 mL in water 

bath no IS
PAHs Calibration Curve

Lab # Instrument Phase Dimensions # points range

1 GC/MS DB-XLB 60m x 0.25 mm, 0.25um film 6 100 - 5000 ng/g

1b GC/MS DB-17MS 60m x 0.25 mm, 0.25um film 5 0.4 - 8 μg extracted

1c GC/MS DB-17 60m x 0.25 mm, 0.25um film 5 4 ng/μL to 0.015 ng/μL

2 GC/MS 5% phenyl 30m x 0.25 mm, 0.25um film 9 10 - 10000 ng/mL47 GC/MS DB-5 30m x 0.25 mm, 0.25um film 6 5 - 500 ppb8 GC/MS HP-5MS 30m x 0.25 mm, 0.25um film 5 10 - 500 ng/mL9 GC/MS Rtx-5MS 30m x 0.25 mm, 0.25um film 6 10 - 200 ng/mL

11 GC/MS DB-5MS 30m x 0.25 mm, 0.25um film 5 20 - 1000 ng/μL12 GC/MS 5% phenyl 30m x 0.25 mm, 0.50um film 7 10 - 250 ppb14 GC/MS DB-5 25m x 0.2 mm, 0.33um film 5 50 - 11408 ng/mL15 GC/MS DB-5 60m x 0.25 mm, 0.25um film 7 0.001 - 1 ng/μL1617 GC/MS DB-5 60m x 0.25 mm, 0.25um film 7 0.005 - 1018 GC/MS Rtx-5 30m x 0.25 mm, 0.25um film 6 10 - 10000 ng/mL19 GC-ITMS Rtx-5MS 30m x 0.25 mm, 0.25um film 7 30 - 13000 ng/mL20 GC/MS HP-5MS 60m x 0.25 mm, 0.25um film 5 20-1000 ng/mL
PCBs Calibration Curve PESTICIDES Calibration Curve

Lab # Instrument Phase Dimensions # points range Instrument Phase Dimensions # points range

1 GC/MS DB-XLB 60m x 0.25 mm, 0.25um 5 2 - 150 ng/g GC/MS DB-XLB 60m x 0.25 mm, 0.25um 5 2 - 150 ng/g

1b GC/MS DB-XLB 60m x 0.25 mm, 0.25um 5 12-260 ng extracted GC/MS DB-XLB 60m x 0.25 mm, 0.25um 5 13 - 235 ng extracted

1c GC-ECD DB-5/DB-XLB

60m x 0.25 mm, 0.25um 

film 5 0.003 - 0.25 ng/uL GC-ECD DB-5/DB-XLB

60m x 0.25 mm, 0.25um 

film 5 0.003 - 0.25 ng/μL

2 GC-ECD

DB-35MS/ DBXLB 30m x 0.32 mm, 0.25um film 6 2.5 - 200 ng/mL

4 GC-ECD Rtx-5/Rtx-1701

30m x 0.25 mm, 0.25um 

film 3 to 8 1 - 200 pg/μL

7 GC-ECD DB-5/DB-17

60m x 0.25 mm, 0.25um 

film 7 0.5 - 100 ppb GC-ECD DB-5/DB-17

60m x 0.25 mm, 0.25um 

film 7 0.5 - 100 ppb

8 GC-ECD

HP-5MS/ DB17 30m x 0.25 mm, 0.25um film 5 5 - 100 ng/mL GC-ECD HP-5MS/ DB-17 30m x 0.25 mm, 0.25um film 5 5 - 100 ng/mL

9 GC-ECD Rtx-5/Rtx-35

60m x 0.25 mm, 0.25um 

film 5 0.5 - 10 ng/mL GC-ECD Rtx-5/Rtx-35

60m x 0.25 mm, 0.25um 

film 5 0.5 - 10 ng/mL

11 GC-ECD DB-5

30m x 0.25 mm, 0.25um 

film 4 5 - 200 ng/μL GC-ECD DB-5

30m x 0.25 mm, 0.25um 

film 4 5 - 200 ng/μL

12 GC/MS 5% phenyl

30m x 0.25 mm, 0.25um 

film 8 5 - 85 ppb GC/MS 5% phenyl

30m x 0.25 mm, 0.25um 

film 6 5 - 80 ppb

14 GC-ECD DB-5

60m x 0.25 mm, 0.25um 

film 5 0.019 - 86 ng/mL GC-ECD DB-5

60m x 0.25 mm, 0.25um 

film 5 2 - 20 ng/mL

15 GC/MS DB-5

60m x 0.25 mm, 0.25um 

film 6 0.001 - 0.32 ng/μL GC/MS DB-5

60m x 0.25 mm, 0.25um 

film 6 0.001 - 0.32 ng/μL

16 GC/HRMS SPB-Octyl

30m x 0.25 mm, 0.25um 

film 6 0.2 - 2000 ng/mL GC/HRMS DB-5

60m x 0.32 mm, 0.25um 

film 6 2.5 - 2500 ng/mL

17 GC-ECD DB-5

60m x 0.25 mm, 0.25um 

film 7 0.001-.0126 GC-ECD DB-5

60m x 0.25 mm, 0.25um 

film 7 0.001-.0125

18 GC/MS Rtx-5

30m x 0.25 mm, 0.25um 

film 6 0.25 - 500 ng/mL GC/MS Rtx-5

30m x 0.25 mm, 0.25um 

film 6 1 - 500 ng/mL

19 GC-ECD Rtx-5/Rtx-50

30m x 0.25 mm, 0.25um 

film 6 0.40 - 100 ng/mL GC-ECD Rtx-5/DB-1701p

30m x 0.25 mm, 0.25um 

film 6 0.4 - 100 ng/mL

20 GC-ECD DB-5/DB-17

30m x 0.25 mm, 0.25um 

film 5 5 - 200 ng/mL GC-ECD DB-5/DB-17

30m x 0.25 mm, 0.25um 

film 5 5 - 200 ng/mL
PAHs corrected for

Lab # IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery? others?

1a

deuterated naphthalene, biphenyl, acenaphthene, phenanthrene, fluoranthene, pyrene, B[a]A, B[a]P, perylene, 

B[ghi]P, DB[a,h]A x

1b d-PAHs x

1c

deuterated naphthalene, biphenyl, acenaphthene, phenanthrene, fluoranthene, pyrene, B[a]A, B[a]P, perylene, 

B[ghi]P, DB[a,h]A x

2 surrogates- deuterated biphenyl, fluorene, fluoranthene, terphenyl IS- deuterated naphthalene, acenaphthene, phenanthrene, chrysene, perylene x n

47 x8 deuterated naphthalene, acenaphthene, phenanthrene, fluoranthene, chrysene, B[a]P deuterated fluorene, pyrene, peryleen x n

9 deuterated fluorene, and chrysene x n

11 deuterated naphthalene, acenaphthene, phenathrene, chrysene, and perylene x deuterated fluorene and B[a]P12 deuterated anthracene, B[a]P, DB[a,h]A, B[a]A x deuterated acenaphthene, perylene, phenanthrene, and chrysene x y14 deuterated naphthalene, fluorene, fluoranthene, and perylene deuterated pheanthrene x

15 deuterated naphthalene, acenphthene, B[a]P x hexamethylbenzene

1617 deuterated naphthalene, phenanthrene, chrysene deuterated acenaphthene, fluorene, B[a]P x y18 deuterated 2-methyl naphthalene, pyrene, B[b]F x deuterated naphthalene, acenphthene, phenanthrene, chrysene, perylene x19 18 deuterated PAHs (see notes) x deuterated terphenyl

20 surrogates- deuterated naphthalene, acenaphthene, phenanthrene, chrysene, perylene IS- deuterated fluorene, pyrene, B[a]P x y
PCBs corrected for Pesticides corrected for

Lab # IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery? others? IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery? others?

1a PCB 103, PCB 198, and deuterated DDD and DDT x PCB 103, PCB 198, and deuterated DDD and DDT x

1b C-13 labeled compounds x C-13 labeled compounds x

1c PCB 103 and 198 x deuterated 4,4'-DDE, 4,4'-DDT, 4,4'-DDD, and endosulfan x

247 x x8 g-chlordene, PCB 103, PCB 198 IS - 4,4'-dibromooctafluorobiphenyl x n g-chlordene, PCB 103, PCB 198 IS - 4,4'-dibromooctafluorobiphenyl x n

9

11 DBOFB, PCB 103, and PCB 198 x TCMX DFOFB, PCB 103, and PCB 198 x TCMX

12 C-13 labeled PCB 194 and 153 x C-13 labeled PCB 138 x y C-13 labled 4,4'-DDE x deuterated 4,4'-DDT x y 14 PCB 14, 65, 166 PCB 30 and 204 x

15 PCB 103 x tetrachloro-o-xylene PCB 103 x tetrachloro-o-xylene

16

Labeled PCB 

1,3,4,19,15,54,104,37,155,81,77,123,118,188,114,105,126,2

02,156,157,169,208,189,205,206,209 x labled PCB 9,52,138, 194

labeled 28, 111,178 added aft 

extraction / bef clean-up

carbon-13 labeled alpha-BHC, beta-BHC, HCB, 4,4'-DDE, 

2,4'-DDT, 4,4'-DDT, and methoxychlor; deuterated 

endosulfan-I, endosulfan-II, and 4,4'-DDD x

carbon-13 labeled delta-BHC and PCB 

101

17 PCB 104, 112, 14, and 35 PCB 166, 96, and 104 x y PCB 104, 112, 14, 35 PCB 166, 96, 103 x y 18 Carbon-13 labeled PCB 15 and PCB 202 x carbon-13 labeled PCB 15 and 180 x Carbon-13 labeled PCB 15 and PCB 202 x carbon-13 labeled PCB 15 and 180 x

19 PCB 103 and 198 x delta-HCH deuterated 4,4'-DDT and endosulfan-II x delta-HCH20

surrogate- 4,4'-dibromooctachlorobiphenyl, 2,3',4,5',6-

pentachlorobiphenyl, 2,2',3,3',4,5,5',6-octachlorobiphenyl IS -tetrachloro-meta-xylene x y 

surrogate- 4,4'-dibromooctachlorobiphenyl, 2,3',4,5',6-

pentachlorobiphenyl, 2,2',3,3',4,5,5',6-octachlorobiphenyl IS -tetrachloro-meta-xylene x y 
 

Appendix F: Laboratory Methods Used, Marine Sediment XII 
g extracted g extracted % water Extraction Extraction Extraction Extraction

Lab # Reported QA03SED12 SRM 1941b Determination Method Solvent Time other

1a 7/12/2003 6 wet 3 dry freeze-dry PFE dichloromethane 3 cycles each 5 min

temp = 100 oC; pressure 2000 psi; 3 

static cycles / sample

1b 10/6/2003 15 wet 10 dry not analyzed Soxhlet dichloromethane overnight activated Cu added to extracts

1c 10/15/2003 6 wet 5 dry freeze-dry PFE dichloromethane 3 cycles each 5 min

temp = 100 oC; pressure 2000 psi; 3 

static cycles / sample

2 6/17/2003

10 wet (5 for 

PAHs)

10 dry (5 for 

PAHs) overn drying - EPA 160.3

Soxhlet (EPA 3540) for PCB; 

automated Soxhlet (EPA 3541 dichloromethane 16 h (PCBs); 2 h (PAHs)

3 7/4/2003 3 wet 1 dry oven dry 105  ̊C for 17h automatic Soxhlet dichloromethane 35 min4 7/10/2003 8 wet 10 dry drying balance Soxhlet dichloromethane 12 h5 7/10/2003 7.5 wet 5 dry oven dry 105  ̊C for 24h PFE dichloromethane 20 min 2 cycles6 7/10/2003 15 wet 0.5 dry oven dry 100  ̊C for 24h PFE dichloromethane 20 min

7 7/2/2003 5 wet 5 dry

approx 2 g dried at 70 oC 

for 48 h PFE dichloromethane/acetone 40 min

9 7/11/2003 5 wet 5 dry EPA 160.3

SW-846 Method 3550B, 

Sonication dichloromethane:acetone (1:1) 4 x 2 min

10 7/11/2003 3 wet 3 dry

oven dry overnight at 105 

 ̊C sonication dichloromethane:acetone (1:1) - 100 mL 3 x 3 min

11 7/11/2003 10.5 wet 1 dry dry at 50  ̊C and weigh PFE dichloromethane 20 min12 7/16/2003 4 wet

air dry in fume hood for 

24h sonication with a probe dichloromethane 3 x 3 min

sonicated in 8 x the mass of 

sediment to volume of solvent

13 7/15/2003 6 wet 

10 g dry 

chlorinated 

and 1g PAHs EPA 160.3 PFE dichloromethane 5 min

temp = 100 oC - 5 min equilibration; 

pressure 1500 - 2000 psi; 0.6 x tube 

volume for flush; purge 45 sec 

nitrogen at 150 psi

14 7/21/2003 2 wet

2 g dried at 100  ̊C for 

24h Soxhlet dichloromethane 18 h

15 8/13/2003 3 wet 1.5 dry 120  ̊C for 24h PFE dichloromethane 16 min temp = 100 oC; pressure 2000 psi

16 8/8/2003 1.1 g wet 1.1 g wet overnight at 100 oC PFE toluene 2 x 5 min static

17 7/10/2003 12 wet 1.1 dry 105  ̊C for at least 24h NOAA NS&T dichloromethane

shaker table - 1st shake 12 h; 

second shake 4 h; third shake 

30 min

18 8/8/2003 5.22 wet 3.16 dry 105 oC oven PFE dichloromethane:acetone 15 min

19 8/22/2003 5 wet 4 dry 120 oC oven PFE dichloroemethane 3 x 5 min

sodium sulfate added prior to 

extraction

20 8/29/2003 4.1 wet 2 dry

105 oC until constant 

weight PFE dichloromethane 13 min

temp = 100 oC; pressure 2000 psi; 2 

static cycles / sample; reduce to 2 to 

3 mL using water bath
PCBs and Pesticides Method of 

Lab # Sample extract cleanup method Separated? quantitation

1a

gel permeation chromatography (GPC); silica solid phase extraction (SPE) column; condition and 

elute with 10 % dichloromethane in hexane no IS

1b SPE column; condition and elute with 10 % dichloromethane in hexane (2 x 20 mL) no IS

1c

1g florisil column - elute with 10.5 mL of dichloromethane:hexane (1:1); following analysis for PAHs 

fractionate on 1 g silica column - 1st fraction eluted with 5 mL hexane; 2nd fraction with 6 mL of 

dichloromethane:hexane (1:1); activated copper added prior to GC-ECD analysis yes IS

2

PCBs - GPC (EPA 3640), florisil (EPA 3620), copper (EPA 3660), sulfuric acid (EPA 3665); PAHs -

silica gel (EPA 3630) no PAH - IS; PCBs- ES

3 silica/alumina column yes IS4 GPC only for PAH; GPC plus alumina silica for pesticides PAH - IS; pesticides- ES5

50% sample used for PAH - silica gel column; 50% of sample used for Pest/PCB - florisil column - 

0% and 50% fractions collected ; aft florisil 0% fraction - tetrabutylammonium hydrogen sulfate 

extraction followed by conc H2SO4 partly PAH - IS; pest & PCBs- ES

6

silica gel and alumina column used to separate into aliphatic and aromatic components - aromatic 

fraction further cleaned up by GPC/HPLC fractionation IS

7 GPC and florisil no ES9

PAH- EPA SW846 3640A (GPC); Pesticides - EPA SW846 3620B (florisil); PCBs - EPA SW846 

3620B (florisil) and 3665 (sulfuric acid) no PAH - IS; pest & PCBs- ES

10 GPC SX-3 biobeads using 100% methylene chloride IS11 silica gel/ alumina no IS12

GPC (OI analytical Envirobeads S-X3 temperature 19  ̊C) - elute with 1:1 DCM:cyclohexane; treated 

for sulphur by adding 20-30 mesh copper pellets activated with HCl and solvent rinsed. no

IS for PAH and PCBs; ES for 

pesticides

13 PAH - alumina/activated copper; PCBs & pesticides - alumina/ activated copper; to hexane no IS14 gravitational alumina column; gravitational florisil chromatography yes IS15 gravity flow column with silica and neutral alumina, followed by HPLC-SEC to elute AH/CH fraction no IS16

pesticides - GPC and multiple silica gel cleanup columns; PCBs - GPC followed by acid/base silica, 

alumina, and light acid/base silica columns IS

17

extracts concentrated; poured through 40g - 6% deactivated super B alumina column- eluted with 

dichloromethane and concentrated for HPLC/GPC fractionation no IS

18 silica gel/ additional sulfuric acid for PCB congeners yes IS19

GPC (SDVB column w/ dichloromethane as mobile phase); 1/2 of extract- aliphatic/aromatic 

fractionation on silica SPE - aromatic fraction analyzed for PAH; other 1/2 of extract - 

PCB/pesticides fractionated on silica SPE yes IS

20

silica/alumina column chromatography, addition of copper granules for sulfur removal, reduce to 1.0 

mL no IS
PAHs Calibration Curve

Lab # Instrument Phase Dimensions # points range

1a GC/MS DB-XLB 60m x 0.25 mm, 0.25um film 6 20 - 1500 ng/g

1b GC/MS DB-17MS 60m x 0.25 mm, 0.25um film 5 0.4 - 8 μg extracted

1c GC/MS DB-17 60m x 0.25 mm, 0.25um film 5 4 ng/μL to 0.015 ng/μL

2 GC/MS 5% phenyl 30m x 0.25 mm, 0.25um film 9 10 - 10000 ng/mL3 GC/MS DB-5MS 30m x 0.25 mm, 0.25um film 5 20 - 800 ng/mL4 GC/MS 5% phenyl 30m x 0.25 mm, 0.25um film 7 50 - 1000 ng/g5 GC/MS DB-5 30m x 0.25 mm, 0.25um film 8 0.01 - 1.6 μg/mL6 GC/MS 5% phenyl 25m x 0.2 mm, 0.33um film 5 6 - 1800 ng/g7 GC/MS DB-5 30m x 0.25 mm, 0.25um film 6 5 - 500 ppb9 GC/MS Rtx-5MS 30m x 0.25 mm, 0.25um film 6 10 - 200 ng/mL

10 GC/MS 5% phenyl 30m x 0.25 mm, 0.25um film 13 0.005 - 40 ng11 GC/MS DB-5MS 30m x 0.25 mm, 0.25um film 5 20 - 1000 ng/μL12 GC/MS 5% phenyl 30m x 0.25 mm, 0.25um film 7 10 - 250 ppb13 Gc/MS DB-5MS 30m x 0.25 mm, 0.25um film 9 50 - 8000 ng/mL14 GC/MS DB-5 25m x 0.2 mm, 0.33um film 5 50 - 11408 ng/mL15 GC/MS DB-5 60m x 0.25 mm, 0.25um film 7 0.015 - 10 ng/μL1617 GC/MS DB-5 60m x 0.25 mm, 0.25um film

6 for # 1 

& 7 for # 

2&3

0.025 - 7.6 for sample 1 & 

0.005 - 10 for samples 2&3

18 GC/MS Rtx-5 30m x 0.25 mm, 0.25um film 6 10 - 10000 ng/mL19 GC-ITMS Rtx-5MS 30m x 0.25 mm, 0.25um film 7 30 - 10000 ng/mL20 GC/MS HP-5MS 60m x 0.25 mm, 0.25um film 5 20-1000 ng/mL
PCBs Calibration Curve PESTICIDES Calibration Curve

Lab # Instrument Phase Dimensions # points range Instrument Phase Dimensions # points range

1a GC/MS DB-XLB 60m x 0.25 mm, 0.25um 5 2 - 150 ng/g GC/MS DB-XLB 60m x 0.25 mm, 0.25um 5 2 - 150 ng/g

1b GC/MS DB-XLB 60m x 0.25 mm, 0.25um 5 12-260 ng extracted GC/MS DB-XLB 60m x 0.25 mm, 0.25um 5 13 - 235 ng extracted

1c GC-ECD DB-5/DB-XLB

60m x 0.25 mm, 0.25um 

film 5 0.003 - 0.25 ng/uL GC-ECD DB-5/DB-XLB

60m x 0.25 mm, 0.25um 

film 5 0.003 - 0.25 ng/μL

2 GC-ECD

DB-35MS/ DBXLB 30m x 0.32 mm, 0.25um film 6 2.5 - 200 ng/mL

34 GC-ECD Rtx-5/Rtx-1701

30m x 0.25 mm, 0.25um 

film 6 5 - 200 pg/μL

5 GC-ECD

RtxCLPesticides/Rtx-CLPesticides II

30m x 0.32 mm, 0.25um 

film 7 1 - 100 ng/mL GC-ECD

RtxCLPesticides/RtxCLPesticides II 30m x 0.32 mm, 0.5um film 8 1 - 250 ng/mL

67 GC-ECD DB-5/DB-17

60m x 0.25 mm, 0.25um 

film 7 0.5 - 100 ppb GC-ECD DB-5/DB-17

60m x 0.25 mm, 0.25um 

film 7 0.5 - 100 ppb

9 GC-ECD Rtx-5/Rtx-35

60m x 0.25 mm, 0.25um 

film 5 0.5 - 10 ng/mL GC-ECD Rtx-5/Rtx-35

60m x 0.25 mm, 0.25um 

film 5 0.5 - 10 ng/mL

1011 GC-ECD DB-5

30m x 0.25 mm, 0.25um 

film 4 5 - 200 ng/μL GC-ECD DB-5

30m x 0.25 mm, 0.25um 

film 4 5 - 200 ng/μL

12 GC/MS 5% phenyl

30m x 0.25 mm, 0.25um 

film 8 5 - 85 ppb GC/MS 5% phenyl

30m x 0.25 mm, 0.25um 

film 6 5 - 80 ppb

13 GC-ECD

DB-5MS/DB17MS 60m x 0.25 mm, 0.25um film 6 5 - 400 ng/mL GC-ECD DB-5MS/DB- 17MS 60m x 0.25 mm, 0.25um film 6 5 - 400 ng/mL

14 GC-ECD DB-5

60m x 0.25 mm, 0.25um 

film 5 0.019 - 86 ng/mL GC-ECD DB-5

60m x 0.25 mm, 0.25um 

film 5 1 - 10 ng/mL

15 GC/MS DB-5

60m x 0.25 mm, 0.25um 

film 6 0.001 - 0.32 ng/μL GC/MS DB-5

60m x 0.25 mm, 0.25um 

film 6 0.001 - 0.32 ng/μL

16 GC/HRMS SPB-Octyl

30m x 0.25 mm, 0.25um 

film 6 0.2 - 2000 ng/mL GC/HRMS DB-5

60m x 0.32 mm, 0.25um 

film 6 2.5 - 2500 ng/mL

17 GC-ECD DB-5

60m x 0.25 mm, 0.25um 

film 7 0.001-.0126 GC-ECD DB-5

60m x 0.25 mm, 0.25um 

film 7 0.001-.0125

18 GC/MS Rtx-5

30m x 0.25 mm, 0.25um 

film 6 0.25 - 500 ng/mL GC/MS Rtx-5

30m x 0.25 mm, 0.25um 

film 6 1 - 500 ng/mL

19 GC-ECD Rtx-5/Rtx-50

30m x 0.25 mm, 0.25um 

film 6 0.4 - 100 ng/mL GC-ECD Rtx-5/DB-1701p

30m x 0.25 mm, 0.25um 

film 6 0.4 - 100 ng/mL

20 GC-ECD DB-5/DB-17

30m x 0.25 mm, 0.25um 

film 5 5 - 200 ng/mL GC-ECD DB-5/DB-17

30m x 0.25 mm, 0.25um 

film 5 5 - 200 ng/mL
PAHs corrected for

Lab # IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery? others?

1a

deuterated naphthalene, biphenyl, acenaphthene, phenanthrene, fluoranthene, pyrene, B[a]A, B[a]P, perylene, 

B[ghi]P, DB[a,h]A x

1b d-PAHs x

1c

deuterated naphthalene, biphenyl, acenaphthene, phenanthrene, fluoranthene, pyrene, B[a]A, B[a]P, perylene, 

B[ghi]P, DB[a,h]A x

2 surrogates- deuterated biphenyl, fluorene, fluoranthene, terphenyl IS- deuterated naphthalene, acenaphthene, phenanthrene, chrysene, perylene x n

3 deuterated naphthalene, acenaphthylene, phenanthrene, fluoranthene, pyrene, B[a]P, B[e]P x y

deuterated anthracene and 

terphenyl added prior to 

extraction

4 deuterated nitrobenzene, 2-fluorobiphenyl, deuterated terphenyl

deuterated 1,4-dichlorobenzene, napthalene, acenaphthene, phenanthrene, chrysene, and 

perylene x n

deuterated B[e]P added prior 

to GPC cleanup

5

deuterated naphthalene, 2-methylnaphthalene, 1-methylnaphthalene, biphenyl, 2,6-dimethylnaphthalene, 

acenaphthylene, acenaphthene, fluorene, dibenzothiophene, phenanthrene, anthracene, fluoranthene, phyrene, 

B[a]A, chrysene, B[b]F, B[k]F, B[e]P, B[a]P, perylene, I[1,2,3-cd]P, DB[a,h]A, B[ghi]P x

6 deuterated naphthalene, acenaphthene, phenanthrene, chrysene, B[a]P, perylene x hexamethylbenzene7 x9 deuterated fluorene and chrysene x n

10 deuterated nitrobenzene, 1,2-dichlorobenzene, 2-fluorobiphenyl, terphenyl deuterated nitrobenzene, 1,2-dichlorobenzene, 2-fluorobiphenyl, terphenyl x

deuterated 1,4-

dichlorobenzene, 

naphthalene, acenaphthene, 

phenathrene, chrysene, 

perylene

11 deuterated naphthalene, acenaphthene, phenathrene, chrysene, and perylene x deuterated fluorene and B[a]P12 deuterated anthracene, B[a]P, DB[a,h]A, B[a]A x deuterated acenaphthene, perylene, phenanthrene, and chrysene x y13 deuterated naphthalene, acenaphthene, phenanthrene, chrysene, perylene x deuterated fluorene and B[a]P x y14 deuterated naphthalene, fluorene, fluoranthene, and perylene deuterated pheanthrene x y

15 deuterated naphthalene, acenphthene, B[a]P x hexamethylbenzene

deuterated phenanthrene 

added prior to HPLC-SEC

1617 deuterated naphthalene, phenanthrene, chrysene deuterated acenaphthene, fluorene, B[a]P x18 deuterated 2-methyl naphthalene, pyrene, B[b]F x deuterated naphthalene, acenphthene, phenanthrene, chrysene, perylene x19 18 deuterated PAHs (see notes) x deuterated terphenyl

20 surrogates- deuterated naphthalene, acenaphthene, phenanthrene, chrysene, perylene IS- deuterated fluorene, pyrene, B[a]P x y
PCBs corrected for Pesticides corrected for

Lab # IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery? others? IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery? others?

1a PCB 103, PCB 198, and deuterated DDD and DDT x PCB 103, PCB 198, and deuterated DDD and DDT x

1b C-13 labeled compounds x C-13 labeled compounds x

1c PCB 103 and 198 x deuterated 4,4'-DDE, 4,4'-DDT, 4,4'-DDD, and endosulfan x

234567 x x9

1011 DBOFB, PCB 103, and PCB 198 x TCMX DFOFB, PCB 103, and PCB 198 x TCMX

12 C-13 labeled PCB 194 and 153 x C-13 labeled PCB 138 x y C-13 labled 4,4'-DDE x deuterated 4,4'-DDT x y 

13 PCB 103 and 198 x TCMX x y TCMX x y 

14 PCB 14, 65, 166 PCB 30 and 204 x15 PCB 103 x tetrachloro-o-xylene TCMX prior to HPLC-SEC PCB 103 x tetrachloro-o-xylene TCMX prior to HPLC-SEC

16

Labeled PCB 

1,3,4,19,15,54,104,37,155,81,77,123,118,188,114,105,126,2

02,156,157,169,208,189,205,206,209 x labled PCB 9,52,138, 194

labeled 28, 111,178 added aft 

extraction / bef clean-up

carbon-13 labeled alpha-BHC, beta-BHC, HCB, 4,4'-DDE, 

2,4'-DDT, 4,4'-DDT, and methoxychlor; deuterated 

endosulfan-I, endosulfan-II, and 4,4'-DDD x

carbon-13 labeled delta-BHC and PCB 

101

17 PCB 104, 112, 14, and 35 PCB 166, 96, and 104 x PCB 104, 112, 14, 34 PCB 166, 96, 103 x

18 Carbon-13 labeled PCB 19 and PCB 202 x carbon-13 labeled PCB 15 and 180 x Carbon-13 labeled PCB 19 and PCB 202 x carbon-13 labeled PCB 15 and 180 x

19 PCB 103 and 198 x delta-HCH deuterated 4,4'-DDT and endosulfan-II x delta-HCH20

surrogate- 4,4'-dibromooctachlorobiphenyl, 2,3',4,5',6-

pentachlorobiphenyl, 2,2',3,3',4,5,5',6-octachlorobiphenyl IS -TCMX x y 

surrogate- 4,4'-dibromooctachlorobiphenyl, 2,3',4,5',6-

pentachlorobiphenyl, 2,2',3,3',4,5,5',6-octachlorobiphenyl IS -TCMX x y 
 

 

Appendix G: Charts of Mussel Tissue XI and SRM 1974b 

Results by Analyte 

See Tables 2 through 7 for results reported as <number, detection limit, etc. Also, note that lab 

9’s data plotted here are as per their original submission (in terms of dry mass). Lab 9 later 

submitted data in terms of wet mass as summarized in Tables 2 through 7. 

Charts for analytes with few reported numerical results are not included in this appendix. 

For Mussel Tissue XI plots: 

Solid line: exercise assigned value 

Dotted line: z = ± 1, i. e., 25 % from assigned value 

Dotted/dashed line: z = ± 2, i. e., 50 % from assigned value 

Dashed line: z = ± 3, i. e., 75 % from assigned value 

For SRM 1974b plots: 

Solid line: material certified concentration or target value (see caption of each plot) 

Dotted line: 95 % confidence interval (CI) 

Dashed line: 30 % from 95 % confidence interval (CI)
0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

naphthalene Tissue XI (QA03TIS11)

Assigned value = 2.19 ng/g s = 0.85 ng/g 95% CL = 0.79 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 11

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

naphthalene SRM 1974b

Certified Value = 2.43 ± 0.12 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 9

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

78.5 

Lab 9 – 

70.7 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

40.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

2-methylnaphthalene Tissue XI (QA03TIS11)

Assigned value = 2.27 ng/g s = 0.78 ng/g 95% CL = 0.82 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 12

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

5.0

10.0

15.0

20.0

25.0

30.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

2-methylnaphthalene SRM 1974b

Reference Value = 1.25 ± 0.09 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 10

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).
 

 

0.0

5.0

10.0

15.0

20.0

25.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

1-methylnaphthalene Tissue XI (QA03TIS11)

Assigned value = 1.65 ng/g s = 0.86 ng/g 95% CL = 0.90 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 12

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

1-methylnaphthalene SRM 1974b

Reference Value = 0.614 ± 0.050 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 10

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 14 – 

34.2 

Lab 14 – 

36.5 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

biphenyl Tissue XI (QA03TIS11)

Assigned value = 1.06 ng/g s = 0.34 ng/g 95% CL = 0.43 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 8

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g wet basis)

biphenyl SRM 1974b

Reference Value = 0.610 ± 0.140 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 7

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

2,6-dimethylnaphthalene Tissue XI (QA03TIS11)

Assigned value = 2.77 ng/g s = 0.52 ng/g 95% CL = 0.40 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 13

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g wet basis)

2,6-dimethylnaphthalene SRM 1974b

Reference Value = 0.330 ± 0.160 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 7

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9– 

35.6; Lab 

11- 47.77 
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

acenaphthylene Tissue XI (QA03TIS11)

Assigned value = 0.584 ng/g s = 0.169 ng/g 95% CL = 0.210 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 9

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

acenaphthylene SRM 1974b

Reference Value = 0.480 ± 0.120 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 9

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9– 

8.10; Lab 

11- 21.4 

Lab 11- 

6.60 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

1,6,7-trimethylnaphthalene Tissue XI (QA03TIS11)

Assigned value = 2.50 ng/g s = 0.84 ng/g 95% CL = 0.88 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 9

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

5.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

1,6,7-trimethylnaphthalene SRM 1974b

Reference Value = 0.400 ± 0.032 ng/g (wet basis)

Reported Results: 12 Quantitative Results: 8

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Lab 11- 

48.8 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

fluorene Tissue XI (QA03TIS11)

Assigned value = 2.26 ng/g s = 0.93 ng/g 95% CL = 0.98 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 10

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g wet basis)

fluorene SRM 1974b

Certified Value = 0.494 ± 0.036 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 9

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Lab 11- 

30.7 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

phenanthrene Tissue XI (QA03TIS11)

Assigned value = 10.8 ng/g s = 1.4 ng/g 95% CL = 0.9 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g wet basis)

phenanthrene SRM 1974b

Certified Value = 2.580 ± 0.110 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 - 

157; Lab 

11 - 123 
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

anthracene Tissue XI (QA03TIS11)

Assigned value = 0.939 ng/g s = 0.022 ng/g 95% CL = 0.197 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 8

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g wet basis)

anthracene SRM 1974b

Certified Value = 0.527 ± 0.071 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 10

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

17.3; Lab 

11 – 25.1 

Lab 9 – 

15.8; Lab 

11 – 15.6 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

1-methylphenanthrene Tissue XI (QA03TIS11)

Assigned value = 4.42 ng/g s = 0.86 ng/g 95% CL = 0.61 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 12

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g wet basis)

1-methylphenanthrene SRM 1974b

Certified Value = 0.980 ± 0.130 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 7

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

40.0; Lab 

11 – 57.8 

Lab 11 – 

9.59 
 

 

0.0

10.0

20.0

30.0

40.0

50.0

60.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

fluoranthene Tissue XI (QA03TIS11)

Assigned value = 28.2 ng/g s = 3.9 ng/g 95% CL = 2.6 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

5.0

10.0

15.0

20.0

25.0

30.0

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g wet basis)

fluoranthene SRM 1974b

Certified Value = 17.1 ± 0.7 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

252; Lab 

11 – 331 

Lab 9 – 

120; Lab 

11 – 169 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

40.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

pyrene Tissue XI (QA03TIS11)

Assigned value = 20.4 ng/g s = 2.7 ng/g 95% CL = 1.5 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

5.0

10.0

15.0

20.0

25.0

30.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

pyrene SRM 1974b

Certified Value = 18.0 ± 0.6 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

132; Lab 

11 – 176 

Lab 9 – 

191; Lab 

11 – 264 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

benz[a]anthracene Tissue XI (QA03TIS11)

Assigned value = 6.41 ng/g s = 1.25 ng/g 95% CL = 0.90 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

benz[a]anthracene SRM 1974b

Certified Value = 4.74 ± 0.53 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

72.7; Lab 

11 – 91.2 

Lab 9 –

48.7; Lab 

11 – 56.5 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

chrysene Tissue XI (QA03TIS11)

Assigned value = 12.8 ng/g s = 2.4 ng/g 95% CL = 6.0 ng/g (wet basis)

Reported Results: 9 Quantitative Results: 7

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g wet basis)

chrysene SRM 1974b

Certified Value = 6.30 ± 1.00 ng/g (wet basis)

Reported Results: 9 Quantitative Results: 7

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

173; Lab 

11 – 205 

Lab 9 –

87.8; Lab 

11 – 98.3 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

30.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

chrysene/triphenylene Tissue XI (QA03TIS11)

Assigned value = 16.3 ng/g s = 2.8 ng/g 95% CL = 2.6 ng/g (wet basis)

Reported Results: 7 Quantitative Results: 7

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

chrysene/triphenylene SRM 1974b

Target Value = 10.6 ± 1.2 ng/g (wet basis)

Reported Results: 7 Quantitative Results: 7

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

benzo[b]fluoranthene Tissue XI (QA03TIS11)

Assigned value = 7.32 ng/g s = 1.23 ng/g 95% CL = 0.94 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 11

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

benzo[b]fluoranthene SRM 1974b

Certified Value = 6.46 ± 0.59 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

80.1; Lab 

11 – 79.5 

Lab 9 –

106; Lab 

11 – 122 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

benzo[j]fluoranthene Tissue XI (QA03TIS11)

Assigned value = 3.38 ng/g s = 1.04 ng/g 95% CL = 1.65 ng/g (wet basis)

Reported Results: 6 Quantitative Results: 4

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

benzo[j]fluoranthene SRM 1974b

Certified Value = 2.99 ± 0.29 ng/g (wet basis)

Reported Results: 6 Quantitative Results: 4

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

benzo[k]fluoranthene Tissue XI (QA03TIS11)

Assigned value = 3.43 ng/g s = 1.28 ng/g 95% CL = 1.19 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 10

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

benzo[k]fluoranthene SRM 1974b

Certified Value = 3.16 ± 0.18 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 10

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

22.7; Lab 

11 – 24.0 

Lab 9 –

28.1; Lab 

11 – 27.5 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

18.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

benzo[e]pyrene Tissue XI (QA03TIS11)

Assigned value = 8.89 ng/g s = 1.48 ng/g 95% CL = 0.94 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

benzo[e]pyrene SRM 1974b

Certified Value = 10.3 ± 1.1 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

61.6; Lab 

11 – 85.0 

Lab 9 –

85.0; Lab 

11 – 95.0 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

benzo[a]pyrene Tissue XI (QA03TIS11)

Assigned value = 2.76 ng/g s = 1.07 ng/g 95% CL = 0.89 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 10

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

benzo[a]pyrene SRM 1974b

Certified Value = 2.80 ± 0.38 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Lab 11 – 

34.5 

Lab 9 –

79.2; Lab 

11 – 31.4 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

perylene Tissue XI (QA03TIS11)

Assigned value = 0.914 ng/g s = 0.257 ng/g 95% CL = 0.215 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 9

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

perylene SRM 1974b

Certified Value = 0.990 ± 0.140 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 8

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
 

 

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

indeno[1,2,3-cd]pyrene Tissue XI (QA03TIS11)

Assigned value = 2.04 ng/g s = 0.84 ng/g 95% CL = 0.65 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 11

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

indeno[1,2,3-cd]pyrene SRM 1974b

Certified Value = 2.14 ± 0.11 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 11

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

18.4; Lab 

11 – 21.3 

Lab 9 –

16.2; Lab 

11 – 18.5 
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

dibenz[a,h]anthracene Tissue XI (QA03TIS11)

Assigned value = 0.380 ng/g s = 0.137 ng/g 95% CL = 0.170 ng/g (wet basis)

Reported Results: 12 Quantitative Results: 7

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g wet basis)

dibenz[a,h]anthracene SRM 1974b

Certified Value = 0.327 ± 0.031 ng/g (wet basis)

Reported Results: 12 Quantitative Results: 7

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Lab 11 – 

4.31 

Lab 11 – 

4.37 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g, wet basis)

benzo[ghi]perylene Tissue XI (QA03TIS11)

Assigned value = 2.19 ng/g s = 0.82 ng/g 95% CL = 0.69 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 11

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

5.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

benzo[ghi]perylene SRM 1974b

Certified Value = 3.12 ± 0.33 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 11

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

22.6; Lab 

11 – 29.7 

Lab 9 – 

17.1; Lab 

11 – 22.5 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

heptachlor Tissue XI (QA03TIS11)

Assigned value = 0.263 ng/g s = 0.211 ng/g 95% CL = 0.335 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 5

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.000

0.100

0.200

0.300

0.400

0.500

0.600

0.700

0.800

0.900

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

heptachlor SRM 1974b

Reference Value = 0.212 ± 0.084 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 6

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
 

 

0.00

0.50

1.00

1.50

2.00

2.50

3.00

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g, wet basis)

gamma-chlordane Tissue XI (QA03TIS11)

Assigned value = 1.19 ng/g s = 0.52 ng/g 95% CL = 0.35 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

gamma-chlordane SRM 1974b

Certified Value = 1.14 ± 0.17 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 13

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

16.9; Lab 

11 – 11.4 

Lab 9 – 

17.0; Lab 

11 – 15.6 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

3.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

cis-chlordane (alpha-chlordane) Tissue XI (QA03TIS11)

Assigned value = 1.19 ng/g s = 0.26 ng/g 95% CL = 0.16 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

cis-chlordane (alpha-chlordane) SRM 1974b

Certified Value = 1.36 ± 0.10 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

11.2; Lab 

11 – 15.2 

Lab 9 – 

10.1; Lab 

11 – 12.4 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

trans-nonachlor Tissue XI (QA03TIS11)

Assigned value = 1.13 ng/g s = 0.28 ng/g 95% CL = 0.18 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

1a1b1c

24789

111214151617181920

laboratory number

concentration (ng/g wet basis)

trans-nonachlor SRM 1974b

Certified Value = 1.30 ± 0.14 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

9.85; Lab 

11 – 14.7 

Lab 9 – 

10.7; Lab 

11 – 12.8 
 

 

0.000

0.100

0.200

0.300

0.400

0.500

0.600

0.700

0.800

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

dieldrin Tissue XI (QA03TIS11)

Assigned value = 0.417 ng/g s = 0.050 ng/g 95% CL = 0.080 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 7

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

dieldrin SRM 1974b

Reference Value = 0.620 ± 0.130 ng/g (wet basis)

Reported Results: 12 Quantitative Results: 9

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

6.25; Lab 

11 – 8.37; 

Lab 18 – 

16.7 

Lab 9 – 

5.33; Lab 

11 – 8.92 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

4,4'-DDE Tissue XI (QA03TIS11)

Assigned value = 2.89 ng/g s = 0.56 ng/g 95% CL = 0.32 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

4,4'-DDE SRM 1974b

Certified Value = 4.15 ± 0.38 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

56.1; Lab 

11 – 41.6 

Lab 9 – 

51.6; Lab 

11 – 39.7 
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

2,4'-DDD Tissue XI (QA03TIS11)

Assigned value = 0.928 ng/g s = 0.172 ng/g 95% CL = 0.109 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

2,4'-DDD SRM 1974b

Reference Value = 1.09 ± 0.16 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Lab 11 – 

13.6 

Lab 11 – 

12.6 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

4,4'-DDD Tissue XI (QA03TIS11)

Assigned value = 2.54 ng/g s = 0.98 ng/g 95% CL = 0.66 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

4,4'-DDD SRM 1974b

Certified Value = 3.34 ± 0.22 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

30.1; Lab 

11 – 30.6 

Lab 9 – 

27.5; Lab 

11 – 31.5 
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

2.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

2,4'-DDT Tissue XI (QA03TIS11)

Assigned value = 0.722 ng/g s = 0.262 ng/g 95% CL = 0.417 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 6

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

2,4'-DDT SRM 1974b

Reference Value = 0.894 ± 0.057 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 8

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Lab 11 – 

6.14 

Lab 11 – 

8.92 
 

 

0.000

0.100

0.200

0.300

0.400

0.500

0.600

0.700

0.800

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

cis-nonachlor Tissue XI (QA03TIS11)

Assigned value = 0.435 ng/g s = 0.181 ng/g 95% CL = 0.151 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 10

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

cis-nonachlor SRM 1974b

Reference Value = 0.640 ± 0.160 ng/g (wet basis)

Reported Results: 12 Quantitative Results: 10

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

5.79; Lab 

11 – 9.20 

Lab 9 – 

8.27; Lab 

11 – 8.93 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

4,4'-DDT Tissue XI (QA03TIS11)

Assigned value = 0.903 ng/g s = 0.312 ng/g 95% CL = 0.289 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 11

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

5.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

4,4'-DDT SRM 1974b

Reference Value = 0.396 ± 0.096 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 10

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 8 Tissue XI (QA03TIS11)

Assigned value = 0.437 ng/g s = 0.262 ng/g 95% CL = 0.219 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 10

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.000

0.100

0.200

0.300

0.400

0.500

0.600

0.700

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 8 SRM 1974b

Reference Value = 0.370 ± 0.110 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 9

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

4.11; Lab 

11 – 8.60 

Lab 9 – 

3.37; Lab 

11 – 29.1 
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 18 Tissue XI (QA03TIS11)

Assigned value = 0.796 ng/g s = 0.186 ng/g 95% CL = 0.112 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 18 SRM 1974b

Certified Value = 0.840 ± 0.130 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

9.55; Lab 

11 – 11.7 

Lab 9 – 

8.41; Lab 

11 – 13.0 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 28 Tissue XI (QA03TIS11)

Assigned value = 3.00 ng/g s = 0.42 ng/g 95% CL = 0.28 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 28 SRM 1974b

Certified Value = 3.43 ± 0.25 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 13

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

27.2; Lab 

11 – 41.5 

Lab 9 – 

29.7; Lab 

11 – 44.3 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

5.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 31 Tissue XI (QA03TIS11)

Assigned value = 2.52 ng/g s = 0.41 ng/g 95% CL = 0.38 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 10

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 31 SRM 1974b

Certified Value = 2.88 ± 0.23 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 10

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

20.0; Lab 

11 – 18.7 

Lab 9 – 

15.3; Lab 

11 – 17.5 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 44 Tissue XI (QA03TIS11)

Assigned value = 3.41 ng/g s = 1.96 ng/g 95% CL = 1.18 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

10.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 44 SRM 1974b

Certified Value = 3.85 ± 0.20 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

29.2; Lab 

11 – 39.0 

Lab 9 – 

33.9; Lab 

11 – 41.8 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 49 Tissue XI (QA03TIS11)

Assigned value = 4.04 ng/g s = 0.92 ng/g 95% CL = 0.62 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 49 SRM 1974b

Certified Value = 5.66 ± 0.23 ng/g (wet basis)

Reported Results: 14 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

20.8; Lab 

11 – 71.4 

Lab 9 – 

18.8; Lab 

11 – 64.5 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 52 Tissue XI (QA03TIS11)

Assigned value = 4.71 ng/g s = 0.73 ng/g 95% CL = 0.44 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 52 SRM 1974b

Certified Value = 6.26 ± 0.37 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

42.3; Lab 

11 – 73.7 

Lab 9 – 

35.5; Lab 

11 – 69.9 
 

 

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 66 Tissue XI (QA03TIS11)

Assigned value = 5.29 ng/g s = 0.82 ng/g 95% CL = 0.55 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 66 SRM 1974b

Certified Value = 6.37 ± 0.37 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

68.4; Lab 

11 – 64.9 

Lab 9 – 

65.7; Lab 

11 – 61.8 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 95 Tissue XI (QA03TIS11)

Assigned value = 4.24 ng/g s = 0.70 ng/g 95% CL = 0.54 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 12

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 95 SRM 1974b

Certified Value = 6.04 ± 0.36 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 – 

39.1; Lab 

11 – 62.6 

Lab 9 – 

44.1; Lab 

11 – 67.9 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 99 Tissue XI (QA03TIS11)

Assigned value = 4.39 ng/g s = 0.83 ng/g 95% CL = 0.60 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 13

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 99 SRM 1974b

Certified Value = 5.92 ± 0.27 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 13

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

36.9; Lab 

11 – 71.6 

Lab 9 –

27.0; Lab 

11 – 63.7 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 101 Tissue XI (QA03TIS11)

Assigned value = 7.95 ng/g s = 0.86 ng/g 95% CL = 0.52 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

18.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 101 SRM 1974b

Certified Value = 10.70 ± 1.10 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 16

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

84.2; Lab 

11 – 114 

Lab 9 –

70.6; Lab 

11 – 109 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 105 Tissue XI (QA03TIS11)

Assigned value = 3.00 ng/g s = 0.43 ng/g 95% CL = 0.29 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 13

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 105 SRM 1974b

Certified Value = 4.00 ± 0.18 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 13

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

32.8; Lab 

11 – 44.3 

Lab 9 –

30.3; Lab 

11 – 41.5 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 118 Tissue XI (QA03TIS11)

Assigned value = 7.38 ng/g s = 0.63 ng/g 95% CL = 0.40 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 118 SRM 1974b

Certified Value = 10.3 ± 0.4 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

83.9; Lab 

11 – 122 

Lab 9 –

67.1; Lab 

11 – 104 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 128 Tissue XI (QA03TIS11)

Assigned value = 1.20 ng/g s = 0.20 ng/g 95% CL = 0.12 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 128 SRM 1974b

Certified Value = 1.79 ± 0.12 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

18.0; Lab 

11 – 21.0 

Lab 9 –

14.1; Lab 

11 – 17.5 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 138 Tissue XI (QA03TIS11)

Assigned value = 7.62 ng/g s = 1.69 ng/g 95% CL = 1.13 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 138 SRM 1974b

Certified Value = 9.20 ± 1.40 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

87.6; Lab 

11 – 127 

Lab 9 –

69.8; Lab 

11 – 109 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 149 Tissue XI (QA03TIS11)

Assigned value = 4.87 ng/g s = 0.64 ng/g 95% CL = 0.49 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 12

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 149 SRM 1974b

Certified Value = 7.01 ± 0.28 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

46.9; Lab 

11 – 71.0 

Lab 9 –

39.5; Lab 

11 – 67.3 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

18.0

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 153 Tissue XI (QA03TIS11)

Assigned value = 9.14 ng/g s = 1.39 ng/g 95% CL = 0.88 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

5.0

10.0

15.0

20.0

25.0

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 153 SRM 1974b

Certified Value = 12.30 ± 0.80 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

80.2; Lab 

11 – 164 

Lab 9 –

63.6; Lab 

11 – 143 
 

 

0.00

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

1a1b1c

24789

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laboratory number

concentration (ng/g, wet basis)

PCB 156 Tissue XI (QA03TIS11)

Assigned value = 0.521 ng/g s = 0.087 ng/g 95% CL = 0.067 ng/g (wet basis)

Reported Results: 12 Quantitative Results: 12

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1a1b1c

24789

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laboratory number

concentration (ng/g wet basis)

PCB 156 SRM 1974b

Certified Value = 0.718 ± 0.080 ng/g (wet basis)

Reported Results: 12 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

10.2; Lab 

11 – 22.0; 

Lab 12 – 

7.75 

Lab 9 –

10.0; Lab 

11 – 17.1; 

Lab 12 – 

7.75 
 

 

0.000

0.050

0.100

0.150

0.200

0.250

0.300

0.350

1a1b1c

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laboratory number

concentration (ng/g, wet basis)

PCB 170 Tissue XI (QA03TIS11)

Assigned value = 0.178 ng/g s = 0.101 ng/g 95% CL = 0.161 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 8

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.000

0.050

0.100

0.150

0.200

0.250

0.300

0.350

0.400

0.450

0.500

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laboratory number

concentration (ng/g wet basis)

PCB 170 SRM 1974b

Certified Value = 0.269 ± 0.034 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 9

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

1.69; Lab 

11 – 5.89 

Lab 9 –

1.68; Lab 

11 – 5.56 
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1a1b1c

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laboratory number

concentration (ng/g, wet basis)

PCB 180 Tissue XI (QA03TIS11)

Assigned value = 0.716 ng/g s = 0.144 ng/g 95% CL = 0.103 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

2.00

1a1b1c

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laboratory number

concentration (ng/g wet basis)

PCB 180 SRM 1974b

Certified Value = 1.17 ± 0.10 ng/g (wet basis)

Reported Results: 16 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

10.2; Lab 

11 – 33.4 

Lab 9 –

7.14; Lab 

11 – 35.1 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

1a1b1c

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laboratory number

concentration (ng/g, wet basis)

PCB 187 Tissue XI (QA03TIS11)

Assigned value = 2.05 ng/g s = 0.19 ng/g 95% CL = 0.12 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

1a1b1c

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laboratory number

concentration (ng/g wet basis)

PCB 187 SRM 1974b

Certified Value = 2.94 ± 0.15 ng/g (wet basis)

Reported Results: 15 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 9 originally submitted data in terms of wet mass. See Tables 2 through 7 for revised data (Lab 9 rev).

Lab 9 –

23.4; Lab 

11 –32.1 

Lab 9 –

20.9; Lab 

11 –29.8 
 

 

Appendix H: Charts of Marine Sediment XII and SRM 1941b 

Results by Analyte 

See Tables 8 through 13 for results reported as <number, detection limit, etc. 

Charts for analytes with few reported numerical results are not included in this appendix. 

For Marine Sediment XII plots: 

Solid line: exercise assigned value 

Dotted line: z = ± 1, i. e., 25 % from assigned value 

Dotted/dashed line: z = ± 2, i. e., 50 % from assigned value 

Dashed line: z = ± 3, i. e., 75 % from assigned value 

For SRM 1941b plots: 

Solid line: material certified concentration or target value (see caption of each plot) 

Dotted line: 95 % confidence interval (CI) 

Dashed line: 30 % from 95 % confidence interval (CI)
 

 

0

50

100

150

200

250

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laboratory number

concentration (ng/g, dry basis)

naphthalene Sediment XII (QA03SED12)

Assigned value = 117 ng/g s = 39 ng/g 95% CL = 22 ng/g (dry basis)

Reported Results: 19 Quantitative Results: 19

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

200

400

600

800

1000

1200

1400

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laboratory number

concentration (ng/g dry basis)

naphthalene SRM 1941b

Certified Value = 848 ± 95 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

20

40

60

80

100

120

140

160

180

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laboratory number

concentration (ng/g, dry basis)

2-methylnaphthalene Sediment XII (QA03SED12)

Assigned value = 80.6 ng/g s = 29.3 ng/g 95% CL = 16.2 ng/g (dry basis)

Reported Results: 19 Quantitative Results: 18

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

50

100

150

200

250

300

350

400

450

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laboratory number

concentration (ng/g dry basis)

2-methylnaphthalene SRM 1941b

Reference Value = 276 ± 53 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 16

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

20

40

60

80

100

120

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laboratory number

concentration (ng/g, dry basis)

1-methylnaphthalene Sediment XII (QA03SED12)

Assigned value = 54.2 ng/g s = 16.5 ng/g 95% CL = 9.6 ng/g (dry basis)

Reported Results: 18 Quantitative Results: 17

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

20

40

60

80

100

120

140

160

180

200

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laboratory number

concentration (ng/g dry basis)

1-methylnaphthalene SRM 1941b

Reference Value = 127 ± 14 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.0

10.0

20.0

30.0

40.0

50.0

60.0

70.0

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laboratory number

concentration (ng/g, dry basis)

biphenyl Sediment XII (QA03SED12)

Assigned value = 28.2 ng/g s = 9.3 ng/g 95% CL = 5.3 ng/g (dry basis)

Reported Results: 18 Quantitative Results: 17

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

20

40

60

80

100

120

140

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laboratory number

concentration (ng/g dry basis)

biphenyl SRM 1941b

Reference Value = 74 ± 8 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

20

40

60

80

100

120

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

2,6-dimethylnaphthalene Sediment XII (QA03SED12)

Assigned value = 39.7 ng/g s = 19.9 ng/g 95% CL = 12.0 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

20

40

60

80

100

120

140

160

180

1a1b1c

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laboratory number

concentration (ng/g dry basis)

2,6-dimethylnaphthalene SRM 1941b

Reference Value = 75.9 ± 4.5 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 16

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

20

40

60

80

100

120

140

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

acenaphthylene Sediment XII (QA03SED12)

Assigned value = 52.0 ng/g s = 34.5 ng/g 95% CL = 18.4 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

100

200

300

400

500

600

1a1b1c

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laboratory number

concentration (ng/g dry basis)

acenaphthylene SRM 1941b

Reference Value = 53.3 ± 6.4 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.0

10.0

20.0

30.0

40.0

50.0

60.0

70.0

80.0

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laboratory number

concentration (ng/g, dry basis)

acenaphthene Sediment XII (QA03SED12)

Assigned value = 37.1 ng/g s = 7.4 ng/g 95% CL = 4.1 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

50

100

150

200

250

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laboratory number

concentration (ng/g dry basis)

acenaphthene SRM 1941b

Reference Value = 38.4 ± 5.2 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.0

10.0

20.0

30.0

40.0

50.0

60.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

1,6,7-trimethylnaphthalene Sediment XII (QA03SED12)

Assigned value = 28.6 ng/g s = 6.6 ng/g 95% CL = 5.1 ng/g (dry basis)

Reported Results: 11 Quantitative Results: 10

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

10.0

20.0

30.0

40.0

50.0

60.0

70.0

1a1b1c

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laboratory number

concentration (ng/g dry basis)

1,6,7-trimethylnaphthalene SRM 1941b

Reference Value = 25.5 ± 5.1 ng/g (dry basis)

Reported Results: 10 Quantitative Results: 10

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

50

100

150

200

250

300

350

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laboratory number

concentration (ng/g, dry basis)

fluorene Sediment XII (QA03SED12)

Assigned value = 62.6 ng/g s = 15.2 ng/g 95% CL = 8.1 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

50

100

150

200

250

300

350

400

450

1a1b1c

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laboratory number

concentration (ng/g dry basis)

fluorene SRM 1941b

Certified Value = 85 ± 15 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

100

200

300

400

500

600

700

800

900

1000

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laboratory number

concentration (ng/g, dry basis)

phenanthrene Sediment XII (QA03SED12)

Assigned value = 505 ng/g s = 100 ng/g 95% CL = 53 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

500

1000

1500

2000

2500

3000

3500

4000

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laboratory number

concentration (ng/g dry basis)

phenanthrene SRM 1941b

Certified Value = 406 ± 44 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

100

200

300

400

500

600

700

800

900

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laboratory number

concentration (ng/g, dry basis)

anthracene Sediment XII (QA03SED12)

Assigned value = 147 ng/g s = 60 ng/g 95% CL = 32 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

100

200

300

400

500

600

700

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laboratory number

concentration (ng/g dry basis)

anthracene SRM 1941b

Certified Value = 184 ± 18 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

20

40

60

80

100

120

140

1a1c

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laboratory number

concentration (ng/g, dry basis)

1-methylphenanthrene Sediment XII (QA03SED12)

Assigned value = 70.5 ng/g s = 15.2 ng/g 95% CL = 8.8 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

20

40

60

80

100

120

1a1c

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laboratory number

concentration (ng/g dry basis)

1-methylphenanthrene SRM 1941b

Certified Value = 73.2 ± 5.9 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

200

400

600

800

1000

1200

1400

1600

1800

2000

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

fluoranthene Sediment XII (QA03SED12)

Assigned value = 1070 ng/g s = 203 ng/g 95% CL = 112 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

100

200

300

400

500

600

700

800

900

1000

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laboratory number

concentration (ng/g dry basis)

fluoranthene SRM 1941b

Certified Value = 651 ± 50 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 10 – 

6656 ng/g 
 

 

0

500

1000

1500

2000

2500

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laboratory number

concentration (ng/g, dry basis)

pyrene Sediment XII (QA03SED12)

Assigned value = 1099 ng/g s = 216 ng/g 95% CL = 115 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

100

200

300

400

500

600

700

800

900

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laboratory number

concentration (ng/g dry basis)

pyrene SRM 1941b

Certified Value = 581 ± 39 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 10 – 

6572 ng/g 
 

 

0

100

200

300

400

500

600

700

800

900

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laboratory number

concentration (ng/g, dry basis)

benz[a]anthracene Sediment XII (QA03SED12)

Assigned value = 442 ng/g s = 105 ng/g 95% CL = 54 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

50

100

150

200

250

300

350

400

450

500

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laboratory number

concentration (ng/g dry basis)

benz[a]anthracene SRM 1941b

Certified Value = 335 ± 25 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 10 – 

3310 ng/g 
 

 

0

200

400

600

800

1000

1200

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laboratory number

concentration (ng/g, dry basis)

chrysene Sediment XII (QA03SED12)

Assigned value = 640 ng/g s = 170 ng/g 95% CL = 142 ng/g (dry basis)

Reported Results: 11 Quantitative Results: 11

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

100

200

300

400

500

600

700

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laboratory number

concentration (ng/g dry basis)

chrysene SRM 1941b

Certified Value = 291 ± 31 ng/g (dry basis)

Reported Results: 10 Quantitative Results: 10

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 10 – 

4280 ng/g 
 

 

0

50

100

150

200

250

300

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laboratory number

concentration (ng/g, dry basis)

triphenylene Sediment XII (QA03SED12)

Assigned value = 144 ng/g s = 24 ng/g 95% CL = 60 ng/g (dry basis)

Reported Results: 3 Quantitative Results: 3

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

20

40

60

80

100

120

140

160

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laboratory number

concentration (ng/g dry basis)

triphenylene SRM 1941b

Certified Value = 108 ± 5 ng/g (dry basis)

Reported Results: 2 Quantitative Results: 2

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

200

400

600

800

1000

1200

1400

1600

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

chrysene+triphenylene Sediment XII (QA03SED12)

Assigned value = 817 ng/g s = 185 ng/g 95% CL = 154 ng/g (dry basis)

Reported Results: 8 Quantitative Results: 8

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

100

200

300

400

500

600

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laboratory number

concentration (ng/g dry basis)

chrysene+triphenylene SRM 1941b

Target Value = 400 ± 36 ng/g (dry basis)

Reported Results: 7 Quantitative Results: 7

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

200

400

600

800

1000

1200

1400

1600

1800

2000

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laboratory number

concentration (ng/g, dry basis)

benzo[b]fluoranthene Sediment XII (QA03SED12)

Assigned value = 999 ng/g s = 358 ng/g 95% CL = 207 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

100

200

300

400

500

600

700

800

1a1b1c

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laboratory number

concentration (ng/g dry basis)

benzo[b]fluoranthene SRM 1941b

Certified Value = 453 ± 21 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 10 –

2949 ng/g 
 

 

0

100

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300

400

500

600

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laboratory number

concentration (ng/g, dry basis)

benzo[j]fluoranthene Sediment XII (QA03SED12)

Assigned value = 280 ng/g s = 4 ng/g 95% CL = 11 ng/g (dry basis)

Reported Results: 3 Quantitative Results: 3

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

50

100

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200

250

300

350

1a1b1c

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laboratory number

concentration (ng/g dry basis)

benzo[j]fluoranthene SRM 1941b

Reference Value = 217 ± 5 ng/g (dry basis)

Reported Results: 3 Quantitative Results: 3

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

200

400

600

800

1000

1200

1400

1600

1800

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

benzo[j]+[k]fluoranthene Sediment XII (QA03SED12)

Assigned value = 943 ng/g s = 327 ng/g 95% CL = 406 ng/g (dry basis)

Reported Results: 5 Quantitative Results: 5

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

100

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400

500

600

700

1a1b1c

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laboratory number

concentration (ng/g dry basis)

benzo[j]+[k]fluoranthene SRM 1941b

Target Value = 442 ± 23 ng/g (dry basis)

Reported Results: 5 Quantitative Results: 5

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

200

400

600

800

1000

1200

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

benzo[k]fluoranthene Sediment XII (QA03SED12)

Assigned value = 392 ng/g s = 98 ng/g 95% CL = 70 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

100

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300

400

500

600

700

1a1b1c

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laboratory number

concentration (ng/g dry basis)

benzo[k]fluoranthene SRM 1941b

Certified Value = 225 ± 18 ng/g (dry basis)

Reported Results: 12 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 10 –

3358 ng/g 
 

 

0

200

400

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800

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1200

1400

1600

1800

2000

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

benzo[e]pyrene Sediment XII (QA03SED12)

Assigned value = 657 ng/g s = 186 ng/g 95% CL = 107 ng/g (dry basis)

Reported Results: 18 Quantitative Results: 18

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

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500

600

1a1b1c

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laboratory number

concentration (ng/g dry basis)

benzo[e]pyrene SRM 1941b

Certified Value = 325 ± 25 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0

200

400

600

800

1000

1200

1400

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

benzo[a]pyrene Sediment XII (QA03SED12)

Assigned value = 718 ng/g s = 238 ng/g 95% CL = 123 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

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500

600

1a1b1c

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laboratory number

concentration (ng/g dry basis)

benzo[a]pyrene SRM 1941b

Certified Value = 358 ± 17 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 10 –

2795 ng/g 
 

 

0

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400

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

perylene Sediment XII (QA03SED12)

Assigned value = 211 ng/g s = 60 ng/g 95% CL = 36 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

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600

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laboratory number

concentration (ng/g dry basis)

perylene SRM 1941b

Certified Value = 397 ± 45 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 14 –

2067 ng/g 
 

 

0

200

400

600

800

1000

1200

1400

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laboratory number

concentration (ng/g, dry basis)

indeno[1,2,3-cd]pyrene Sediment XII (QA03SED12)

Assigned value = 680 ng/g s = 214 ng/g 95% CL = 118 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

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300

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600

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laboratory number

concentration (ng/g dry basis)

indeno[1,2,3-cd]pyrene SRM 1941b

Certified Value = 341 ± 57 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 10 –

1875 ng/g 
 

 

0

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300

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laboratory number

concentration (ng/g, dry basis)

dibenz[a,h]anthracene Sediment XII (QA03SED12)

Assigned value = 137 ng/g s = 66 ng/g 95% CL = 44 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

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120

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laboratory number

concentration (ng/g dry basis)

dibenz[a,h]anthracene SRM 1941b

Certified Value = 53 ± 10 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 10 –

713 ng/g 
 

 

0

200

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1200

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laboratory number

concentration (ng/g, dry basis)

benzo[ghi]perylene Sediment XII (QA03SED12)

Assigned value = 608 ng/g s = 200 ng/g 95% CL = 103 ng/g (dry basis)

Reported Results: 20 Quantitative Results: 20

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0

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500

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laboratory number

concentration (ng/g dry basis)

benzo[ghi]perylene SRM 1941b

Certified Value = 307 ± 45 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 10 –

2205 ng/g 
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

hexachlorobenzene Sediment XII (QA03SED12)

Assigned value = 0.315 ng/g s = 0.123 ng/g 95% CL = 0.153 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 11

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

1a1b1c

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laboratory number

concentration (ng/g dry basis)

hexachlorobenzene SRM 1941b

Certified Value = 5.83 ± 0.38 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 4 –

7.20 ng/g 
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

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laboratory number

concentration (ng/g, dry basis)

gamma-chlordane Sediment XII (QA03SED12)

Assigned value = 0.753 ng/g s = 0.466 ng/g 95% CL = 0.431 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 8

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

1a1b1c

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laboratory number

concentration (ng/g dry basis)

gamma-chlordane SRM 1941b

Certified Value = 0.57 ± 0.09 ng/g (dry basis)

Reported Results: 13 Quantitative Results: 11

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

2,4'-DDE Sediment XII (QA03SED12)

Assigned value = 0.782 ng/g s = 0.299 ng/g 95% CL = 0.371 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 7

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.000

0.100

0.200

0.300

0.400

0.500

0.600

0.700

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laboratory number

concentration (ng/g dry basis)

2,4'-DDE SRM 1941b

Reference Value = 0.38 ± 0.12 ng/g (dry basis)

Reported Results: 13 Quantitative Results: 8

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 12 –

8.84 ng/g; 

Lab 14 – 

10.1 ng/g 

Lab 13 – 

8.10 ng/g 
 

 

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

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laboratory number

concentration (ng/g, dry basis)

cis-chlordane (alpha-chlordane) Sediment XII (QA03SED12)

Assigned value = 0.639 ng/g s = 0.326 ng/g 95% CL = 0.273 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 12

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

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laboratory number

concentration (ng/g dry basis)

cis-chlordane (alpha-chlordane) SRM 1941b

Certified Value = 0.85 ± 0.11 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 13

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

9.92 ng/g 

Lab 19 – 

5.63 ng/g 
 

 

0.00

0.20

0.40

0.60

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1.00

1.20

1.40

1.60

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laboratory number

concentration (ng/g, dry basis)

trans-nonachlor Sediment XII (QA03SED12)

Assigned value = 0.271 ng/g s = 0.144 ng/g 95% CL = 0.229 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 7

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.000

0.100

0.200

0.300

0.400

0.500

0.600

0.700

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laboratory number

concentration (ng/g dry basis)

trans-nonachlor SRM 1941b

Certified Value = 0.438 ± 0.073 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 11

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

5.39 ng/g 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

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laboratory number

concentration (ng/g, dry basis)

dieldrin Sediment XII (QA03SED12)

Assigned value = 0.978 ng/g s = 0.523 ng/g 95% CL = 0.484 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 7

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

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laboratory number

concentration (ng/g dry basis)

dieldrin SRM 1941b

Target Value = no target ng/g (dry basis)

Reported Results: 12 Quantitative Results: 7

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

18.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

4,4'-DDE Sediment XII (QA03SED12)

Assigned value = 7.30 ng/g s = 3.28 ng/g 95% CL = 1.98 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

5.00

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laboratory number

concentration (ng/g dry basis)

4,4'-DDE SRM 1941b

Certified Value = 3.22 ± 0.28 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 13

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

44.3 ng/g 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

2,4'-DDD Sediment XII (QA03SED12)

Assigned value = 6.93 ng/g s = 3.12 ng/g 95% CL = 2.10 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 12

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.0

5.0

10.0

15.0

20.0

25.0

30.0

1a1b1c

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laboratory number

concentration (ng/g dry basis)

2,4'-DDD SRM 1941b

Target Value = no target ng/g (dry basis)

Reported Results: 13 Quantitative Results: 8

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.0

5.0

10.0

15.0

20.0

25.0

30.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

4,4'-DDD Sediment XII (QA03SED12)

Assigned value = 15.3 ng/g s = 2.8 ng/g 95% CL = 1.9 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

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laboratory number

concentration (ng/g dry basis)

4,4'-DDD SRM 1941b

Certified Value = 4.66 ± 0.46 ng/g (dry basis)

Reported Results: 13 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

80.5 ng/g 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

2,4'-DDT Sediment XII (QA03SED12)

Assigned value = 5.09 ng/g s = 1.61 ng/g 95% CL = 0.93 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

2,4'-DDT SRM 1941b

Target Value = no target ng/g (dry basis)

Reported Results: 14 Quantitative Results: 3

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

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laboratory number

concentration (ng/g, dry basis)

cis-nonachlor Sediment XII (QA03SED12)

Assigned value = 1.38 ng/g s = 0.79 ng/g 95% CL = 1.25 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 5

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

2.00

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laboratory number

concentration (ng/g dry basis)

cis-nonachlor SRM 1941b

Certified Value = 0.378 ± 0.053 ng/g (dry basis)

Reported Results: 13 Quantitative Results: 8

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

40.0

45.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

4,4'-DDT Sediment XII (QA03SED12)

Assigned value = 18.6 ng/g s = 6.3 ng/g 95% CL = 3.7 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

2.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

4,4'-DDT SRM 1941b

Reference Value = 1.12 ± 0.42 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 11

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

107 ng/g 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 8 Sediment XII (QA03SED12)

Assigned value = 1.43 ng/g s = 0.77 ng/g 95% CL = 0.55 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 12

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 8 SRM 1941b

Certified Value = 1.65 ± 0.19 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

16.6 ng/g 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 18 Sediment XII (QA03SED12)

Assigned value = 3.12 ng/g s = 1.01 ng/g 95% CL = 0.58 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 18 SRM 1941b

Certified Value = 2.39 ± 0.29 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

41.5 ng/g 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 28 Sediment XII (QA03SED12)

Assigned value = 4.75 ng/g s = 1.19 ng/g 95% CL = 0.75 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 28 SRM 1941b

Certified Value = 4.52 ± 0.57 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

55.6 ng/g 
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 31 Sediment XII (QA03SED12)

Assigned value = 4.51 ng/g s = 1.41 ng/g 95% CL = 1.01 ng/g (dry basis)

Reported Results: 12 Quantitative Results: 10

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 31 SRM 1941b

Certified Value = 3.18 ± 0.41 ng/g (dry basis)

Reported Results: 11 Quantitative Results: 11

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

53.7 ng/g 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

18.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 44 Sediment XII (QA03SED12)

Assigned value = 9.09 ng/g s = 2.30 ng/g 95% CL = 1.39 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 44 SRM 1941b

Certified Value = 3.85 ± 0.20 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

34.9 ng/g 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 49 Sediment XII (QA03SED12)

Assigned value = 6.21 ng/g s = 1.91 ng/g 95% CL = 1.21 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 49 SRM 1941b

Certified Value = 4.34 ± 0.28 ng/g (dry basis)

Reported Results: 13 Quantitative Results: 13

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

36.0 ng/g 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

30.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 52 Sediment XII (QA03SED12)

Assigned value = 16.1 ng/g s = 4.6 ng/g 95% CL = 2.8 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 52 SRM 1941b

Certified Value = 5.24 ± 0.28 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

47.7 ng/g 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 66 Sediment XII (QA03SED12)

Assigned value = 8.46 ng/g s = 2.22 ng/g 95% CL = 1.34 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 66 SRM 1941b

Certified Value = 4.96 ± 0.53 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

b

Lab 13 – 

42.3 ng/g 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

40.0

45.0

50.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 95 Sediment XII (QA03SED12)

Assigned value = 23.4 ng/g s = 10.1 ng/g 95% CL = 6.8 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 13

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 95 SRM 1941b

Certified Value = 3.93 ± 0.62 ng/g (dry basis)

Reported Results: 12 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

30.2 ng/g 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 99 Sediment XII (QA03SED12)

Assigned value = 11.5 ng/g s = 5.3 ng/g 95% CL = 3.8 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 13

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 99 SRM 1941b

Certified Value = 2.90 ± 0.36 ng/g (dry basis)

Reported Results: 12 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

19.0 ng/g 
 

 

0.0

10.0

20.0

30.0

40.0

50.0

60.0

70.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 101 Sediment XII (QA03SED12)

Assigned value = 34.9 ng/g s = 11.7 ng/g 95% CL = 6.8 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 101 SRM 1941b

Certified Value = 5.11 ± 0.34 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

42.6 ng/g 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 105 Sediment XII (QA03SED12)

Assigned value = 12.2 ng/g s = 4.5 ng/g 95% CL = 2.7 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 105 SRM 1941b

Certified Value = 1.43 ± 0.10 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

17.2 ng/g 
 

 

0.0

10.0

20.0

30.0

40.0

50.0

60.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 118 Sediment XII (QA03SED12)

Assigned value = 27.6 ng/g s = 10.0 ng/g 95% CL = 6.1 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 118 SRM 1941b

Certified Value = 4.23 ± 0.19 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

37.5 ng/g 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 128 Sediment XII (QA03SED12)

Assigned value = 7.65 ng/g s = 2.50 ng/g 95% CL = 1.51 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 128 SRM 1941b

Certified Value = 0.696 ± 0.044 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

6.63 ng/g 
 

 

0.0

10.0

20.0

30.0

40.0

50.0

60.0

70.0

80.0

90.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 138 Sediment XII (QA03SED12)

Assigned value = 36.7 ng/g s = 11.3 ng/g 95% CL = 7.6 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 138 SRM 1941b

Certified Value = 3.60 ± 0.28 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 – 

26.9 ng/g 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

40.0

45.0

50.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 149 Sediment XII (QA03SED12)

Assigned value = 26.6 ng/g s = 8.9 ng/g 95% CL = 6.0 ng/g (dry basis)

Reported Results: 13 Quantitative Results: 13

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 149 SRM 1941b

Certified Value = 4.35 ± 0.26 ng/g (dry basis)

Reported Results: 12 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 –

28.3 ng/g 
 

 

0.0

10.0

20.0

30.0

40.0

50.0

60.0

70.0

80.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 153 Sediment XII (QA03SED12)

Assigned value = 41.5 ng/g s = 19.2 ng/g 95% CL = 11.6 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 153 SRM 1941b

Certified Value = 5.47 ± 0.32 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 13 –

53.9 ng/g 
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 156 Sediment XII (QA03SED12)

Assigned value = 4.43 ng/g s = 1.80 ng/g 95% CL = 1.29 ng/g (dry basis)

Reported Results: 13 Quantitative Results: 12

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 156 SRM 1941b

Certified Value = 0.507 ± 0.090 ng/g (dry basis)

Reported Results: 12 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

18.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 170 Sediment XII (QA03SED12)

Assigned value = 9.11 ng/g s = 3.75 ng/g 95% CL = 2.52 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

2.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 170 SRM 1941b

Certified Value = 1.35 ± 0.09 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

Lab 11 –

23.1 ng/g; 

lab 13 – 

12.6 ng/g 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

40.0

1a1b1c

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laboratory number

concentration (ng/g, dry basis)

PCB 180 Sediment XII (QA03SED12)

Assigned value = 19.1 ng/g s = 6.2 ng/g 95% CL = 3.7 ng/g (dry basis)

Reported Results: 17 Quantitative Results: 17

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

5.00

1a1b1c

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laboratory number

concentration (ng/g dry basis)

PCB 180 SRM 1941b

Certified Value = 3.24 ± 0.51 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

lab 13 – 

35.8 ng/g 
 

 

0.0

5.0

10.0

15.0

20.0

25.0

1a1b1c

2345679

1011121314151617181920

laboratory number

concentration (ng/g, dry basis)

PCB 187 Sediment XII (QA03SED12)

Assigned value = 10.8 ng/g s = 3.5 ng/g 95% CL = 2.1 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

2.00

4.00

6.00

8.00

10.00

12.00

14.00

1a1b1c

2345679

1011121314151617181920

laboratory number

concentration (ng/g dry basis)

PCB 187 SRM 1941b

Certified Value = 2.17 ± 0.22 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

1a1b1c

2345679

1011121314151617181920

laboratory number

concentration (ng/g, dry basis)

PCB 194 Sediment XII (QA03SED12)

Assigned value = 3.86 ng/g s = 2.16 ng/g 95% CL = 1.45 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 14

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

1a1b1c

2345679

1011121314151617181920

laboratory number

concentration (ng/g dry basis)

PCB 194 SRM 1941b

Certified Value = 1.04 ± 0.06 ng/g (dry basis)

Reported Results: 12 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.

lab 13 – 

9.92 ng/g 
 

 

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

1a1b1c

2345679

1011121314151617181920

laboratory number

concentration (ng/g, dry basis)

PCB 195 Sediment XII (QA03SED12)

Assigned value = 1.79 ng/g s = 0.63 ng/g 95% CL = 0.40 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 15

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

1a1b1c

2345679

1011121314151617181920

laboratory number

concentration (ng/g dry basis)

PCB 195 SRM 1941b

Certified Value = 0.645 ± 0.060 ng/g (dry basis)

Reported Results: 15 Quantitative Results: 12

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.00

1.00

2.00

3.00

4.00

5.00

6.00

1a1b1c

2345679

1011121314151617181920

laboratory number

concentration (ng/g, dry basis)

PCB 206 Sediment XII (QA03SED12)

Assigned value = 2.57 ng/g s = 1.25 ng/g 95% CL = 0.75 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

1a1b1c

2345679

1011121314151617181920

laboratory number

concentration (ng/g dry basis)

PCB 206 SRM 1941b

Certified Value = 2.42 ± 0.19 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 13

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

1a1b1c

2345679

1011121314151617181920

laboratory number

concentration (ng/g, dry basis)

PCB 209 Sediment XII (QA03SED12)

Assigned value = 1.62 ng/g s = 1.10 ng/g 95% CL = 0.63 ng/g (dry basis)

Reported Results: 16 Quantitative Results: 16

Solid line : exercise assigned value (EAV); dotted line: z=±1 (25% from EAV); dotted/dashed 

line: z=±2 (50% from EAV); dashed line: z=±3 (75% from EAV)

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

1a1b1c

2345679

1011121314151617181920

laboratory number

concentration (ng/g dry basis)

PCB 209 SRM 1941b

Certified Value = 4.86 ± 0.45 ng/g (dry basis)

Reported Results: 14 Quantitative Results: 14

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits

Note: Lab 3 used SRM 1941a as the control, and labs 5, 6, 17, and 18 used SRM 1944.
 

 

Appendix I: List of Laboratories Participating 

in 2003 Intercomparison Exercises

For this exercise, data were received from the following laboratories within the required 

timeframe. (This listing does NOT correspond to the laboratory number identification 

codes used in this report which were assigned in order of receipt of data with the 

exception of NIST which is Laboratory #1 in this exercise. The same code was used for 

both exercises.) 

Academy of Natural Sciences 

1900 Benjamin Franklin Parkway 

Philadelphia, PA 19103 

Jeffrey Ashley 

B& B Laboratories 

1902 Pinon 

College Station, TX 77845 

Jaun Ramirez 

Battelle Columbus 

505 King Ave 

Columbus, OH 43201 

Mary Schrock 

Battelle Duxbury Operations 

397 Washington Street 

Duxbury, MA 02332 

Carole-Sue Peven McCarthy 

Bedford Institute of Oceanography 

Marine Environmental Sciences Division 

1 Challenger Drive 

P.O. Box 1006 

Dartmouth, NS B2Y 4A2 

Sean Stellar 

CA Dept. of Fish and Game 

2005 Nimbus Road 

Rancho Cordova, CA 95670 

Kathleen Regaldo and David Crane 

Columbia Analytical Services 

1317 S. 13th Avenue 

Kelso, WA 98626 

Lee Wolf 
 

 

East Bay Municipal Utility District 

PO Box 24055, MS 59 

Oakland, CA 94623 

François Rodigari 

Environment Canada 

Environmental Science Center 

Corner Morton & Université Ave 

Moncton, NB E1A3E9 Canada 

Jamie Aubé 

Freshwater Institute 

Dept of Fisheries and Oceans 

501 University Crescent 

Winnipeg, Manitoba, Canada 

Brian Billeck 

King County Environmental Laboratory 

322 West Ewing Street 

Seattle, WA 98119 

Michael Doubrava 

Manchester Environmental Laboratory 

7411 Beach Drive East 

Port Orchard, WA 98366 

Karin Feddersen 

Massachusetts Water Resources Authourity 

100 Tafts Ave. 

Winthrop, MA 02152 

Jennifer Prasse / Mark Lambert 

NIST 

100 Bureau Drive, Stop 8392 

Gaithersburg, MD 20899-8392 

Michele Schantz / Dianne Poster 

NIST-Charleston Laboratory 

219 Fort Johnson Road 

Charleston, SC 29412-9110 

John Kucklick 

NOAA Fisheries / ABL 

11305 Glacier Hwy 

Juneau, AK 99801 

Marie Larsen 
 

 

NOAA-NMFS 

2725 Montlake Boulevard, East 

Seattle, WA 98112 

Donald Brown / Jennie Bolton 

NOAA/NOS/CCEHBR 

219 Fort Johnson Road 

Charleston, SC 29412 

Dan Bearden 

Texas A & M University 

GERG 

833 Graham Road 

College Station, TX 77845 

Terry Wade 

USGS 

National Water Quality Laboratory 

PO Box 25046 

Denver Federal Center 

Bldg 95, Ent E3, MS 407 

Denver, CO 80225-0048 

Mary Cast 

Woods Hole Group Environ. Lab 

375 Paramount Dr, Suite B 

Raynham, MA 02767 

Elizabeth Porta