Interlaboratory Analytical Comparison 

Study to Support Deepwater Horizon 

Natural Resource Damage Assessment: 

Description and Results for Mussel 

Tissue QA10TIS01

Michele M. Schantz

John R. Kucklick

NISTIR 7819
2

NISTIR 7819

Interlaboratory Analytical Comparison Study to Support 

Deepwater Horizon Natural Resource Damage 

Assessment: Description and Results for Mussel Tissue

QA10TIS01

Michele M. Schantz and John R. Kucklick

Analytical Chemistry Division

Material Measurement Laboratory

National Institute of Standards and Technology

Gaithersburg, MD 20899 and Charleston, SC 29412

September 2011

U.S. Department of Commerce

Rebecca M. Blank, Acting Secretary

National Institute of Standards and Technology

Patrick D. Gallagher, Under Secretary for Standards and Technology and Director
3

ABSTRACT

To support natural resource damage assessment (NRDA) in response to the Deepwater Horizon (DWH) 

oil spill in the Gulf of Mexico, a large number of coastal sediment and tissue (i.e., oysters) samples 

have been collected outside of the spill zone to define baseline environmental conditions prior to being 

exposed to oil. Analysis of oiled sediments and oil-exposed oysters will continue for the foreseeable 

future. To support these efforts, NOAA will require additional analytical laboratories to perform

NRDA sample analyses in addition to the commercial laboratories currently providing analyses in 

support of NRDA. To compare the data among these laboratories, inter-laboratory comparison studies 

have been initiated with the results from the third exercise, mussel tissue QA10TIS01 reported here. In 

this exercise, selected polycyclic aromatic hydrocarbons (PAHs), alkylated PAHs, hopanes, and 

steranes were determined in the exercise material, which consisted of a cryogenically homogenized 

mussel tissue sample, and in SRM 1974b Organics in Mussel Tissue (Mytilus edulis). The results from 

this third exercise are reported along with a summary of the analytical methods used. 

INTRODUCTION

On April 20, 2010, a fatal explosion, fire, and sinking of BP’s Deepwater Horizon drilling rig occurred 

approximately 40 miles off the Louisiana coast. The disaster resulted in the discharge of tens of 

thousands of barrels of oil per day from the seafloor into the Gulf of Mexico. In what has become the 

worst offshore oil spill in U.S. history, a wide expanse and variety of natural resources have become 

exposed and potentially impacted by oil and other consequences of the spill. Under the Oil Pollution

Act, those responsible for an oil spill are liable for clean-up and for natural resource damages. Several 

federal and state agencies are conducting a natural resource damage assessment (NRDA) to determine 

what resources have been injured and what uses of the resources have been lost due to the spill. 

To support this NRDA, the trustees and BP’s representatives have been collecting and analyzing tens of 

thousands of environmental samples to characterize both pre-spill and post-spill environmental 

conditions. A broad range of sample types have been collected including oil in various forms, water, 

sediment, and biota. For the foreseeable future, subsequent sampling and analysis will be required. In 

addition, numerous other entities have collected environmental samples for hydrocarbon analysis and 

submitted them to different laboratories throughout the country. 

In the past the National Institute of Standards and Technology (NIST) has helped benchmark and 

improve the quality of analytical data gathered on the marine environment by administering 

interlaboratory comparison exercises. To compare the data among the many laboratories analyzing 

samples from this spill, the National Oceanic and Atmospheric Administration (NOAA) has requested 

that NIST coordinate interlaboratory comparison studies with sediment, crude oil, and bivalve tissue 

being the three matrices of interest. These studies are performance-based with each laboratory using its 

current methods for analysis of similar matrices that it would use for its program customers. The target 

analytes for each study are selected polycyclic aromatic hydrocarbons (PAHs), alkylated PAHs, 

hopanes, and steranes. More than three dozen laboratory facilities were contacted by NOAA and 

invited to participate in the studies; for all three matrix studies a large number of laboratories agreed to 

receive samples and report their analytical results to NIST.

The data received from 34 laboratories for the mussel tissue QA10TIS01 are summarized in this report

along with summaries of the analytical methods used by each laboratory. Numerical indices, z- and p-
4

scores, are used to assess and track laboratory performances for accuracy and precision, respectively, 

and to provide a mechanism for assessing the comparability of data produced by the participating 

laboratories for the target analytes. 

SOURCE OF MATERIAL 

A previous tissue control material (NIST/NOAA NS&T QA Program Tissue Control Material III 

QC90TC Prepared Summer 90) was relabeled for use as the unknown material in this exercise. The 

new labels read:

Intercomparison Exercise to Support DWH NRDA

Sample: QA10TIS01 Mussel Tissue

Bottle # ---

Prepared Nov 2010

The mussels used for preparation of QC90TC were collected and stored at one of the NOAA NS&T 

laboratories prior to being shucked and shipped to NIST. QC90TC was prepared by NIST in 1990 as a 

frozen bivalve tissue homogenate still containing its endogenous water. The material was used by the 

NS&T laboratories in an interlaboratory study in 1991 [3]. 

SAMPLE DISTRIBUTION

Three bottles of QA10TIS01 Mussel Tissue each containing approximately 15 g of frozen mussel tissue 

were distributed to each of 45 laboratories during the week of February 21, 2011. Each laboratory was 

requested to analyze three samples of QA10TIS01 mussel tissue and at least one or more samples of 

SRM 1974b Organics in Mussel Tissue (Mytilus edulis) [4] (not provided to the laboratories) with their 

laboratory's and/or program's current analytical protocols being used for the determination of the 

concentrations (mass fractions) of the parent polycyclic aromatic hydrocarbon (PAH) compounds, 

alkylated PAH compounds, hopanes, and steranes. 

The instructions including the list of target analytes sent to participants are attached in Appendix A.

EVALUATION OF EXERCISE RESULTS 

Establishment of the Assigned Values

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

replicate determinations of the “unknown” material QA10TIS01 and was requested to report results of 

concurrent analyses of NIST SRM 1974b Organics in Mussel Tissue (Mytilus edulis). Laboratories 

were requested to report these results to three significant figures and to provide brief descriptions of 

their 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 
5

as follows: A mean "<value" was used when three "<values" were reported; NA (not 

analyzed/determined) was used for three reported NAs; 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, SRM 1974b, was initially 

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 Certificate of Analysis for SRM 

974b [4]. The criterion of 30 % is the same as the one that was used for the National Oceanic and 

Atmospheric Administration (NOAA) Mussel Watch and National Status and Trends Quality 

Assurance Programs [5]. 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 judgment 

were used after viewing both normal and log-normal plots of the data. This judgment utilized 

knowledge of potential coeluters based on the laboratory's reported methods. In instances for 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 consensus means and other values.

REPORTED RESULTS

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

of the two NIST laboratories which are Lab 1 and 14 in this exercise. The laboratory mean replicate 

data are shown in Tables 1 to 3 for QA10TIS01. Included in these tables are the exercise assigned 

mean values and the standard deviation of the assigned mean values along with the exercise assigned 

median values. Summaries of the methods used by each laboratory are in Appendix B, and notes 

included by a laboratory with its data are listed in Appendix C. In Appendix D, charts of the mean 

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

the corresponding reference material, SRM 1974b. 

Performance Scores

The exercise coordinators recognize that different environmental monitoring programs have different 

data quality objectives and 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, each 

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 most 

environmental monitoring programs in their acceptability assessments. 

IUPAC guidelines 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 to compare the 
6

performance of different laboratories among the participants 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. 

The choice of σ is dependent upon data quality objectives of a particular program, or as ISO 17043 

suggests “a fitness for purpose goal for performance as determined by expert judgement” [6]. It can be 

"fixed" and arrived at by perception, prescription, or referenced 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. The measurement of analytes targeted in this study is 

not particularly problematic.

 

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

each laboratory using "25 % of the exercise assigned value" as the fixed target value for standard 

deviation for this program. The use of z-score (25 % X) is also taken from the NOAA Mussel Watch 

and National Status and Trends Quality Assurance Programs [5]. 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.

A common classification of z-scores is [7]:

z  2 Satisfactory

2 < z < 3 Questionable

z  3 Unsatisfactory.

This classification has been deemed acceptable within the measurement community. 

Tables 4 through 6 summarize the z-scores (25 %) for each laboratory for each reported analyte in 

QA10TIS01. 

Precision Assessment (p-score) 

p-score = σlab / σtarget

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 
7

15 %. Tables 7 through 9 summarize the relative standard deviations (RSDs) calculated from the three 

concentrations reported by the laboratory for each analyte quantified while Tables 10 through 12 

summarize the p-scores (15%). A p-score of 1 indicates that the laboratory’s CV was 15%, and a pscore of 2 indicates that the laboratory’s CV was 30%.

 

DISCUSSION

NOAA’s NRDA office solicited laboratories involved in the analysis of samples shortly after the DWH 

disaster for their interest in participating in this interlaboratory study for analytes of interest in bivalve 

tissue. The participation by the laboratories was voluntary, and samples of QA10TIS01 were provided 

free of charge. Laboratories were provided with information for ordering SRM 1974b (See Appendix 

A). Interested laboratories were requested to quantify selected PAHs, alkylated PAHs (some individual 

and some as groups), and biomarkers (hopanes and steranes) in three aliquots of QA10TIS01 and SRM 

1974b using their laboratories’ analytical protocols for these analyses. A total of 45 laboratories 

received samples of which 34 laboratories submitted data. The 34 participating laboratories are listed 

in alphabetical order in Appendix E. 

Tables 1 through 3 summarize the laboratory means and exercise assigned values for the PAHs, 

alkylated PAHs, and hopanes and steranes, respectively. The consensus value for a given compound in

QA10TIS01 was derived by combining data where corresponding values in SRM 1974b were within 30 

% of the expanded uncertainty of the SRM value. In the absence of a corresponding SRM value, 

individual results were screened using outlier tests and included in the consensus value if values were 

shown not to be statistical outliers. Appendix D contains the charts of the QA10TIS01 and SRM 1974b

data by analyte. In these charts, the analytes that are not included on the Certificate of Analysis for 

SRM 1974b are shown with no target value; however, a median value calculated from the data 

submitted is included in each chart. Note that laboratory 24 submitted two sets of data, 24a and 24b. 

The differences in the two sets of data included the extraction method, accelerated solvent extraction 

(ASE) for 24a versus QuEChERS for 24b, and final analysis step, gas chromatography with mass 

spectrometric detection (GC/MS) for 24a and liquid chromatography with fluorescence detection (LCFLD) for 24b. 

No assigned values were calculated for chrysene, triphenylene, or benzo[j]fluoranthene in QA10TIS01. 

Chrysene and triphenylene coelute when using a 5% phenyl phase in GC analysis as do several of the 

benzofluoranthene isomers. Although several laboratories recognized and reported coelutions for 

chrysene with triphenylene and among the benzofluoranthenes using this phase, several did not, thus 

reporting the combined value for chrysene and triphenylene as only the chrysene peak and in a similar 

fashion for the benzofluoranthenes.

The spread in the PAH data for QA10TIS01 among the laboratories is highest for biphenyl, 

acenaphthylene, anthracene, benzo[a]fluoranthene and dibenz[a,h]anthracene, analytes that are either 

relatively volatile (biphenyl and acenaphthylene) or at relatively low mass fractions and determined by 

fewer laboratories. The range in mass fractions for the PAHs in the mussel tissue QA10TIS01 is from

3 ng/g for benzo[a]fluoranthene and dibenz[a,h]anthracene to 220 ng/g for fluorene. The agreement 

among the data for the PAHs was better in the previous crude oil study [2] than in this study or in the 

previous sediment study [1] suggesting that extraction and sample concentration may be issues. 
8

The alkylated PAH data for crude oil QA10 OIL01 [2] do not show as much spread among the 

laboratories as for the mussel tissue reported here or the sediment material QA10SED01 [1]. As for the 

previous studies, there are issues with the choice of the representative compound used for quantification 

of the alkylated PAHs, as well as the interpretation of the chromatograms as to what peaks should and 

should not be included in the summation for the alkylated groups. For an alkylated group of PAHs, the 

mass spectra are different based on where the PAH is alkylated (or if it is alkylated) thus resulting in 

different response factors for isomers in a homolog group. These issues need to be explored in more

detail in future discussions. 

Fewer laboratories reported data for the selected biomarkers with seven or fewer laboratories reporting 

quantitative results. The largest spread in the data seen for 5α(H),14α(H),17α(H)-cholestane 20R while 

very good agreement was seen for 17α(H),21β(H)-hopane (an RSD of 12%). The quantification issues 

for the hopanes and steranes include the lack of authentic calibration standards. 

A range of extraction methods was used in this study as summarized in Appendix B by laboratory: nine

data sets used Soxhlet extraction (Figure 1), five used QuEChERS (Figure 2), six used sonication 

(Figure 3), ten used ASE (Figure 4), three used a tissumizer (Figure 5), one used base digestion (Figure 

5), and one used microwave extraction (Figure 5). Figures 1 through 5 show the comparison among 

laboratories using the same extraction method for selected compounds along with the median for the 

data sets. Figure 6 compares the medians for each extraction method for the same selection of 

compounds. The data for all of the compounds are summarized by extraction method in Tables 13, 14, 

and 15 for the PAHs, alkylated PAHs, and hopanes and steranes, respectively. No concrete conclusions 

can be drawn from comparing the data obtained by the different extraction methods as there is a large 

spread in the data (see table below) from each extraction method, with the tissumizer results (from three 

laboratories being the least variable. This table summarizes the number of laboratories who performed

each extraction method (not necessarily reporting data for each analyte), the average relative standard 

deviations (avg RSD in %) for each class of compounds, and the number of compounds in each class 

for which more than one data set was received by the indicated extraction method (for n=). No data 

were excluded when calculating the RSDs shown. 

alkylated hopanes/

Extraction Method # labs PAHs total n=34 PAHs total n=40 steranes total n=18

reporting avg rsd (%) for n= avg rsd (%) for n= avg rsd (%) for n=

Soxhlet 9 50 27 50 31 35 2

QuEChERS 5 51 13 0 0

Tissumizer 3 18 24 27 38 27 17

Sonication 6 116 17 123 15 0

ASE 10 32 24 44 29 0

Base digestion 1 20 27 8

Microwave extraction 1 5 8 0

Caution should be used when interpreting these data as for the sonication method, one laboratory (17) 

reported high values for many of the analytes. These high values are probably not a result of the 

extraction method since their data for the corresponding analytes in SRM 1974b generally fell within

the 30% criterion mentioned in the “Determination of assigned values” section. See Appendix D for 

the charts of the individual analytes. 
9

The majority of the z-scores based on 25 % (Tables 4 through 6) are within ± 2 while the majority of 

the p-scores based on 15 % (Tables 10 through 12) are within ± 1. This indicates that the laboratories 

are internally consistent, but there is still a fair amount of spread in the data among the laboratories. 

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 Tables 1 through 3 

of this report. The laboratory and its data users should closely examine these non-quantitative 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 the 

exercise material that may be too high for the data quality objectives and needs of their program(s), and 

these issues should be assessed as well.

Intercomparison exercises provide an important mechanism for assessing the comparability, 

repeatability, and trueness 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 

measurement and method problems. Minimizing the among-laboratory biases so that the analytical 

variability is significantly less than the field sampling variability should be an achievable goal in 

environmental monitoring.

Acknowledgments

The time and effort of the analysts and management of the participating laboratories 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. Schantz, M.M. and Kucklick, J.R., Interlaboratory Analytical Comparisons Study to Support 

Deepwater Horizon Natural Resource Damage Assessment: Description and Results for Marine 

Sediment QA10SED01, NISTIR ???, Gaithersburg, MD (2011).

2. Schantz, M.M. and Kucklick, J.R., Interlaboratory Analytical Comparisons Study to Support 

Deepwater Horizon Natural Resource Damage Assessment: Description and Results for Crude 

Oil QA10OIL01, NISTIR ???, Gaithersburg, MD (2011).

3. NOAA Technical Memorandum NOS ORCA 79 Quality Assurance Project Intercomparison 

Exercise Results 1991-1993, August, 1995

4. Certificate of Analysis for Standard Reference Material (SRM) 974b Organics in Mussel Tissue 

(Mytilus edulis), National Institute of Standards and Technology (NIST), Gaithersburg, MD, 

2003. (https://www-s.nist.gov/srmors/view_detail.cfm?srm=1974B)
10

5. Schantz, M.M., Parris, R.M., and Wise, S.A., NIST Intercomparison Exercise Program for 

Organic Contaminants in the Marine Environment: Description and Results of 2007 Organic 

Intercomparison Exercises, NISTIR 7501, Gaithersburg, MD (2008).

6. ISO/IEC 17043: 2010 Conformity Assessment-General Requirements for Proficiency Testing

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

Analytical Laboratories,” Pure & Appl. Chem., 65 (9), 2123-2144 (1993).
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0

50

100

150

200

phenanthrene anthracene pyrene B[e]P B[a]P perylene I[1,2,3-cd]P B[ghi]P 2-me-naphth 1-me-phen 17α,21β-hopane

ng/g dry mass

1

4

7

10

12

13

15

20

26

median

Figure 1. Data from laboratories performing Soxhlet extraction. Medians are not calculated when there are two or fewer sets of data.
12

0

50

100

150

200

phenanthrene anthracene pyrene B[e]P B[a]P perylene I[1,2,3-cd]P B[ghi]P 2-me-naphth 1-me-phen 17α,21βhopane

ng/g dry mass

2

6

8

9

24b

median

Figure 2. Data from laboratories performing QuEChERS. Medians are not calculated when there are two or fewer sets of data.
13

0

50

100

150

200

250

phenanthrene anthracene pyrene B[e]P B[a]P perylene I[1,2,3-cd]P B[ghi]P 2-me-naphth 1-me-phen 17α,21βhopane

ng/g dry mass

3

17

19

25

30

31

median

760 733 653 2465 558

Figure 3. Data from laboratories performing sonication. Medians are not calculated when there are two or fewer sets of data.
14

0

50

100

150

200

phenanthrene anthracene pyrene B[e]P B[a]P perylene I[1,2,3-cd]P B[ghi]P 2-me-naphth 1-me-phen 17α,21βhopane

ng/g dry mass

5

11

14

18

21

24a

27

28

29

33

median

212

Figure 4. Data from laboratories performing ASE. Medians are not calculated when there are two or fewer sets of data.
15

0

50

100

150

200

phenanthrene anthracene pyrene B[e]P B[a]P perylene I[1,2,3-cd]P B[ghi]P 2-me-naphth 1-me-phen 17α,21βhopane

ng/g dry mass

16 - T

23-T

34-T

median-T

22-B

32M

Figure 5. Data from the three laboratories using the tissumizer method (T) along with the medians for that method and from the one 

laboratory using base digestion (B) and one laboratory using microwave extraction (M). Medians are not calculated when there are two or 

fewer sets of data.
16

0

50

100

150

200

phenanthrene anthracene pyrene B[e]P B[a]P perylene I[1,2,3-cd]P B[ghi]P 2-me-naphth 1-me-phen 17α,21βhopane

ng/g dry mass

Soxhlet 

QuChERS

Sonication

ASE

Tissumizer

Base dig

Microwave

Figure 6. Data comparison by extraction method. Medians are shown for the data sets with 2 or data points that were not excluded from the 

assignment of the consensus means. Otherwise, the data represent one set of data. See Tables 13 to 15 for the complete summary.
17

Table 1. Mussel Tissue (QA10TIS01): Laboratory means of three replicates and exercise assigned values - Water and PAHs 

 (reported as if three figures were significant)

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19

Percent Water 85.4 87.8 86.0 87.3 87.9 86.9 86.3 86.7 87.3 87.2 86.2 88.8 86.9 86.4 86.6 88.2 86.7 87.8 87.0

ng/g dry mass

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19

naphthalene 43.0 37.2 <294 19.7 12.9 104 36.2 31.3 other <5700 18.4 24.2 54.5 NA 350 34.6 625 30.2 <78

biphenyl 12.9 130 16.0 Other NA <14.8 NA NA <5700 NA 9.18 21.1 NA 18.3 13.6 567 19.1 <78

acenaphthene 14.0 nd <294 11.3 9.59 0.00 <14.8 <0.2 <11 <5700 NA 7.42 < 30 9.70 <10 11.7 <3.2 9.64 <78

acenaphthylene <10 <294 9.03 2.74 NA <14.8 <0.2 NA <5700 NA 4.50 < 30 8.08 12.7 10.7 <3.2 6.77 <78

fluorene 33.9 14.3 <294 24.3 26.0 43.6 19.8 25.2 17.7 <5700 19.7 14.8 33.3 30.9 25.3 24.0 227 20.3 <78

phenanthrene 119 56.1 101 97.0 149 153 139 134 144 <5700 114 117 126 114 127 157 760 118 99.3

anthracene 10.3 2.76 <294 13.3 10.0 12.1 <14.8 other 10.0 <5700 11.4 10.3 9.69 7.70 17.7 15.7 85 17.3 <78

fluoranthene 246 115 181 140 305 247 196 241 260 183 221 269 210 209 173 288 1160 303 207

pyrene 207 85.4 112 107 212 191 121 153 196 101 141 149 149 158 121 189 733 140 133

benzo[b]fluorene NA NA 17.3 NA NA NA NA NA NA NA 15.8 NA NA NA NA <3.2 NA NA

benz[a]anthracene 37.3 8.87 <294 19.7 57.8 49.9 16.3 28.3 other <5700 35.8 32.1 30.8 38.6 26.7 35.4 198 53.2 <78

chrysene coelute 59.1 <294 54.7 Other 94.8 93.9 49.8 107 <5700 96.2 73.0 52.9 35.3 88.3 coelute coelute 82.5 <78

triphenylene coelute NA Other NA NA NA NA NA NA NA NA 38.3 NA NA coelute 82.5 NA

chrysene/triphenylene 144 139 108 421

benzo[b ]fluoranthene 26.3 14.4 <294 20.7 38.1 29.8 21.9 27.3 30.8 <5700 44.0 25.0 35.1 31.0 Other 34.6 261 32.6 <78

benzo[j ]fluoranthene 28.6 NA Other NA NA NA NA NA NA NA NA 16.6 Other NA coelute NA NA

benzo[k ]fluoranthene 15.4 3.54 <294 13.0 Other 16.6 20.3 11.9 16.8 <5700 25.4 24.7 14.4 15.1 11.0 coelute coelute 14.7 <78

benzo[b+j ]fluoranthene 0.027

benzo[j+k ]fluoranthene 32.8 31.7 194

benzo[b+j+k ]fluoranthene

benzo[a]fluoranthene <10 NA 1.33 NA NA NA NA NA NA NA NA NA 5.42 NA NA <3.2 NA NA

benzo[e]pyrene 38.8 <294 24.3 48.9 NA 36.6 39.9 NA <5700 NA 29.3 39.9 36.1 NA 46.7 232 39.4 <78

benzo[a]pyrene 11.4 3.91 <294 7.40 11.8 14.7 <14.8 9.03 18.4 <5700 11.5 7.55 11.7 11.0 10.7 11.0 <3.2 16.7 <78

perylene 4.96 191 2.97 5.68 NA <14.8 NA NA <5700 NA 3.93 5.86 4.74 <10 6.55 <3.2 4.16 <78

indeno[1,2,3-cd]pyrene 4.75 nd <294 21.3 8.35 0.00 <14.8 5.83 <21 <5700 9.39 4.39 4.58 8.22 <10 7.70 207 7.65 <78

benzo[ghi]perylene 7.81 nd <294 6.67 10.8 3.83 <14.8 8.03 <7 <5700 NA 7.81 11.9 9.88 <10 9.92 204 13.1 <78

dibenz[a,h]anthracene 1.12 nd <294 0.00 Other 0.00 <14.8 <0.2 <9 <5700 18.2 2.28 2.11 <1.5 <10 2.54 175 3.14 <78

dibenz[a,h+a,c]anthracene 2.35

cis/trans-decalin NA NA 63.3 NA NA NA NA NA NA NA NA NA NA NA 142 <3.2 NA NA

dibenzofuran NA <294 21.3 NA NA NA NA NA NA NA 13.8 19.8 NA NA 18.2 143 NA <78

retene NA NA 42.3 11.8 NA NA NA NA NA NA 50.1 NA 28.3 30.0 56.2 245 NA NA

benzothiophene NA NA 0.00 NA NA <14.8 NA NA NA NA <40 NA NA NA 1.30 <3.2 NA NA

dibenzothiophene <15 <294 12.7 20.9 NA <14.8 NA NA <5700 NA 16.0 12.9 13.4 12.0 20.4 <3.2 11.8 <78

naphthobenzothiophene NA NA 11.7 Other NA NA NA NA NA NA 13.6 NA NA NA 7.41 <3.2 NA NA

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus statistics
18

Table 1 (cont). Mussel Tissue (QA10TIS01): Laboratory means of three replicates and exercise assigned values - Water and PAHs 

 (reported as if three figures were significant) Consensus Values (%)

Laboratory No. 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34 mean std dev median

Percent Water 86.7 85.6 86.8 85.4 84.6 84.6 87.0 87.1 84.9 85.9 86.9 85.5 NA 88.7 87.6 87.4 86.7 1.1 86.8

Consensus Values 

ng/g dry mass (ng/g dry mass)

Laboratory No. 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34 mean std dev median

naphthalene 37.0 23.0 24.3 26.5 47.0 117 <conc 24.3 <12.2 15.0 31.0 14.7 5.50 <26 22.5 28.4 27.2 9.2 30.2

biphenyl 35.0 NA 11.8 16.5 NA NA <conc 16.3 13.3 NA NA <39.8 6.87 <26 NA 12.2 16.6 6.4 16.1

acenaphthene < 7.4 6.67 10.4 9.06 NA DL <conc 11.1 7.12 NA DL 6.69 11.7 <26 NA 10.4 9.63 2.13 9.67

acenaphthylene 13.8 4.45 7.68 16.0 NA NA <conc 10.1 12.5 NA DL 6.29 <3.0 <26 NA 7.86 8.88 3.76 8.08

fluorene 23.5 20.6 18.6 20.8 DL DL <conc 18.7 19.5 18.5 29.2 18.7 <3.0 <26 25.2 21.5 23.4 6.6 21.5

phenanthrene 133 114 121 118 DL 116 92.8 126 108 119 134 56.6 18.7 30.3 145 148 120 24 119

anthracene 28.2 12.8 < 40 24.2 DL 6.10 67.7 11.4 16.1 <6.21 DL 8.75 13.7 <26 8.29 12.7 12.6 5.7 12.1

fluoranthene 127 238 200 221 DL 215 114 227 242 231 215 176 24.0 52.7 277 262 217 50 218

pyrene 179 117 154 150 DL 182 73.0 158 134 111 154 75.8 17.3 35.0 194 175 146 38 149

benzo[b]fluorene NA NA NA NA NA NA <conc 37.0 <15.4 22.4 DL <39.8 NA NA NA 12.2 20.9 9.7 17.3

benz[a]anthracene 63.6 33.7 27.4 28.9 DL 50.3 <conc 28.3 34.2 33.8 37.2 24.0 5.20 <26 55.9 34.8 36.6 12.1 34.0

chrysene 88.7 58.7 other Other 29.2 85.7 43.8 Other coelute 83.3 coelute 56.0 15.3 26.0 71.2 coelute No Target 65.2

triphenylene NA NA other Other NA NA NA Other NA NA coelute NA NA NA NA NA No Target 60.4

chrysene/triphenylene 84.4 69.6 79.3 91.6 107 102 103 25 105

benzo[b ]fluoranthene 36.0 55.5 25.0 37.6 48.3 20.8 <conc 37.5 42.1 22.4 28.1 21.8 <3.0 coelute 57.2 30.5 32.4 10.5 30.9

benzo[j ]fluoranthene NA NA other NA NA NA NA Other coelute NA coelute NA NA coelute NA NA No Target 22.6

benzo[k ]fluoranthene 65.8 14.3 other 12.5 DL 7.83 <conc Other NA 30.1 coelute 14.2 3.20 coelute 19.3 coelute 15.8 6.2 14.7

benzo[b+j ]fluoranthene No Target

benzo[j+k ]fluoranthene 24.7 9.97 14.7 32.8 33.9 28.4 7.5 32.2

benzo[b+j+k ]fluoranthene <26 No Target

benzo[a]fluoranthene NA NA NA NA NA NA NA 3.99 <2.94 NA DL NA NA NA NA 1.96 3.17 1.88 2.97

benzo[e]pyrene 68.6 NA 37.5 36.9 NA NA <conc 37.4 40.8 NA 43.1 <39.8 4.00 <26 NA 42.3 38.6 5.9 39.4

benzo[a]pyrene 29.5 12.9 10.6 10.4 23.3 7.05 <conc 12.7 8.42 11.4 16.5 6.36 26.0 <26 12.3 15.2 12.3 5.3 11.4

perylene 172 NA 4.57 9.40 NA NA <conc <10 <7.65 NA 6.50 <39.8 12.1 <26 NA 5.22 5.38 1.64 5.68

indeno[1,2,3-cd]pyrene 5.12 13.4 6.61 6.44 14.2 DL <conc 7.07 <4.58 10.5 DL 6.36 <3.0 <26 16.8 7.24 8.05 4.00 7.45

benzo[ghi]perylene < 7.4 11.0 8.75 7.73 NA DL <conc 8.68 7.29 NA 10.5 6.36 <3.0 <26 NA 10.7 8.92 2.25 8.75

dibenz[a,h]anthracene < 7.4 5.09 other 1.77 DL DL <conc 7.83 <3.28 <4.81 DL <39.8 <3.0 <26 3.23 coelute 3.00 2.07 2.54

dibenz[a,h+a,c]anthracene 1.92 3.63 2.63 0.89 2.35

cis/trans-decalin NA NA NA NA NA NA NA 91.9 53.9 NA DL <39.8 NA 38.3 NA 113 No Target 77.6

dibenzofuran < 7.4 NA NA NA NA NA <conc 15.8 17.1 NA DL <39.8 <3.0 <26 NA 15.7 17.4 2.6 17.7

retene NA NA 30.7 NA NA NA NA 25.4 <9.61 NA DL NA NA <26 NA <2.26 34.4 14.4 30.7

benzothiophene NA NA NA NA NA NA NA <1.3 <5.15 NA DL <39.8 NA <26 NA 1.66 No Target 1.30

dibenzothiophene < 7.4 14.0 14.6 15.8 NA NA <conc 16.7 17.6 NA 18.6 <39.8 <3.0 <26 NA 18.4 15.7 3.0 15.8

naphthobenzothiophene NA NA NA NA NA NA NA 12.7 20.4 NA NA NA NA <26 NA 18.0 14.0 4.6 13.1

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus statistics (Lab 31 reported values on a wet mass basis)
19

Table 2. Mussel Tissue (QA10TIS01): Laboratory means of three replicates and exercise assigned values - Alkylated PAHs (ng/g dry mass)

 (reported as if three figures were significant)

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19

1-methylnaphthalene 27.2 <294 15.0 21.0 NA 113 50.3 NA <5700 27.4 23.0 50.5 29.8 37.7 40.1 <6.4 19.9 <78

2-methylnaphthalene 36.2 226 23.7 37.1 NA 64.4 31.5 NA <5700 43.8 38.0 90.3 47.6 67.7 60.2 653 31.8 <78

2,6-dimethylnaphthalene 67.0 102 42.3 68.8 NA NA 70.5 NA NA 46.9 65.4 101 41.5 NA 90.2 1062 46.5 <78

1,6,7-trimethylnaphthalene 46.5 112 46.3 39.4 NA NA NA NA NA NA 50.5 74.3 NA NA 76.8 325 41.4 <78

1-methylphenanthrene 54.6 <294 23.7 81.1 NA NA 61.1 NA NA 56.4 70.9 Other 77.1 NA 67.5 2465 64.8 <78

C1-decalins NA NA 390 NA NA NA NA NA NA NA NA NA NA NA 831 2467 NA NA

C2-decalins NA NA 1333 NA NA NA NA NA NA NA NA NA NA NA 2137 14233 NA NA

C3-decalins NA NA 1900 NA NA NA NA NA NA NA NA NA NA NA 1727 21200 NA NA

C4-decalins NA NA 2533 NA NA NA NA NA NA NA NA NA NA NA 2707 24533 NA NA

C1-naphthalenes 63.4 596 23.7 58.2 NA NA NA NA <5700 NA 35.5 NA NA NA 64.7 862 NA <78

C2-naphthalenes 255 378 78.3 236 NA NA NA NA <5700 NA 125 NA NA 313 194 2728 NA 123

C3-naphthalenes 629 391 153 606 NA NA NA NA 207 NA 253 NA NA 419 406 4270 NA 200

C4-naphthalenes 498 594 170 600 NA NA NA NA 110 NA 210 NA NA 466 362 5307 NA 227

C1-benzothiophenes NA NA 0.00 NA NA NA NA NA NA NA NA NA NA NA 16.9 <3.2 NA NA

C2-benzothiophenes NA NA 0.00 NA NA NA NA NA NA NA NA NA NA NA 34.6 <3.2 NA NA

C3-benzothiophenes NA NA 0.00 NA NA NA NA NA NA NA NA NA NA NA 55.8 <3.2 NA NA

C4-benzothiophenes NA NA 0.00 NA NA NA NA NA NA NA NA NA NA NA 41.6 <3.2 NA NA

C1-fluorenes 76.8 <294 34.0 68.6 NA NA NA NA <5700 NA 37.7 NA NA 75.7 72.4 856 NA <78

C2-fluorenes 181 <294 107 186 NA NA NA NA <5700 NA 109 NA NA 188 209 2563 NA 147

C3-fluorenes 296 <294 473 262 NA NA NA NA <5700 NA 173 NA NA 436 300 <3.2 NA 217

C1-phenanthrenes/anthracenes 280 <294 163 425 NA NA NA NA <5700 NA 226 NA NA 415 321 <3.2 NA 190

C2-phenanthrenes/anthracenes 521 662 263 626 NA NA NA NA 102 NA 326 NA NA 689 510 2353 NA 307

C3-phenanthrenes/anthracenes 467 <294 323 508 NA NA NA NA <5700 NA 232 NA NA 1044 361 3257 NA 263

C4-phenanthrenes/anthracenes 145 <294 230 209 NA NA NA NA <5700 NA 113 NA NA 597 130 1380 NA 117

C1-dibenzothiophenes 95.9 <294 55.3 92.1 NA NA NA NA <5700 NA 72.3 NA NA 64.7 99.4 385 NA <78

C2-dibenzothiophenes 237 <294 140 245 NA NA NA NA <5700 NA 193 NA NA 192 269 946 NA 107

C3-dibenzothiophenes 223 <294 143 206 NA NA NA NA <5700 NA 163 NA NA 155 256 1113 NA 110

C4-dibenzothiophenes 110 <294 87.0 103 NA NA NA NA <5700 NA 68.7 NA NA <40 110 877 NA <78

C1-fluoranthenes/pyrenes 145 <294 70.0 114 NA NA NA NA <5700 NA 91.9 NA NA 66.7 134 717 NA 99

C2-fluoranthenes/pyrenes 62.3 166 42.7 68.3 NA NA NA NA <5700 NA 55.3 NA NA 43.0 67.1 <3.2 NA <78

C3-fluoranthenes/pyrenes 33.4 <294 31.7 37.1 NA NA NA NA <5700 NA 24.3 NA NA <40 40.2 <3.2 NA <78

C4-fluoranthenes/pyrenes <15 NA 12.6 12.2 NA NA NA NA NA NA NA NA NA NA NA <3.2 NA NA

C1-naphthobenzothiophenes NA NA 55.7 20.4 NA NA NA NA NA NA NA NA NA NA 12.2 <3.2 NA NA

C2-naphthobenzothiophenes NA NA 0.00 13.8 NA NA NA NA NA NA NA NA NA NA 8.7 <3.2 NA NA

C3-naphthobenzothiophenes NA NA 0.00 6.97 NA NA NA NA NA NA NA NA NA NA 7.59 <3.2 NA NA

C4-naphthobenzothiophenes NA NA 0.00 3.10 NA NA NA NA NA NA NA NA NA NA 0.00 <3.2 NA NA

C1-chrysenes 42.6 <294 25.7 56.9 NA NA NA NA <5700 NA 28.9 NA NA NA 44.4 308 NA <78

C2-chrysenes 25.7 <294 21.3 31.2 NA NA NA NA <5700 NA 16.2 NA NA NA 32.2 <3.2 NA <78

C3-chrysenes <10 <294 9.93 13.5 NA NA NA NA <5700 NA 6.20 NA NA NA 0.00 <3.2 NA <78

C4-chrysenes <10 <294 0.00 <1.79 NA NA NA NA NA NA <40 NA NA NA 0.00 <3.2 NA <78

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus statistics
20

Table 2 (cont). Mussel Tissue (QA10TIS01): Laboratory means of three replicates and exercise assigned valuess - Alkylated PAHs (ng/g dry mass) Consensus Values 

 (reported as if three figures were significant) (ng/g dry mass)

Laboratory No. 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34 mean std dev median

1-methylnaphthalene 37.6 25.6 24.8 30.4 58.3 NA <conc 29.7 <24.3 38.3 31.2 16.1 7.90 <52 47.6 34.2 31.7 11.1 30.1

2-methylnaphthalene 34.4 42.3 40.8 45.1 94.0 NA <conc 41.4 <24.3 24.0 52.5 70.5 6.90 <52 30.0 52.2 43.6 15.3 43.1

2,6-dimethylnaphthalene 106 41.6 76.2 53.7 118 NA 104 78.8 48.4 69.7 DL 27.1 13.2 <52 87.5 73.3 70.7 24.9 69.7

1,6,7-trimethylnaphthalene 168 NA NA 41.7 NA NA <conc 81.4 30.6 NA 46.0 NA 17.7 <52 NA 35.6 63.6 37.6 46.4

1-methylphenanthrene < 7.4 57.3 57.3 59.2 DL NA <conc 43.7 35.1 <8.65 83.8 NA <3.0 <52 0.00 42.3 58.5 16.4 58.3

C1-decalins NA NA NA NA NA NA <conc 560 30.6 NA DL NA NA <52 NA 547 582 183 554

C2-decalins NA NA NA NA NA NA <conc 1733 45.6 NA DL NA NA <52 NA 1353 1639 379 1543

C3-decalins NA NA NA NA NA NA <conc 2967 310 NA DL NA NA <52 NA 1127 1930 766 1813

C4-decalins NA NA NA NA NA NA <conc 3533 506 NA DL NA NA <52 NA 1493 2567 838 2620

C1-naphthalenes 47.2 63.4 65.5 75.4 NA NA <conc 48.3 <24.3 62.3 90.0 NA 13.0 <52 77.5 55.3 59.3 17.0 63.4

C2-naphthalenes 212 277 298 173 508 NA <conc 180 102 263 229 NA 26.0 <52 321 138 232 106 229

C3-naphthalenes 314 390 615 306 497 NA <conc 290 226 498 695 NA 27.0 54.3 435 235 386 165 390

C4-naphthalenes 319 240 554 326 683 NA <conc 400 279 138 Other NA 18.3 76.0 313 247 552 173 316

C1-benzothiophenes NA NA NA NA NA NA <conc <39 21.1 NA DL NA NA <52 NA 14.4 17.5 3.4 15.7

C2-benzothiophenes NA NA NA NA NA NA <conc <39 12.4 NA DL NA NA <52 NA 19.5 22.2 11.3 15.9

C3-benzothiophenes NA NA NA NA NA NA <conc <39 20.4 NA DL NA NA <52 NA 49.4 41.8 18.9 34.9

C4-benzothiophenes NA NA NA NA NA NA <conc 54.0 37.8 NA DL NA NA NA NA 50.2 45.9 7.5 41.6

C1-fluorenes < 7.4 84.9 140 68.6 98.7 NA <conc 68.3 70.1 21.5 446 NA <3.0 <52 103 51.8 71.4 29.3 72.4

C2-fluorenes < 7.4 195 312 146 193 NA <conc 373 190 181 658 NA <3.0 60.0 77.2 150 177 77 186

C3-fluorenes < 7.4 48.4 530 242 DL NA <conc 780 354 <6.89 558 NA <3.0 67.0 277 228 328 190 287

C1-phenanthrenes/anthracenes < 7.4 312 328 258 685 NA <conc 187 230 360 554 NA <3.0 59.3 433 257 331 138 296

C2-phenanthrenes/anthracenes < 7.4 113 546 378 1457 NA 106 493 393 536 934 NA <3.0 93.3 639 398 434 219 502

C3-phenanthrenes/anthracenes < 7.4 155 547 294 469 NA <conc 460 307 356 837 NA <3.0 77.0 482 240 457 224 361

C4-phenanthrenes/anthracenes < 7.4 NA 590 141 5.48 NA <conc 260 159 <9.48 426 NA <3.0 <52 237 92.5 246 170 184

C1-dibenzothiophenes 46.2 NA 103 85.1 NA NA <conc 82.7 71.6 NA 188 NA <3.0 <52 NA 71.4 86.8 35.0 83.9

C2-dibenzothiophenes < 7.4 NA 355 215 NA NA <conc 287 226 NA 651 NA <3.0 54.0 NA 201 211 134 226

C3-dibenzothiophenes 61.7 NA 321 190 NA NA <conc 303 234 NA 705 NA <3.0 <52 NA 186 196 73 206

C4-dibenzothiophenes 55.6 NA 132 NA NA NA <conc 263 108 NA 433 NA <3.0 NA NA 95.4 113 57 109

C1-fluoranthenes/pyrenes 373 338 376 123 NA NA <conc 127 115 NA 112 NA <3.0 <52 NA 107 159 107 119

C2-fluoranthenes/pyrenes < 7.4 91.6 291 59.1 NA NA <conc 92.7 71.7 NA 84.2 NA <3.0 <52 NA 59.3 74.1 31.8 67.7

C3-fluoranthenes/pyrenes 57.9 NA 99.1 27.0 NA NA <conc 52.3 36.2 NA 40.9 NA <3.0 <52 NA 30.2 42.5 20.3 36.7

C4-fluoranthenes/pyrenes NA NA 22.4 NA NA NA <conc <39 16.9 NA 18.5 NA <3.0 NA NA 15.2 16.3 3.9 16.0

C1-naphthobenzothiophenes NA NA NA NA NA NA <conc <39 19.1 NA NA NA <3.0 <52 NA 18.9 25.2 17.3 19.1

C2-naphthobenzothiophenes NA NA NA NA NA NA <conc <39 16.0 NA NA NA <3.0 <52 NA 15.9 13.6 3.4 13.8

C3-naphthobenzothiophenes NA NA NA NA NA NA <conc <39 <8.19 NA NA NA <3.0 <52 NA 9.75 8.11 1.46 7.28

C4-naphthobenzothiophenes NA NA NA NA NA NA <conc <39 <8.19 NA NA NA <3.0 NA NA <0.707 No Target

C1-chrysenes 35.5 NA 60.9 44.7 NA NA <conc 43.5 41.6 NA 43.9 NA <3.0 <52 NA 38.7 42.3 9.9 43.5

C2-chrysenes 210 NA 30.6 19.5 NA NA <conc 43.0 22.4 NA 21.8 NA <3.0 <52 NA 23.9 26.2 7.6 24.8

C3-chrysenes < 7.4 NA 6.74 6.84 NA NA <conc <39 <13.8 NA 12.3 NA <3.0 <52 NA <0.595 9.25 3.14 6.84

C4-chrysenes < 7.4 NA 0.540 2.93 NA NA <conc <39 <13.8 NA 7.81 NA <3.0 <52 NA <0.595 No Target 0.540

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus statistics (Lab 31 reported values on a wet mass basis)
21

Table 3. Mussel Tissue (QA10TIS01): Laboratory means of three replicates and exercise assigned valuess - Biomarkers (ng/g dry mass)

 (reported as if three figures were significant)

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19

Carbazole NA NA NA NA NA NA NA NA NA <40 NA NA Other NA 223 NA NA

18a(H)-22,29,30-Trisnorhopane NA <294 NA NA NA NA NA <5700 NA <40 NA NA Other 15.3 NA NA <78

17a(H)-22,29,30-Trisnorhopane <25 <294 NA NA NA NA NA <5700 NA <40 NA coelution Other 15.7 NA NA <78

17α(H),21β(H)-30-Norhopane <25 <294 NA NA NA NA NA <5700 NA <40 NA 20.3 Other 0.00 NA NA <78

18a(H)-30-Norneohopane NA <294 NA NA NA NA NA <5700 NA <40 NA NA Other 48.2 NA NA <78

17a(H)-Diahopane NA <294 NA NA NA NA NA <5700 NA <40 NA NA Other 0.00 NA NA <78

17α(H),21β(H)-Hopane 65.7 <294 NA NA NA NA NA <5700 NA <40 NA 65.3 Other 59.8 558 NA <78

17α(H),21β(H)-22R-Homohopane <20 <294 NA NA NA NA NA <5700 NA <40 NA 12.4 Other 18.4 NA NA <78

17α(H),21β(H)-22S-Homohopane 23.1 <294 NA NA NA NA NA <5700 NA <40 NA 20.8 Other 25.0 NA NA <78

13b(H)17a(H)-Diacholestane 20S NA <294 NA NA NA NA NA <5700 NA <40 NA NA Other 18.2 NA NA <78

5a(H),14a(H),17a(H)-Cholestane 20S NA <294 NA NA NA NA NA NA NA <40 NA NA Other 26.8 NA NA <78

5a(H),14a(H),17a(H)-Cholestane 20R 38.2 <294 NA NA NA NA NA <5700 NA <40 NA 36.8 Other 47.1 NA NA <78

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S NA <294 NA NA NA NA NA <5700 NA <40 NA 16.8 Other 12.4 NA NA <78

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R 29.0 <294 NA NA NA NA NA <5700 NA <40 NA NA Other 31.0 NA NA <78

5a(H),14b(H),17b(H)-Cholestane 20R <20 <294 NA NA NA NA NA <5700 NA <40 NA 20.0 Other 17.1 NA NA <78

5a(H),14b(H),17b(H)-Cholestane 20S NA <294 NA NA NA NA NA <5700 NA <40 NA NA Other 18.5 NA NA <78

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R <20 <294 NA NA NA NA NA <5700 NA <40 NA 8.75 Other 19.8 NA NA <78

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S NA <294 NA NA NA NA NA <5700 NA <40 NA NA Other 20.0 NA NA <78

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus statistics

Table 3 (cont). Mussel Tissue (QA10TIS01): Laboratory means of three replicates and exercise assigned values - Biomarkers (ng/g dry mass) Consensus Values 

 (reported as if three figures were significant) (ng/g dry mass)

Laboratory No. 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34 mean std dev median

Carbazole NA NA < 10 NA NA NA <conc <1.7 NA NA NA NA NA NA NA 6.85 No Target 115

18a(H)-22,29,30-Trisnorhopane 131 NA NA NA NA NA <conc NA NA NA NA NA <3.0 NA NA 19.8 No Target 19.8

17a(H)-22,29,30-Trisnorhopane 79.6 NA 23.2 NA NA NA <conc NA NA NA NA NA <3.0 NA NA 20.8 No Target 22.0

17α(H),21β(H)-30-Norhopane < 7.4 NA 60.2 NA NA NA <conc NA NA NA NA NA 112 NA NA 51.2 No Target 51.2

18a(H)-30-Norneohopane < 7.4 NA NA NA NA NA <conc NA NA NA NA NA 86.7 NA NA 18.1 No Target 48.2

17a(H)-Diahopane < 7.4 NA NA NA NA NA <conc NA NA NA NA NA <3.0 NA NA 5.48 No Target 2.74

17α(H),21β(H)-Hopane < 7.4 NA 68.8 NA NA NA <conc 81.1 NA NA NA NA <3.0 NA NA 78.9 69.9 8.3 68.8

17α(H),21β(H)-22R-Homohopane < 7.4 NA 23.8 NA NA NA <conc NA NA NA NA NA <3.0 NA NA 20.5 18.8 4.8 19.4

17α(H),21β(H)-22S-Homohopane < 7.4 NA 29.4 NA NA NA <conc NA NA NA NA NA <3.0 NA NA 24.4 24.5 3.2 24.4

13b(H)17a(H)-Diacholestane 20S 50.6 NA NA NA NA NA <conc NA NA NA NA NA <3.0 NA NA 17.7 No Target 18.2

5a(H),14a(H),17a(H)-Cholestane 20S < 7.4 NA NA NA NA NA <conc NA NA NA NA NA <3.0 NA NA 29.1 No Target 28.0

5a(H),14a(H),17a(H)-Cholestane 20R < 7.4 NA 36.4 NA NA NA <conc NA NA NA NA NA <3.0 NA NA 52.4 42.2 7.2 38.2

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S 21.0 NA NA NA NA NA <conc NA NA NA NA NA <3.0 NA NA 11.3 15.4 4.4 14.6

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R 66.2 NA 27.6 NA NA NA <conc NA NA NA NA NA 24.7 NA NA 32.4 37.2 16.3 30.0

5a(H),14b(H),17b(H)-Cholestane 20R < 7.4 NA < 30 NA NA NA <conc NA NA NA NA NA 67.3 NA NA 17.7 18.3 1.5 18.8

5a(H),14b(H),17b(H)-Cholestane 20S < 7.4 NA NA NA NA NA <conc NA NA NA NA NA 59.7 NA NA 18.8 No Target 18.8

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R < 7.4 NA 13.0 NA NA NA <conc NA NA NA NA NA <3.0 NA NA 23.7 16.3 6.7 16.4

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S < 7.4 NA NA NA NA NA <conc NA NA NA NA NA <3.0 NA NA 18.1 No Target 19.1

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus statistics (Lab 31 reported values on a wet mass basis)
22

Table 4. Mussel Tissue (QA10TIS01): z scores (25% by laboratory)- Water and PAHs 

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

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18

Percent Water -0.1 0.0 0.0 0.0 0.1 0.0 0.0 0.0 0.0 0.0 0.0 0.1 0.0 0.0 0.0 0.1 0.0 0.0

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18

naphthalene 2.3 1.5 -1.1 -2.1 11.3 1.3 0.6 -1.3 -0.4 4.0 47.4 1.1 87.9 0.4

biphenyl -0.7 28.8 0.0 -1.7 1.3 0.6 -0.6 138.8 0.8

acenaphthene 1.7 0.6 -0.1 -1.0 0.0 0.8 -0.1

acenaphthylene 0.1 -2.8 -2.0 -0.4 1.7 0.8 -1.0

fluorene 1.8 -1.6 0.2 0.4 3.5 -0.6 0.3 -1.0 -0.6 -1.5 1.7 1.3 0.3 0.1 34.8 -0.5

phenanthrene -0.1 -2.1 -0.7 -0.8 0.9 1.1 0.6 0.4 0.8 -0.2 -0.1 0.2 -0.2 0.2 1.2 21.1 -0.1

anthracene -0.7 -3.1 0.2 -0.8 -0.2 -0.8 -0.4 -0.8 -0.9 -1.6 1.6 1.0 22.8 1.5

fluoranthene 0.5 -1.9 -0.7 -1.4 1.6 0.5 -0.4 0.4 0.8 -0.6 0.1 0.9 -0.1 -0.2 -0.8 1.3 17.3 1.5

pyrene 1.7 -1.7 -1.0 -1.1 1.8 1.2 -0.7 0.2 1.3 -1.2 -0.2 0.1 0.1 0.3 -0.7 1.1 16.0 -0.2

benzo[b]fluorene -0.7 -1.0

benz[a]anthracene 0.1 -3.0 -1.8 2.3 1.5 -2.2 -0.9 -0.1 -0.5 -0.6 0.2 -1.1 -0.1 17.7 1.8

chrysene

triphenylene

chrysene/triphenylene 1.6 1.4 0.2 12.4

benzo[b ]fluoranthene -0.8 -2.2 -1.4 0.7 -0.3 -1.3 -0.6 -0.2 1.4 -0.9 0.3 -0.2 0.3 28.2 0.0

benzo[j]fluoranthene

benzo[k ]fluoranthene 0.0 -3.1 -0.6 0.4 1.3 -0.9 0.4 2.7 2.5 -0.2 0.0 -1.1 -0.1

benzo[b+j ]fluoranthene

benzo[j+k ]fluoranthene 0.6 0.5 23.3

benzo[b+j+k ]fluoranthene

benzo[a]fluoranthene -2.3 2.8

benzo[e]pyrene 0.0 -1.5 1.1 -0.2 0.1 -1.0 0.1 -0.3 0.8 20.0 0.1

benzo[a]pyrene -0.5 -2.8 -1.7 -0.3 0.6 -1.2 1.7 -0.4 -1.6 -0.4 -0.6 -0.7 -0.6 1.2

perylene -0.6 125.4 -2.0 -0.1 -1.3 0.0 -0.8 0.4 -1.2

indeno[1,2,3-cd]pyrene -1.6 6.6 0.2 -1.1 0.7 -1.8 -1.7 0.1 -0.2 98.9 -0.2

benzo[ghi]perylene -0.5 -1.0 0.8 -2.3 -0.4 -0.5 1.3 0.4 0.4 87.4 1.9

dibenz[a,h]anthracene -2.5 20.2 -1.0 -1.2 -0.6 229.2 0.2

dibenz[a,h+a,c]anthracene -0.4

cis/trans-decalin

dibenzofuran 0.9 -0.8 0.5 0.2 28.9

retene 0.9 -2.6 1.8 -0.7 -0.5 2.5 24.5

benzothiophene

dibenzothiophene -0.8 1.3 0.1 -0.7 -0.6 -0.9 1.2 -1.0

naphthobenzothiophene -0.7 -0.1 -1.9
23

Table 4 (cont). Mussel Tissue (QA10TIS01): z scores (25% by laboratory)- Water and PAHs 

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

Laboratory No. 19 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34

Percent Water 0.0 0.0 -0.1 0.0 -0.1 -0.1 -0.1 0.0 0.0 -0.1 0.0 0.0 -0.1 0.1 0.0 0.0

Laboratory No. 19 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34

naphthalene 1.4 -0.6 -0.4 -0.1 2.9 13.2 -0.4 -1.8 0.6 -1.8 -3.2 -0.7 0.2

biphenyl 4.5 -1.2 0.0 -0.1 -0.8 -2.3 -1.0

acenaphthene -1.2 0.3 -0.2 0.6 -1.0 -1.2 0.8 0.3

acenaphthylene 2.2 -2.0 -0.5 3.2 0.5 1.6 -1.2 -0.5

fluorene 0.0 -0.5 -0.8 -0.4 -0.8 -0.7 -0.8 1.0 -0.8 0.3 -0.3

phenanthrene -0.7 0.4 -0.2 0.0 -0.1 -0.1 -0.9 0.2 -0.4 0.0 0.5 -2.1 -3.4 -3.0 0.8 0.9

anthracene 5.0 0.1 3.7 -2.1 17.5 -0.4 1.1 -1.2 0.3 -1.4 0.0

fluoranthene -0.2 -1.7 0.4 -0.3 0.1 0.0 -1.9 0.2 0.4 0.3 0.0 -0.8 -3.6 -3.0 1.1 0.8

pyrene -0.3 0.9 -0.8 0.2 0.1 1.0 -2.0 0.3 -0.3 -1.0 0.2 -1.9 -3.5 -3.0 1.3 0.8

benzo[b]fluorene 3.1 0.3 -1.7

benz[a]anthracene 3.0 -0.3 -1.0 -0.8 1.5 -0.9 -0.3 -0.3 0.1 -1.4 -3.4 2.1 -0.2

chrysene

triphenylene

chrysene/triphenylene -0.7 -1.3 -0.9 -0.4 0.2 0.0

benzo[b ]fluoranthene 0.4 2.9 -0.9 0.6 2.0 -1.4 0.6 1.2 -1.2 -0.5 -1.3 3.1 -0.2

benzo[j ]fluoranthene

benzo[k ]fluoranthene 12.6 -0.4 -0.8 -2.0 3.6 -0.4 -3.2 0.9

benzo[b+j ]fluoranthene

benzo[j+k ]fluoranthene -0.5 -2.6 -1.9 0.6 0.8

benzo[b+j+k ]fluoranthene

benzo[a]fluoranthene 1.0 -1.5

benzo[e]pyrene 3.1 -0.1 -0.2 -0.1 0.2 0.5 -3.6 0.4

benzo[a]pyrene 5.6 0.2 -0.6 -0.6 3.6 -1.7 0.1 -1.3 -0.3 1.3 -1.9 4.4 0.0 0.9

perylene 123.8 -0.6 3.0 0.8 5.0 -0.1

indeno[1,2,3-cd]pyrene -1.5 2.6 -0.7 -0.8 3.0 -0.5 1.2 -0.8 4.4 -0.4

benzo[ghi]perylene 0.9 -0.1 -0.5 -0.1 -0.7 0.7 -1.1 0.8

dibenz[a,h]anthracene 2.8 -1.6 6.4 0.3

dibenz[a,h+a,c]anthracene -1.1 1.5

cis/trans-decalin

dibenzofuran -0.4 -0.1 -0.4

retene -0.4 -1.0

benzothiophene

dibenzothiophene -0.4 -0.3 0.0 0.2 0.5 0.7 0.7

naphthobenzothiophene -0.4 1.8 1.2

Lab 31 reported values on a wet mass basis
24

Table 5. Mussel Tissue (QA10TIS01): z scores (25% by laboratory)- Alkylated PAHs 

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

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18

1-methylnaphthalene -0.6 -2.1 -1.3 10.2 2.4 -0.5 -1.1 2.4 -0.2 0.8 1.1 -1.5

2-methylnaphthalene -0.7 16.7 -1.8 -0.6 1.9 -1.1 0.0 -0.5 4.3 0.4 2.2 1.5 55.9 -1.1

2,6-dimethylnaphthalene -0.2 1.8 -1.6 -0.1 0.0 -1.3 -0.3 1.7 -1.7 1.1 56.1 -1.4

1,6,7-trimethylnaphthalene -1.1 3.0 -1.1 -1.5 -0.8 0.7 0.8 16.4 -1.4

1-methylphenanthrene -0.3 -2.4 1.5 0.2 -0.1 0.8 1.3 0.6 164.6 0.4

C1-decalins -1.3 1.7 13.0

C2-decalins -0.7 1.2 30.7

C3-decalins -0.1 -0.4 39.9

C4-decalins -0.1 0.2 34.2

C1-naphthalenes 0.3 36.2 -2.4 -0.1 -1.6 0.4 54.2

C2-naphthalenes 0.4 2.5 -2.6 0.1 -1.8 1.4 -0.7 43.1

C3-naphthalenes 2.5 0.1 -2.4 2.3 -1.9 -1.4 0.3 0.2 40.3

C4-naphthalenes -0.4 0.3 -2.8 0.3 -3.2 -2.5 -0.6 -1.4 34.5

C1-benzothiophenes -0.1

C2-benzothiophenes 2.2

C3-benzothiophenes 1.3

C4-benzothiophenes -0.4

C1-fluorenes 0.3 -2.1 -0.2 -1.9 0.2 0.1 44.0

C2-fluorenes 0.1 -1.6 0.2 -1.5 0.3 0.7 54.0

C3-fluorenes -0.4 1.8 -0.8 -1.9 1.3 -0.3

C1-phenanthrenes/anthracenes -0.6 -2.0 1.1 -1.3 1.0 -0.1

C2-phenanthrenes/anthracenes 0.8 2.1 -1.6 1.8 -3.1 -1.0 2.4 0.7 17.7

C3-phenanthrenes/anthracenes 0.1 -1.2 0.4 -2.0 5.1 -0.8 24.5

C4-phenanthrenes/anthracenes -1.6 -0.3 -0.6 -2.2 5.7 -1.9 18.4

C1-dibenzothiophenes 0.4 -1.4 0.2 -0.7 -1.0 0.6 13.7

C2-dibenzothiophenes 0.5 -1.3 0.6 -0.3 -0.4 1.1 13.9

C3-dibenzothiophenes 0.5 -1.1 0.2 -0.7 -0.8 1.2 18.7

C4-dibenzothiophenes -0.1 -0.9 -0.4 -1.6 -0.1 26.9

C1-fluoranthenes/pyrenes -0.4 -2.2 -1.1 -1.7 -2.3 -0.6 14.0

C2-fluoranthenes/pyrenes -0.6 5.0 -1.7 -0.3 -1.0 -1.7 -0.4

C3-fluoranthenes/pyrenes -0.9 -1.0 -0.5 -1.7 -0.2

C4-fluoranthenes/pyrenes -0.9 -1.0

C1-naphthobenzothiophenes 4.8 -0.8 -2.1

C2-naphthobenzothiophenes 0.1 -1.4

C3-naphthobenzothiophenes -0.6 -0.3

C4-naphthobenzothiophenes

C1-chrysenes 0.0 -1.6 1.4 -1.3 0.2 25.2

C2-chrysenes -0.1 -0.7 0.8 -1.5 0.9

C3-chrysenes 0.3 1.8 -1.3

C4-chrysenes
25

Table 5 (cont). Mussel Tissue (QA10TIS01): z scores (25% by laboratory)- Alkylated PAHs 

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

Laboratory No. 19 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34

1-methylnaphthalene 0.7 -0.8 -0.9 -0.2 3.4 -0.2 0.8 -0.1 -2.0 -3.0 2.0 0.3

2-methylnaphthalene -0.8 -0.1 -0.3 0.1 4.6 -0.2 -1.8 0.8 2.5 -3.4 -1.2 0.8

2,6-dimethylnaphthalene 2.0 -1.6 0.3 -1.0 2.7 1.9 0.5 -1.3 -0.1 -2.5 -3.3 0.9 0.1

1,6,7-trimethylnaphthalene 6.6 -1.4 1.1 -2.1 -1.1 -2.9 -1.8

1-methylphenanthrene -0.1 -0.1 0.0 -1.0 -1.6 1.7 -1.1

C1-decalins -0.2 -3.8 -0.2

C2-decalins 0.2 -3.9 -0.7

C3-decalins 2.1 -3.4 -1.7

C4-decalins 1.5 -3.2 -1.7

C1-naphthalenes -0.8 0.3 0.4 1.1 -0.7 0.2 2.1 -3.1 1.2 -0.3

C2-naphthalenes -1.9 -0.3 0.8 1.2 -1.0 4.8 -0.9 -2.2 0.5 0.0 -3.6 1.5 -1.6

C3-naphthalenes -1.9 -0.7 0.0 2.4 -0.8 1.2 -1.0 -1.7 1.2 3.2 -3.7 -3.4 0.5 -1.6

C4-naphthalenes -2.4 -1.7 -2.3 0.0 -1.6 1.0 -1.1 -2.0 -3.0 -3.9 -3.4 -1.7 -2.2

C1-benzothiophenes 0.8 -0.7

C2-benzothiophenes -1.8 -0.5

C3-benzothiophenes -2.1 0.7

C4-benzothiophenes 0.7 -0.7 0.4

C1-fluorenes 0.8 3.8 -0.2 1.5 -0.2 -0.1 -2.8 21.0 1.8 -1.1

C2-fluorenes -0.7 0.4 3.1 -0.7 0.4 4.5 0.3 0.1 10.9 -2.6 -2.3 -0.6

C3-fluorenes -1.4 -3.4 2.5 -1.0 5.5 0.3 2.8 -3.2 -0.6 -1.2

C1-phenanthrenes/anthracenes -1.7 -0.2 0.0 -0.9 4.3 -1.7 -1.2 0.4 2.7 -3.3 1.2 -0.9

C2-phenanthrenes/anthracenes -1.2 -3.0 1.0 -0.5 9.4 -3.0 0.5 -0.4 0.9 4.6 -3.1 1.9 -0.3

C3-phenanthrenes/anthracenes -1.7 -2.6 0.8 -1.4 0.1 0.0 -1.3 -0.9 3.3 -3.3 0.2 -1.9

C4-phenanthrenes/anthracenes -2.1 5.6 -1.7 -3.9 0.2 -1.4 2.9 -0.2 -2.5

C1-dibenzothiophenes -1.9 0.8 -0.1 -0.2 -0.7 4.7 -0.7

C2-dibenzothiophenes -2.0 2.7 0.1 1.4 0.3 8.3 -3.0 -0.2

C3-dibenzothiophenes -1.8 -2.7 2.5 -0.1 2.2 0.8 10.4 -0.2

C4-dibenzothiophenes -2.0 0.7 5.3 -0.2 11.3 -0.6

C1-fluoranthenes/pyrenes -1.5 5.4 4.5 5.4 -0.9 -0.8 -1.1 -1.2 -1.3

C2-fluoranthenes/pyrenes 0.9 11.7 -0.8 1.0 -0.1 0.5 -0.8

C3-fluoranthenes/pyrenes 1.4 5.3 -1.5 0.9 -0.6 -0.2 -1.2

C4-fluoranthenes/pyrenes 1.5 0.1 0.5 -0.3

C1-naphthobenzothiophenes -1.0 -1.0

C2-naphthobenzothiophenes 0.7 0.7

C3-naphthobenzothiophenes 0.8

C4-naphthobenzothiophenes

C1-chrysenes -0.6 1.8 0.2 0.1 -0.1 0.2 -0.3

C2-chrysenes 28.0 0.7 -1.0 2.6 -0.6 -0.7 -0.4

C3-chrysenes -1.1 -1.0 1.3

C4-chrysenes

Lab 31 reported values on a wet mass basis
26

Table 6. Mussel Tissue (QA10TIS01): z scores (25% by laboratory)- Biomarkers 

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

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18

Carbazole

18a(H)-22,29,30-Trisnorhopane

17a(H)-22,29,30-Trisnorhopane

17α(H),21β(H)-30-Norhopane

18a(H)-30-Norneohopane

17a(H)-Diahopane

17α(H),21β(H)-Hopane -0.2 -0.3 -0.6 27.9

17α(H),21β(H)-22R-Homohopane -1.4 -0.1

17α(H),21β(H)-22S-Homohopane -0.2 -0.6 0.1

13b(H)17a(H)-Diacholestane 20S

5a(H),14a(H),17a(H)-Cholestane 20S

5a(H),14a(H),17a(H)-Cholestane 20R -0.4 -0.5 0.5

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S 0.4 -0.8

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R -0.7 -0.5

5a(H),14b(H),17b(H)-Cholestane 20R -1.4 -1.8

5a(H),14b(H),17b(H)-Cholestane 20S

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R -1.9 0.9

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S

Table 6 (cont). Mussel Tissue (QA10TIS01): z scores (25% by laboratory)- Biomarkers 

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

Laboratory No. 19 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34

Carbazole

18a(H)-22,29,30-Trisnorhopane

17a(H)-22,29,30-Trisnorhopane

17α(H),21β(H)-30-Norhopane

18a(H)-30-Norneohopane

17a(H)-Diahopane

17α(H),21β(H)-Hopane -0.1 0.6 0.5

17α(H),21β(H)-22R-Homohopane 1.1 0.4

17α(H),21β(H)-22S-Homohopane 0.8 0.0

13b(H)17a(H)-Diacholestane 20S

5a(H),14a(H),17a(H)-Cholestane 20S

5a(H),14a(H),17a(H)-Cholestane 20R -0.6 1.0

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S 1.5 -1.1

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R 3.1 -1.0 -1.3 -0.5

5a(H),14b(H),17b(H)-Cholestane 20R 10.8 -0.1

5a(H),14b(H),17b(H)-Cholestane 20S

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R -0.8 1.8

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S

Lab 31 reported values on a wet mass basis
27

Table 7. Mussel Tissue (QA10TIS01): Laboratory relative standard deviations of three replicates - Water and PAHs 

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17

Percent Water 0.1% 0.4% 0.0% 0.2% 0.2% 0.4% 0.4% 0.3% 0.6% 1.2% n=1 1.4% 0.1% 0.4% 2.5% 0.6% 0.7%

naphthalene 7.2% 36.5% 21.2% 4.3% 2.9% 16.7% 16.7% 26.7% 22.4% 11.2% 5.5% 29.8% 13.4% 24.5%

biphenyl 7.8% 65.6% 16.5% 7.2% 9.0% 2.4% 13.7% 14.8% 31.7%

acenaphthene 4.2% 10.2% 9.8% 8.4% 6.4% 12.0%

acenaphthylene 15.7% 23.3% 2.0% 4.1% 4.6% 11.2%

fluorene 6.1% 18.6% 12.6% 1.4% 8.1% 4.2% 5.4% 9.6% 7.4% 9.8% 4.6% 4.6% 6.0% 15.2% 20.5%

phenanthrene 2.7% 1.3% 24.1% 15.2% 2.1% 4.7% 5.0% 3.8% 12.7% 4.4% 11.9% 3.6% 4.4% 12.2% 11.9% 9.3%

anthracene 4.0% 78.2% 22.1% 3.2% 3.4% 31.3% 3.9% 11.9% 24.4% 3.8% 3.3% 13.6% 6.3%

fluoranthene 2.2% 9.2% 19.5% 14.3% 2.6% 3.7% 3.8% 3.4% 16.5% 3.1% 5.6% 11.4% 2.2% 16.4% 11.2% 7.8%

pyrene 3.6% 3.6% 7.6% 14.3% 2.6% 3.1% 4.1% 3.2% 25.2% 8.5% 3.3% 12.5% 2.7% 3.2% 13.8% 10.7% 11.4%

benzo[b]fluorene 8.8% 8.4% 4.2%

benz[a]anthracene 7.4% 14.9% 17.9% 3.5% 5.0% 1.1% 4.2% 12.0% 8.0% 8.8% 0.4% 12.1% 8.9% 31.7%

chrysene 7.9% 16.0% 3.3% 3.1% 6.2% 12.2% 2.7% 10.7% 5.6% 3.0% 15.2%

triphenylene 3.6%

benzo[b ]fluoranthene 3.1% 5.0% 14.8% 3.0% 2.4% 4.6% 5.1% 12.0% 4.7% 11.4% 5.8% 3.9% 13.6% 37.4%

benzo[j]fluoranthene 7.7% 3.9%

benzo[k ]fluoranthene 10.0% 5.1% 20.4% 8.3% 3.0% 11.2% 16.7% 16.3% 18.2% 7.5% 5.0% 0.0%

benzo[a]fluoranthene 173.2% 2.8%

benzo[e]pyrene 5.4% 16.6% 3.6% 0.9% 6.3% 9.0% 2.0% 9.3% 12.2% 8.9%

benzo[a]pyrene 10.6% 12.0% 27.9% 1.5% 4.1% 5.5% 36.3% 3.5% 19.8% 14.5% 6.0% 5.4% 14.3%

perylene 6.1% 4.3% 22.4% 3.6% 13.4% 12.8% 1.4% 14.4%

indeno[1,2,3-cd]pyrene 10.6% 7.2% 1.4% 12.3% 4.2% 17.2% 35.2% 9.8%

benzo[ghi]perylene 6.5% 23.4% 2.8% 25.5% 5.9% 10.8% 23.5% 15.7%

dibenz[a,h]anthracene 11.6% 8.4% 11.9% 13.8% 19.7%

cis/trans-decalin 12.9% 3.5% 10.2%

dibenzofuran 16.5% 11.4% 3.4% 11.3% 2.5%

retene 17.1% 3.4% 10.5% 2.6% 10.0% 9.6% 22.3%

benzothiophene 17.8%

dibenzothiophene 12.1% 4.8% 12.1% 5.5% 14.4% 12.2%

naphthobenzothiophene 4.9% 10.5% 13.1%
28

Table 7 (cont). Mussel Tissue (QA10TIS01): Laboratory relative standard deviations of three replicates - Water and PAHs 

Laboratory No. 18 19 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34

Percent Water 0.7% 0.1% 0.2% 0.0% 0.8% 0.6% 1.5% 1.5% 0.0% 0.0% 0.8% 2.1% 0.3% 0.1% 0.7% 0.41% 0.2%

naphthalene 28.9% 9.8% 8.9% 6.2% 2.7% 43.6% 7.4% 14.6% 6.4% 6.4% 10.2% 6.3% 5.8% 5.0%

biphenyl 6.6% 10.9% 4.2% 5.8% 10.3% 5.3% 25.1% 6.0%

acenaphthene 15.1% 2.1% 5.9% 8.0% 13.3% 10.4% 23.6% 17.8% 22.0%

acenaphthylene 29.7% 24.7% 17.5% 11.6% 1.7% 10.5% 4.5% 34.1% 7.3%

fluorene 1.8% 49.1% 3.7% 3.4% 3.2% 4.3% 9.1% 0.0% 2.0% 22.9% 7.0% 12.4%

phenanthrene 9.8% 0.6% 19.3% 7.9% 5.6% 2.9% 7.0% 33.5% 5.2% 7.5% 11.0% 2.0% 17.4% 18.8% 8.3% 1.6% 10.2%

anthracene 6.7% 69.7% 6.8% 4.1% 4.0% 10.6% 4.9% 5.9% 11.2% 3.4% 23.0%

fluoranthene 7.6% 2.8% 17.4% 2.4% 7.1% 3.3% 8.1% 47.7% 5.3% 5.4% 10.9% 2.3% 13.3% 15.0% 9.0% 2.0% 8.0%

pyrene 32.5% 4.3% 25.1% 13.6% 5.8% 3.9% 8.6% 58.0% 3.0% 6.8% 11.6% 2.3% 71.6% 35.3% 7.6% 3.9% 8.6%

benzo[b]fluorene 2.0% 9.7% 7.1%

benz[a]anthracene 30.4% 33.9% 1.0% 5.7% 4.4% 7.7% 6.2% 4.0% 10.2% 3.8% 10.4% 21.8% 3.1% 21.4%

chrysene 7.9% 20.4% 13.8% 18.6% 9.3% 37.1% 11.0% 15.2% 49.4% 6.7%

triphenylene 7.9%

benzo[b ]fluoranthene 11.4% 105.8% 5.9% 5.0% 2.7% 10.2% 20.7% 8.0% 4.2% 9.7% 7.5% 15.3% 5.0% 21.1%

benzo[j ]fluoranthene

benzo[k ]fluoranthene 3.1% 70.0% 8.1% 4.8% 9.1% 13.6% 18.9% 3.6%

benzo[a]fluoranthene 38.8%

benzo[e]pyrene 7.0% 66.2% 2.4% 2.2% 7.9% 5.9% 1.7% 10.9%

benzo[a]pyrene 6.9% 82.4% 11.7% 9.9% 3.9% 6.2% 10.2% 5.9% 10.6% 7.8% 5.8% 10.2% 7.3% 34.2%

perylene 7.4% 52.7% 3.9% 5.8% 4.4% 50.6% 21.5%

indeno[1,2,3-cd]pyrene 66.6% 35.0% 10.2% 11.6% 40.8% 5.0% 10.9% 13.4% 31.3%

benzo[ghi]perylene 1.5% 29.5% 8.1% 8.8% 3.5% 5.9% 32.2%

dibenz[a,h]anthracene 18.4% 22.3% 28.9% 52.5% #DIV/0! 8.7%

cis/trans-decalin 21.7% 20.3% 16.6% 7.7%

dibenzofuran 7.2% 4.7% 10.5%

retene 7.9% 4.3%

benzothiophene 11.6%

dibenzothiophene 10.3% 7.8% 6.2% 2.4% 3.6% 12.8% 5.9% 10.4%

naphthobenzothiophene 4.4% 10.8% 7.0%
29

Table 8. Mussel Tissue (QA10TIS01): Laboratory relative standard deviations of three replicates - Alkylated PAHs 

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17

1-methylnaphthalene 0.8% 11.5% 0.5% 38.7% 11.5% 8.3% 4.7% 17.0% 5.7% 17.7% 12.1%

2-methylnaphthalene 2.4% 28.4% 13.6% 1.1% 5.7% 13.1% 8.1% 4.6% 48.8% 4.9% 18.4% 13.8% 12.8%

2,6-dimethylnaphthalene 2.1% 15.6% 13.0% 0.9% 4.8% 8.0% 4.3% 9.5% 6.6% 10.2% 15.1%

1,6,7-trimethylnaphthalene 0.7% 4.5% 27.0% 10.9% 8.8% 4.6% 14.2% 9.6%

1-methylphenanthrene 5.5% 14.8% 2.6% 2.7% 1.4% 15.3% 5.9% 8.5% 25.0%

C1-decalins 16.0% 10.9% 18.5%

C2-decalins 11.5% 12.9% 9.6%

C3-decalins 9.1% 13.2% 28.0%

C4-decalins 9.9% 11.2% 20.8%

C1-naphthalenes 1.4% 11.8% 9.8% 0.9% 4.7% 12.8% 15.7%

C2-naphthalenes 2.9% 4.4% 13.8% 1.3% 5.4% 7.0% 11.7% 13.5%

C3-naphthalenes 2.1% 11.0% 13.6% 0.8% 12.2% 8.2% 6.1% 12.2% 15.4%

C4-naphthalenes 3.1% 13.4% 15.6% 1.3% 8.5% 4.7% 12.4% 17.3%

C1-benzothiophenes 16.9%

C2-benzothiophenes 10.3%

C3-benzothiophenes 21.4%

C4-benzothiophenes 9.9%

C1-fluorenes 4.1% 15.6% 0.5% 6.5% 2.0% 9.4% 5.2%

C2-fluorenes 5.0% 14.3% 1.1% 7.9% 4.5% 11.3% 11.0%

C3-fluorenes 9.1% 1.2% 3.3% 5.9% 22.3% 11.5%

C1-phenanthrenes/anthracenes 6.0% 18.7% 3.3% 10.9% 7.7% 11.7%

C2-phenanthrenes/anthracenes 4.8% 16.0% 15.3% 1.9% 80.4% 9.2% 8.8% 10.0% 4.7%

C3-phenanthrenes/anthracenes 2.2% 17.6% 2.2% 9.9% 13.6% 11.3% 8.0%

C4-phenanthrenes/anthracenes 7.0% 15.7% 0.6% 9.3% 2.5% 14.4% 19.5%

C1-dibenzothiophenes 13.6% 2.0% 10.3% 2.4% 13.0% 8.6%

C2-dibenzothiophenes 7.1% 1.7% 10.3% 0.8% 12.0% 20.8%

C3-dibenzothiophenes 14.5% 2.8% 9.7% 3.6% 10.6% 7.0%

C4-dibenzothiophenes 16.1% 4.1% 7.6% 12.0% 8.3%

C1-fluoranthenes/pyrenes 2.5% 14.3% 1.5% 9.5% 8.8% 10.6% 7.1%

C2-fluoranthenes/pyrenes 5.4% 13.4% 18.8% 0.2% 12.1% 9.9% 13.5%

C3-fluoranthenes/pyrenes 4.9% 14.9% 1.6% 8.9% 10.7%

C4-fluoranthenes/pyrenes 19.2% 3.1%

C1-naphthobenzothiophenes 12.0% 3.6% 13.0%

C2-naphthobenzothiophenes 2.5% 10.3%

C3-naphthobenzothiophenes 4.4% 21.6%

C4-naphthobenzothiophenes 10.4%

C1-chrysenes 7.6% 15.7% 3.1% 8.8% 10.1% 13.4%

C2-chrysenes 21.1% 1.6% 4.5% 18.7%

C3-chrysenes 32.0% 5.9% 11.4%

C4-chrysenes
30

Table 8 (cont). Mussel Tissue (QA10TIS01): Laboratory relative standard deviations of three replicates - Alkylated PAHs 

Laboratory No. 18 19 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34

1-methylnaphthalene 6.6% 45.5% 5.8% 17.2% 5.9% 31.5% 9.5% 4.3% 11.8% 13.9% 2.5% 6.5% 6.0%

2-methylnaphthalene 12.8% 23.6% 9.8% 11.0% 4.5% 26.9% 10.1% 6.1% 2.8% 14.0% 17.1% 4.6% 8.3%

2,6-dimethylnaphthalene 9.9% 12.6% 5.3% 3.5% 7.1% 39.6% 8.0% 8.7% 4.4% 21.4% 75.4% 6.8% 5.5%

1,6,7-trimethylnaphthalene 11.2% 23.1% 5.4% 6.1% 10.6% 10.9% 21.4% 21.0%

1-methylphenanthrene 9.0% 6.7% 10.0% 2.5% 4.8% 6.6% 3.9% 1.9%

C1-decalins 22.8% 9.2% 3.0%

C2-decalins 27.3% 46.6% 1.5%

C3-decalins 19.5% 26.4% 5.4%

C4-decalins 20.9% 19.5% 16.7%

C1-naphthalenes 24.8% 8.4% 13.4% 5.1% 12.6% 4.9% 2.5% 0.0% 5.7% 1.7%

C2-naphthalenes 4.7% 21.2% 5.8% 5.8% 2.0% 33.5% 5.6% 9.6% 3.3% 3.0% 24.0% 8.0% 7.1%

C3-naphthalenes 0.0% 15.4% 14.2% 13.2% 2.3% 12.8% 6.0% 6.2% 32.5% 5.4% 23.1% 7.4% 10.6% 11.3%

C4-naphthalenes 6.7% 8.7% 8.7% 15.4% 2.5% 19.7% 7.5% 5.3% 75.8% 20.7% 13.7% 15.5% 12.9%

C1-benzothiophenes 3.8% 15.1%

C2-benzothiophenes 15.9% 5.2%

C3-benzothiophenes 33.3% 8.6%

C4-benzothiophenes 17.2% 8.8%

C1-fluorenes 10.1% 10.7% 3.5% 49.7% 4.7% 8.6% 21.4% 6.7% 3.7% 2.6%

C2-fluorenes 7.9% 12.7% 11.7% 1.7% 19.8% 4.1% 7.8% 20.8% 2.3% 1.2% 4.1%

C3-fluorenes 2.7% 19.9% 14.3% 1.1% 19.2% 7.0% 4.9% 21.1% 7.5% 2.7%

C1-phenanthrenes/anthracenes 5.3% 3.3% 7.6% 2.4% 19.4% 72.7% 6.4% 14.7% 1.3% 6.8% 15.8% 2.8%

C2-phenanthrenes/anthracenes 1.9% 4.5% 5.7% 1.7% 22.0% 41.1% 4.2% 7.6% 20.5% 4.2% 8.9% 14.5% 1.9%

C3-phenanthrenes/anthracenes 4.4% 2.9% 14.2% 3.7% 16.6% 3.8% 7.2% 12.3% 6.2% 23.6% 1.8% 2.3%

C4-phenanthrenes/anthracenes 4.9% 16.0% 5.9% 41.5% 3.8% 9.4% 4.2% 8.5% 5.2%

C1-dibenzothiophenes 16.1% 6.5% 3.0% 4.9% 6.6% 0.8% 7.6%

C2-dibenzothiophenes 5.4% 8.0% 2.8% 14.1% 7.4% 7.1% 3.2%

C3-dibenzothiophenes 0.0% 9.6% 2.3% 5.0% 7.9% 4.7% 1.1%

C4-dibenzothiophenes 13.1% 2.2% 11.3% 5.3% 1.7%

C1-fluoranthenes/pyrenes 2.3% 41.7% 11.2% 16.1% 5.1% 4.6% 8.0% 2.1% 5.7%

C2-fluoranthenes/pyrenes 15.4% 8.3% 4.2% 8.1% 5.2% 2.9% 3.4%

C3-fluoranthenes/pyrenes n=1 1.4% 2.8% 7.7% 6.4% 9.8% 5.6%

C4-fluoranthenes/pyrenes 45.5% 8.1% 7.1% 11.4%

C1-naphthobenzothiophenes 11.2% 5.5%

C2-naphthobenzothiophenes 10.2% 6.9%

C3-naphthobenzothiophenes 13.3%

C4-naphthobenzothiophenes

C1-chrysenes 62.6% 4.6% 2.9% 1.6% 6.5% 4.1% 4.1%

C2-chrysenes 52.6% 4.0% 2.9% 0.0% 7.5% 3.0% 5.8%

C3-chrysenes 26.8% 21.0% 2.2%

C4-chrysenes 35.3% 53.6% 2.0%
31

Table 9. Mussel Tissue (QA10TIS01): Laboratory relative standard deviations of three replicates - Biomarkers

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17

Carbazole 23.1%

18a(H)-22,29,30-Trisnorhopane 19.0%

17a(H)-22,29,30-Trisnorhopane 6.8%

17α(H),21β(H)-30-Norhopane 4.7%

18a(H)-30-Norneohopane 14.3%

17a(H)-Diahopane

17α(H),21β(H)-Hopane 4.9% 10.9% 6.8%

17α(H),21β(H)-22R-Homohopane 1.3% 13.0%

17α(H),21β(H)-22S-Homohopane 4.2% 1.4% 13.4%

13b(H)17a(H)-Diacholestane 20S 8.6%

5a(H),14a(H),17a(H)-Cholestane 20S 8.0%

5a(H),14a(H),17a(H)-Cholestane 20R 5.1% 11.5%

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S 4.6% 4.6%

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R 10.9%

5a(H),14b(H),17b(H)-Cholestane 20R 6.6% 6.3%

5a(H),14b(H),17b(H)-Cholestane 20S 5.3%

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R 2.8% 7.1%

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S 7.1%

Table 9 (cont). Mussel Tissue (QA10TIS01): Laboratory relative standard deviations of three replicates - Biomarkers

Laboratory No. 18 19 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34

Carbazole 2.5%

18a(H)-22,29,30-Trisnorhopane 61.4% 7.9%

17a(H)-22,29,30-Trisnorhopane 73.5% 1.3% 2.8%

17α(H),21β(H)-30-Norhopane 4.0% 60.9% 0.8%

18a(H)-30-Norneohopane 73.3% 4.3%

17a(H)-Diahopane 25.9%

17α(H),21β(H)-Hopane 3.3% 13.9% 5.2%

17α(H),21β(H)-22R-Homohopane 3.9% 6.6%

17α(H),21β(H)-22S-Homohopane 4.2% 4.1%

13b(H)17a(H)-Diacholestane 20S 84.6% 7.0%

5a(H),14a(H),17a(H)-Cholestane 20S 6.4%

5a(H),14a(H),17a(H)-Cholestane 20R 5.9% 4.9%

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S 5.4%

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R 72.4% 3.4% 23.1% 4.2%

5a(H),14b(H),17b(H)-Cholestane 20R 38.7% 2.7%

5a(H),14b(H),17b(H)-Cholestane 20S 45.8% 4.2%

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R 5.4% 3.2%

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S 5.3%
32

Table 10. Mussel Tissue (QA10TIS01): p scores (15%) - Water and PAHs 

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17

Percent Water 0.01 0.02 0.01 0.01 0.03 0.03 0.02 0.04 0.08 n=1 0.09 0.01 0.02 0.16 0.04 0.04

naphthalene 0.48 2.43 1.41 0.28 0.19 1.11 1.11 1.78 1.50 0.75 0.37 1.99 0.90 1.63

biphenyl 0.52 4.37 1.10 0.48 0.60 0.16 0.92 0.99 2.12

acenaphthene 0.28 0.68 0.65 0.56 0.43 0.80

acenaphthylene 1.04 1.55 0.13 0.27 0.30 0.74

fluorene 0.40 1.24 0.84 0.09 0.54 0.28 0.36 0.64 0.49 0.65 0.30 0.31 0.40 1.01 1.37

phenanthrene 0.18 0.09 1.60 1.01 0.14 0.32 0.33 0.25 0.85 0.29 0.80 0.24 0.29 0.81 0.80 0.62

anthracene 0.27 5.21 1.48 0.21 0.23 2.09 0.26 0.79 1.63 0.25 0.22 0.91 0.42

fluoranthene 0.15 0.61 1.30 0.95 0.18 0.25 0.25 0.23 1.10 0.21 0.37 0.76 0.15 1.10 0.75 0.52

pyrene 0.24 0.24 0.51 0.95 0.18 0.20 0.28 0.21 1.68 0.56 0.22 0.83 0.18 0.21 0.92 0.71 0.76

benzo[b]fluorene 0.59 0.56 0.28

benz[a]anthracene 0.49 0.99 1.19 0.23 0.34 0.07 0.28 0.80 0.53 0.59 0.02 0.80 0.59 2.12

chrysene 0.53 1.07 0.22 0.21 0.42 0.82 0.18 0.71 0.37 0.20 1.01

triphenylene 0.24

benzo[b ]fluoranthene 0.21 0.33 0.99 0.20 0.16 0.31 0.34 0.80 0.31 0.76 0.39 0.26 0.91 2.49

benzo[j ]fluoranthene 0.51 0.26

benzo[k ]fluoranthene 0.66 0.34 1.36 0.55 0.20 0.75 1.11 1.09 1.21 0.50 0.33

benzo[a]fluoranthene 11.55 0.19

benzo[e]pyrene 0.36 1.11 0.24 0.06 0.42 0.60 0.13 0.62 0.82 0.59

benzo[a]pyrene 0.70 0.80 1.86 0.10 0.28 0.37 2.42 0.23 1.32 0.96 0.40 0.36 0.95

perylene 0.40 0.29 1.50 0.24 0.90 0.85 0.10 0.96

indeno[1,2,3-cd]pyrene 0.71 0.48 0.10 0.82 0.28 1.15 2.35 0.66

benzo[ghi]perylene 0.43 1.56 0.19 1.70 0.40 0.72 1.57 1.04

dibenz[a,h]anthracene 0.77 0.56 0.79 0.92 1.32

cis/trans-decalin 0.86 0.23 0.68

dibenzofuran 1.10 0.76 0.22 0.75 0.17

retene 1.14 0.23 0.70 0.17 0.67 0.64 1.49

benzothiophene 1.19

dibenzothiophene 0.80 0.32 0.81 0.36 0.96 0.82

naphthobenzothiophene 0.33 0.70 0.87
33

Table 10 (cont). Mussel Tissue (QA10TIS01): p scores (15%) - Water and PAHs 

Laboratory No. 18 19 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34

Percent Water 0.05 0.01 0.01 0.00 0.05 0.04 0.10 0.10 0.00 0.00 0.05 0.14 0.02 0.01 0.04 0.03 0.01

naphthalene 1.93 0.65 0.59 0.42 0.18 2.91 0.49 0.97 0.42 0.43 0.68 0.42 0.39 0.33

biphenyl 0.44 0.73 0.28 0.39 0.69 0.35 1.67 0.40

acenaphthene 1.01 0.14 0.39 0.54 0.88 0.70 1.57 1.19 1.46

acenaphthylene 1.98 1.65 1.17 0.78 0.11 0.70 0.30 2.27 0.49

fluorene 0.12 3.27 0.24 0.22 0.21 0.29 0.61 0.13 1.53 0.46 0.83

phenanthrene 0.65 0.04 1.29 0.53 0.38 0.20 0.47 2.24 0.35 0.50 0.73 0.13 1.16 1.25 0.55 0.11 0.68

anthracene 0.44 4.65 0.45 0.28 0.27 0.70 0.33 0.40 0.75 0.23 1.53

fluoranthene 0.50 0.19 1.16 0.16 0.47 0.22 0.54 3.18 0.35 0.36 0.73 0.16 0.89 1.00 0.60 0.13 0.53

pyrene 2.16 0.29 1.67 0.90 0.39 0.26 0.57 3.87 0.20 0.46 0.77 0.16 4.77 2.35 0.50 0.26 0.57

benzo[b]fluorene 0.13 0.65 0.48

benz[a]anthracene 2.03 2.26 0.07 0.38 0.29 0.51 0.41 0.27 0.68 0.25 0.70 1.45 0.21 1.43

chrysene 0.53 1.36 0.92 1.24 0.62 2.47 0.74 1.01 3.29 0.45

triphenylene 0.53

benzo[b ]fluoranthene 0.76 7.05 0.39 0.34 0.18 0.68 1.38 0.53 0.28 0.65 0.50 1.02 0.34 1.41

benzo[j ]fluoranthene

benzo[k ]fluoranthene 0.20 4.67 0.54 0.32 0.61 0.91 1.26 0.24

benzo[a]fluoranthene 2.58

benzo[e]pyrene 0.47 4.41 0.16 0.15 0.53 0.39 0.11 0.72

benzo[a]pyrene 0.46 5.49 0.78 0.66 0.26 0.42 0.68 0.40 0.70 0.52 0.39 0.68 0.49 2.28

perylene 0.49 3.51 0.26 0.39 0.29 3.38 1.43

indeno[1,2,3-cd]pyrene 4.44 2.33 0.68 0.77 2.72 0.33 0.73 0.89 2.09

benzo[ghi]perylene 0.10 1.97 0.54 0.58 0.24 0.39 2.14

dibenz[a,h]anthracene 1.23 1.49 1.93 3.50 0.58 0.00

cis/trans-decalin 1.45 1.35 1.10 0.51

dibenzofuran 0.48 0.32 0.70

retene 0.52 0.29 0.00

benzothiophene 0.77

dibenzothiophene 0.69 0.52 0.42 0.16 0.24 0.86 0.40 0.69

naphthobenzothiophene 0.29 0.72 0.46
34

Table 11. Mussel Tissue (QA10TIS01): p scores (15%) - Alkylated PAHs 

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17

1-methylnaphthalene 0.05 0.77 0.04 2.58 0.77 0.55 0.31 1.13 0.38 1.18 0.81

2-methylnaphthalene 0.16 1.89 0.91 0.07 0.38 0.88 0.54 0.30 3.25 0.32 1.22 0.92 0.85

2,6-dimethylnaphthalene 0.14 1.04 0.87 0.06 0.32 0.53 0.29 0.63 0.44 0.68 1.01

1,6,7-trimethylnaphthalene 0.05 0.30 1.80 0.73 0.59 0.31 0.95 0.64

1-methylphenanthrene 0.37 0.99 0.17 0.18 0.09 1.02 0.39 0.57 1.67

C1-decalins 1.07 0.72 1.24

C2-decalins 0.76 0.86 0.64

C3-decalins 0.61 0.88 1.87

C4-decalins 0.66 0.75 1.39

C1-naphthalenes 0.09 0.79 0.65 0.06 0.31 0.86 1.05

C2-naphthalenes 0.19 0.29 0.92 0.09 0.36 0.46 0.78 0.90

C3-naphthalenes 0.14 0.73 0.91 0.06 0.81 0.55 0.40 0.81 1.03

C4-naphthalenes 0.21 0.89 1.04 0.09 0.56 0.32 0.83 1.15

C1-benzothiophenes 1.13

C2-benzothiophenes 0.69

C3-benzothiophenes 1.43

C4-benzothiophenes 0.66

C1-fluorenes 0.28 1.04 0.04 0.43 0.13 0.63 0.35

C2-fluorenes 0.34 0.95 0.07 0.53 0.30 0.76 0.73

C3-fluorenes 0.61 0.08 0.22 0.39 1.49 0.77

C1-phenanthrenes/anthracenes 0.40 1.25 0.22 0.73 0.51 0.78

C2-phenanthrenes/anthracenes 0.32 1.06 1.02 0.13 5.36 0.61 0.59 0.67 0.31

C3-phenanthrenes/anthracenes 0.14 1.17 0.15 0.66 0.91 0.76 0.53

C4-phenanthrenes/anthracenes 0.46 1.05 0.04 0.62 0.17 0.96 1.30

C1-dibenzothiophenes 0.90 0.13 0.68 0.16 0.87 0.58

C2-dibenzothiophenes 0.48 0.11 0.68 0.05 0.80 1.39

C3-dibenzothiophenes 0.97 0.19 0.65 0.24 0.71 0.47

C4-dibenzothiophenes 1.07 0.27 0.51 0.80 0.55

C1-fluoranthenes/pyrenes 0.17 0.95 0.10 0.63 0.59 0.71 0.47

C2-fluoranthenes/pyrenes 0.36 0.89 1.25 0.01 0.81 0.66 0.90

C3-fluoranthenes/pyrenes 0.33 0.99 0.11 0.59 0.71

C4-fluoranthenes/pyrenes 1.28 0.21 0.00

C1-naphthobenzothiophenes 0.80 0.24 0.87

C2-naphthobenzothiophenes 0.17 0.69

C3-naphthobenzothiophenes 0.29 1.44

C4-naphthobenzothiophenes 0.70

C1-chrysenes 0.51 1.05 0.21 0.58 0.67 0.89

C2-chrysenes 1.41 0.11 0.30 1.25

C3-chrysenes 2.14 0.40 0.76

C4-chrysenes
35

Table 11 (cont). Mussel Tissue (QA10TIS01): p scores (15%) - Alkylated PAHs 

Laboratory No. 18 19 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34

1-methylnaphthalene 0.44 3.04 0.39 1.15 0.39 2.10 0.63 0.29 0.79 0.92 0.17 0.43 0.40

2-methylnaphthalene 0.85 1.57 0.65 0.73 0.30 1.79 0.67 0.40 0.18 0.93 1.14 0.31 0.55

2,6-dimethylnaphthalene 0.66 0.84 0.36 0.23 0.48 2.64 0.53 0.58 0.29 1.43 5.03 0.45 0.37

1,6,7-trimethylnaphthalene 0.75 1.54 0.36 0.41 0.71 0.72 1.43 1.40

1-methylphenanthrene 0.60 0.45 0.67 0.17 0.32 0.44 0.26 0.13

C1-decalins 1.52 0.61 0.20

C2-decalins 1.82 3.11 0.10

C3-decalins 1.30 1.76 0.36

C4-decalins 1.39 1.30 1.11

C1-naphthalenes 1.65 0.56 0.89 0.34 0.84 0.33 0.17 0.38 0.12

C2-naphthalenes 0.31 1.41 0.39 0.38 0.14 2.23 0.37 0.64 0.22 0.20 1.60 0.53 0.47

C3-naphthalenes 1.03 0.95 0.88 0.15 0.85 0.40 0.41 2.17 0.36 1.54 0.50 0.71 0.75

C4-naphthalenes 0.45 0.58 0.58 1.03 0.16 1.31 0.50 0.35 5.06 1.38 0.92 1.03 0.86

C1-benzothiophenes 0.25 0.00 1.01

C2-benzothiophenes 1.06 0.34

C3-benzothiophenes 2.22 0.57

C4-benzothiophenes 1.15 0.58

C1-fluorenes 0.67 0.72 0.23 3.32 0.31 0.57 1.43 0.45 0.24 0.18

C2-fluorenes 0.52 0.85 0.78 0.12 1.32 0.27 0.52 1.39 0.16 0.08 0.27

C3-fluorenes 0.18 1.33 0.95 0.07 1.28 0.46 0.33 1.41 0.50 0.18

C1-phenanthrenes/anthracenes 0.35 0.22 0.51 0.16 1.29 4.85 0.43 0.98 0.08 0.45 1.05 0.19

C2-phenanthrenes/anthracenes 0.13 0.30 0.38 0.11 1.47 2.74 0.28 0.50 1.36 0.28 0.59 0.96 0.13

C3-phenanthrenes/anthracenes 0.29 0.19 0.95 0.25 1.11 0.25 0.48 0.82 0.41 1.58 0.12 0.15

C4-phenanthrenes/anthracenes 0.33 1.07 0.39 2.76 0.26 0.63 0.28 0.56 0.35

C1-dibenzothiophenes 1.08 0.44 0.20 0.33 0.44 0.05 0.51

C2-dibenzothiophenes 0.36 0.54 0.19 0.94 0.49 0.48 0.21

C3-dibenzothiophenes 0.64 0.15 0.34 0.53 0.31 0.07

C4-dibenzothiophenes 0.88 0.15 0.75 0.35 0.11

C1-fluoranthenes/pyrenes 0.16 2.78 0.75 1.07 0.34 0.30 0.53 0.14 0.38

C2-fluoranthenes/pyrenes 1.02 0.55 0.28 0.54 0.35 0.20 0.23

C3-fluoranthenes/pyrenes n=1 0.10 0.19 0.51 0.43 0.66 0.37

C4-fluoranthenes/pyrenes 3.04 0.54 0.47 0.76

C1-naphthobenzothiophenes 0.75 0.37

C2-naphthobenzothiophenes 0.68 0.46

C3-naphthobenzothiophenes 0.89

C4-naphthobenzothiophenes

C1-chrysenes 4.18 0.31 0.20 0.11 0.44 0.27 0.27

C2-chrysenes 3.51 0.27 0.19 0.50 0.20 0.39

C3-chrysenes 1.78 1.40 0.14

C4-chrysenes 2.35 3.58 0.13
36

Table 12. Mussel Tissue (QA10TIS01): p scores (15%) - Biomarkers

Laboratory No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17

Carbazole 1.54

18a(H)-22,29,30-Trisnorhopane 1.26

17a(H)-22,29,30-Trisnorhopane 0.46

17α(H),21β(H)-30-Norhopane 0.31

18a(H)-30-Norneohopane 0.96

17a(H)-Diahopane

17α(H),21β(H)-Hopane 0.33 0.72 0.45

17α(H),21β(H)-22R-Homohopane 0.09 0.87

17α(H),21β(H)-22S-Homohopane 0.28 0.09 0.89

13b(H)17a(H)-Diacholestane 20S 0.57

5a(H),14a(H),17a(H)-Cholestane 20S 0.53

5a(H),14a(H),17a(H)-Cholestane 20R 0.34 0.77

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S 0.31 0.30

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R 0.72

5a(H),14b(H),17b(H)-Cholestane 20R 0.44 0.42

5a(H),14b(H),17b(H)-Cholestane 20S 0.35

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R 0.19 0.47

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S 0.47

Table 12 (cont). Mussel Tissue (QA10TIS01): p scores (15%) - Biomarkers

Laboratory No. 18 19 20 21 22 23 24a 24b 25 26 27 28 29 30 31 32 33 34

Carbazole 0.17

18a(H)-22,29,30-Trisnorhopane 4.09 0.53

17a(H)-22,29,30-Trisnorhopane 4.90 0.09 0.19

17α(H),21β(H)-30-Norhopane 0.27 4.06 0.05

18a(H)-30-Norneohopane 4.89 0.29

17a(H)-Diahopane 1.73

17α(H),21β(H)-Hopane 0.22 0.34

17α(H),21β(H)-22R-Homohopane 0.26 0.44

17α(H),21β(H)-22S-Homohopane 0.28 0.28

13b(H)17a(H)-Diacholestane 20S 5.64 0.47

5a(H),14a(H),17a(H)-Cholestane 20S 0.43

5a(H),14a(H),17a(H)-Cholestane 20R 0.40 0.33

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S 0.36

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R 4.82 0.23 1.54 0.28

5a(H),14b(H),17b(H)-Cholestane 20R 2.58 0.18

5a(H),14b(H),17b(H)-Cholestane 20S 3.05 0.28

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R 0.36 0.21

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S 0.36
37

Table 13. Mussel Tissue (QA10TIS01): Laboratory means of three replicates summarzed by extraction method along with the median values for the extraction method - PAHs (ng/g dry mass) 

 (reported as if three figures were significant)

Soxhlet QuEChERS tissuemizer

Laboratory No. 1 4 7 10 12 13 15 20 26 median 2 6 8 9 24b median 16 23 34 median

naphthalene 43.0 19.7 36.2 <5700 24.2 54.5 350 37.0 24.3 36.6 37.2 104 31.3 other 117 70.6 34.6 26.5 28.4 28.4

biphenyl 12.9 16.0 <14.8 <5700 9.18 21.1 18.3 35.0 16.3 16.3 NA NA NA NA 13.6 16.5 12.2 13.6

acenaphthene 14.0 11.3 <14.8 <5700 7.42 < 30 <10 < 7.4 11.1 11.2 nd 0.00 <0.2 <11 DL 11.7 9.06 10.4 10.4

acenaphthylene <10 9.03 <14.8 <5700 4.50 < 30 12.7 13.8 10.1 10.1 NA <0.2 NA NA 10.7 16.0 7.86 10.7

fluorene 33.9 24.3 19.8 <5700 14.8 33.3 25.3 23.5 18.7 23.9 14.3 43.6 25.2 17.7 DL 21.4 24.0 20.8 21.5 21.5

phenanthrene 119 97.0 139 <5700 117 126 127 133 126 126 56.1 153 134 144 116 134 157 118 148 148

anthracene 10.3 13.3 <14.8 <5700 10.3 9.69 17.7 28.2 11.4 11.4 2.76 12.1 other 10.0 6.10 8.06 15.7 24.2 12.7 15.7

fluoranthene 246 140 196 183 269 210 173 127 227 196 115 247 241 260 215 241 288 221 262 262

pyrene 207 107 121 101 149 149 121 179 158 149 85.4 191 153 196 182 182 189 150 175 175

benzo[b]fluorene NA 17.3 NA NA 15.8 NA NA NA 37.0 17.3 NA NA NA NA NA NA 12.2 12.2

benz[a]anthracene 37.3 19.7 16.3 <5700 32.1 30.8 26.7 63.6 28.3 29.6 8.87 49.9 28.3 other 50.3 39.1 35.4 28.9 34.8 34.8

chrysene coelute 54.7 93.9 <5700 73.0 52.9 88.3 88.7 Other 80.6 59.1 94.8 49.8 107 85.7 85.7 coelute Other coelute

triphenylene coelute NA NA NA NA NA NA Other NA NA NA NA NA Other NA

chrysene/triphenylene 144 79.3 111 108 69.6 102 102

benzo[b ]fluoranthene 26.3 20.7 21.9 <5700 25.0 35.1 Other 36.0 37.5 26.3 14.4 29.8 27.3 30.8 20.8 27.3 34.6 37.6 30.5 34.6

benzo[j ]fluoranthene 28.6 NA NA NA NA Other NA Other 28.6 NA NA NA NA NA NA NA

benzo[k ]fluoranthene 15.4 13.0 20.3 <5700 24.7 14.4 11.0 65.8 Other 15.4 3.54 16.6 11.9 16.8 7.83 11.9 coelute 12.5 coelute 12.5

benzo[b+j ]fluoranthene 0.027

benzo[j+k ]fluoranthene 9.97 31.7 33.9 32.8

benzo[b+j+k ]fluoranthene

benzo[a]fluoranthene <10 1.33 NA NA NA NA NA NA 3.99 2.66 NA NA NA NA NA NA 1.96 1.96

benzo[e]pyrene 38.8 24.3 36.6 <5700 29.3 39.9 NA 68.6 37.4 37.4 NA 39.9 NA NA 39.9 46.7 36.9 42.3 42.3

benzo[a]pyrene 11.4 7.40 <14.8 <5700 7.55 11.7 10.7 29.5 12.7 11.4 3.91 14.7 9.03 18.4 7.05 9.03 11.0 10.4 15.2 11.0

perylene 4.96 2.97 <14.8 <5700 3.93 5.86 <10 172 <10 4.96 NA NA NA NA 6.55 9.40 5.22 6.55

indeno[1,2,3-cd]pyrene 4.75 21.3 <14.8 <5700 4.39 4.58 <10 5.12 7.07 4.93 nd 0.00 5.83 <21 DL 7.70 6.44 7.24 7.24

benzo[ghi]perylene 7.81 6.67 <14.8 <5700 7.81 11.9 <10 < 7.4 8.68 7.81 nd 3.83 8.03 <7 DL 5.93 9.92 7.73 10.7 9.92

dibenz[a,h]anthracene 1.12 0.00 <14.8 <5700 2.28 2.11 <10 < 7.4 7.83 2.11 nd 0.00 <0.2 <9 DL 2.54 1.77 coelute 2.16

dibenz[a,h+a,c]anthracene 3.63 3.63

cis/trans-decalin NA 63.3 NA NA NA NA NA NA 91.9 77.6 NA NA NA NA 142 NA 113 128

dibenzofuran NA 21.3 NA NA 13.8 19.8 NA < 7.4 15.8 17.8 NA NA NA NA 18.2 NA 15.7 17.0

retene NA 42.3 NA NA 50.1 NA 30.0 NA 25.4 36.2 NA NA NA NA 56.2 NA <2.26 56.2

benzothiophene NA 0.00 <14.8 NA <40 NA NA NA <1.3 NA NA NA NA 1.30 NA 1.66 1.48

dibenzothiophene <15 12.7 <14.8 <5700 16.0 12.9 12.0 < 7.4 16.7 12.9 NA NA NA NA 20.4 15.8 18.4 18.4

naphthobenzothiophene NA 11.7 NA NA 13.6 NA NA NA 12.7 12.7 NA NA NA NA 7.41 NA 18.0 12.7

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus means in Tables 1 through 3.
38

Table 13 (cont). Mussel Tissue (QA10TIS01): Laboratory means of three replicates summarzed by extraction method along with the median values for the extraction method - PAHs (ng/g dry mass)

 (reported as if three figures were significant)

Sonication ASE base digestion microwave

Laboratory No. 3 17 19 25 30 31 median 5 11 14 18 21 24a 27 28 29 33 median 22 32

naphthalene <294 625 <78 <conc 14.7 5.50 14.7 12.9 18.4 NA 30.2 23.0 47.0 <12.2 15.0 31.0 22.5 22.8 24.3 <26

biphenyl 130 567 <78 <conc <39.8 6.87 130 Other NA NA 19.1 NA NA 13.3 NA NA NA 16.2 11.8 <26

acenaphthene <294 <3.2 <78 <conc 6.69 11.7 9.18 9.59 NA 9.70 9.64 6.67 NA 7.12 NA DL NA 9.59 10.4 <26

acenaphthylene <294 <3.2 <78 <conc 6.29 <3.0 6.29 2.74 NA 8.08 6.77 4.45 NA 12.5 NA DL NA 6.77 7.68 <26

fluorene <294 227 <78 <conc 18.7 <3.0 18.7 26.0 19.7 30.9 20.3 20.6 DL 19.5 18.5 29.2 25.2 20.6 18.6 <26

phenanthrene 101 760 99.3 92.8 56.6 18.7 96.1 149 114 114 118 114 DL 108 119 134 145 118 121 30.3

anthracene <294 84.6 <78 67.7 8.75 13.7 11.2 10.0 11.4 7.70 17.3 12.8 DL 16.1 <6.21 DL 8.29 11.4 < 40 <26

fluoranthene 181 1160 207 114 176 24.0 179 305 221 209 303 238 DL 242 231 215 277 238 200 52.7

pyrene 112 733 133 73.0 75.8 17.3 93.7 212 141 158 140 117 DL 134 111 154 194 141 154 35.0

benzo[b]fluorene NA <3.2 NA <conc <39.8 NA NA NA NA NA NA NA <15.4 22.4 DL NA 22.4 NA NA

benz[a]anthracene <294 198 <78 <conc 24.0 5.20 24.0 57.8 35.8 38.6 53.2 33.7 DL 34.2 33.8 37.2 55.9 37.2 27.4 <26

chrysene <294 coelute <78 43.8 56.0 15.3 43.8 Other 96.2 35.3 82.5 58.7 29.2 coelute 83.3 coelute 71.2 71.2 other 26.0

triphenylene NA coelute NA NA NA NA Other NA 38.3 82.5 NA NA NA NA coelute NA 60.4 other NA

chrysene/triphenylene 421 139 91.6 107 107 84.4

benzo[b ]fluoranthene <294 261 <78 <conc 21.8 <3.0 38.1 44.0 31.0 32.6 55.5 48.3 42.1 22.4 28.1 57.2 40.1 25.0 coelute

benzo[j]fluoranthene NA coelute NA NA NA NA Other NA 16.6 NA NA NA coelute NA coelute NA 16.6 other coelute

benzo[k ]fluoranthene <294 coelute <78 <conc 14.2 3.20 8.70 Other 25.4 15.1 14.7 14.3 DL NA 30.1 coelute 19.3 17.2 other coelute

benzo[b+j]fluoranthene

benzo[j+k ]fluoranthene 194 32.8 14.7 32.8 32.8 24.7

benzo[b+j+k ]fluoranthene <26

benzo[a]fluoranthene NA <3.2 NA NA NA NA NA NA 5.42 NA NA NA <2.94 NA DL NA 5.42 NA NA

benzo[e]pyrene <294 232 <78 <conc <39.8 4.00 48.9 NA 36.1 39.4 NA NA 40.8 NA 43.1 NA 40.8 37.5 <26

benzo[a]pyrene <294 <3.2 <78 <conc 6.36 26.0 16.2 11.8 11.5 11.0 16.7 12.9 23.3 8.42 11.4 16.5 12.3 12.0 10.6 <26

perylene 191 <3.2 <78 <conc <39.8 12.1 12.1 5.68 NA 4.74 4.16 NA NA <7.65 NA 6.50 NA 5.21 4.57 <26

indeno[1,2,3-cd]pyrene <294 207 <78 <conc 6.36 <3.0 6.36 8.35 9.39 8.22 7.65 13.4 14.2 <4.58 10.5 DL 16.8 10.0 6.61 <26

benzo[ghi]perylene <294 204 <78 <conc 6.36 <3.0 6.36 10.8 NA 9.88 13.1 11.0 NA 7.29 NA 10.5 NA 10.6 8.75 <26

dibenz[a,h]anthracene <294 175 <78 <conc <39.8 <3.0 Other 18.2 <1.5 3.14 5.09 DL <3.28 <4.81 DL 3.23 4.16 other <26

dibenz[a,h+a,c]anthracene 2.35 2.35 1.92

cis/trans-decalin NA <3.2 NA NA <39.8 NA NA NA NA NA NA NA 53.9 NA DL NA 53.9 NA 38.3

dibenzofuran <294 143 <78 <conc <39.8 <3.0 NA NA NA NA NA NA 17.1 NA DL NA 17.1 NA <26

retene NA 245 NA NA NA NA 11.8 NA 28.3 NA NA NA <9.61 NA DL NA 20.1 30.7 <26

benzothiophene NA <3.2 NA NA <39.8 NA NA NA NA NA NA NA <5.15 NA DL NA NA <26

dibenzothiophene <294 <3.2 <78 <conc <39.8 <3.0 20.9 NA 13.4 11.8 14.0 NA 17.6 NA 18.6 NA 15.8 14.6 <26

naphthobenzothiophene NA <3.2 NA NA NA NA Other NA NA NA NA NA 20.4 NA NA NA 20.4 NA <26

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus means in Tables 1 through 3.
39

Table 14. Mussel Tissue (QA10TIS01): Laboratory means of three replicates summarzed by extraction method along with the median values for the extraction method - Alkylated PAHs (ng/g dry mass) 

 (reported as if three figures were significant)

Soxhlet QuEChERS tissuemizer

Laboratory No. 1 4 7 10 12 13 15 20 26 median 2 6 8 9 24b median 16 23 34 median

1-methylnaphthalene 27.2 15.0 113 <5700 23.0 50.5 37.7 37.6 29.7 33.6 NA 50.3 NA NA 50.3 40.1 30.4 34.2 34.2

2-methylnaphthalene 36.2 23.7 64.4 <5700 38.0 90.3 67.7 34.4 41.4 39.7 NA 31.5 NA NA 31.5 60.2 45.1 52.2 52.2

2,6-dimethylnaphthalene 67.0 42.3 NA NA 65.4 101 NA 106 78.8 72.9 NA 70.5 NA NA 70.5 90.2 53.7 73.3 73.3

1,6,7-trimethylnaphthalene 46.5 46.3 NA NA 50.5 74.3 NA 168 81.4 62.4 NA NA NA NA 76.8 41.7 35.6 41.7

1-methylphenanthrene 54.6 23.7 NA NA 70.9 Other NA < 7.4 43.7 49.1 NA 61.1 NA NA 61.1 67.5 59.2 42.3 59.2

C1-decalins NA 390 NA NA NA NA NA NA 560 475 NA NA NA NA 831 NA 547 689

C2-decalins NA 1333 NA NA NA NA NA NA 1733 1533 NA NA NA NA 2137 NA 1353 1745

C3-decalins NA 1900 NA NA NA NA NA NA 2967 2433 NA NA NA NA 1727 NA 1127 1427

C4-decalins NA 2533 NA NA NA NA NA NA 3533 3033 NA NA NA NA 2707 NA 1493 2100

C1-naphthalenes 63.4 23.7 NA <5700 35.5 NA NA 47.2 48.3 47.2 NA NA NA NA 64.7 75.4 55.3 64.7

C2-naphthalenes 255 78.3 NA <5700 125 NA 313 212 180 196 NA NA NA NA 194 173 138 173

C3-naphthalenes 629 153 NA 207 253 NA 419 314 290 290 NA NA NA NA 406 306 235 306

C4-naphthalenes 498 170 NA 110 210 NA 466 319 400 319 NA NA NA NA 362 326 247 326

C1-benzothiophenes NA 0.00 NA NA NA NA NA NA <39 NA NA NA NA 16.9 NA 14.4 15.7

C2-benzothiophenes NA 0.00 NA NA NA NA NA NA <39 NA NA NA NA 34.6 NA 19.5 27.0

C3-benzothiophenes NA 0.00 NA NA NA NA NA NA <39 NA NA NA NA 55.8 NA 49.4 52.6

C4-benzothiophenes NA 0.00 NA NA NA NA NA NA 54.0 54.0 NA NA NA NA 41.6 NA 50.2 45.9

C1-fluorenes 76.8 34.0 NA <5700 37.7 NA 75.7 < 7.4 68.3 68.3 NA NA NA NA 72.4 68.6 51.8 68.6

C2-fluorenes 181 107 NA <5700 109 NA 188 < 7.4 373 181 NA NA NA NA 209 146 150 150

C3-fluorenes 296 473 NA <5700 173 NA 436 < 7.4 780 436 NA NA NA NA 300 242 228 242

C1-phenanthrenes/anthracenes 280 163 NA <5700 226 NA 415 < 7.4 187 226 NA NA NA NA 321 258 257 258

C2-phenanthrenes/anthracenes 521 263 NA 102 326 NA 689 < 7.4 493 410 NA NA NA NA 510 378 398 398

C3-phenanthrenes/anthracenes 467 323 NA <5700 232 NA 1044 < 7.4 460 460 NA NA NA NA 361 294 240 294

C4-phenanthrenes/anthracenes 145 230 NA <5700 113 NA 597 < 7.4 260 230 NA NA NA NA 130 141 92.5 130

C1-dibenzothiophenes 95.9 55.3 NA <5700 72.3 NA 64.7 46.2 82.7 68.5 NA NA NA NA 99.4 85.1 71.4 85.1

C2-dibenzothiophenes 237 140 NA <5700 193 NA 192 < 7.4 287 193 NA NA NA NA 269 215 201 215

C3-dibenzothiophenes 223 143 NA <5700 163 NA 155 61.7 303 159 NA NA NA NA 256 190 186 190

C4-dibenzothiophenes 110 87.0 NA <5700 68.7 NA <40 55.6 263 87.0 NA NA NA NA 110 NA 95.4 103

C1-fluoranthenes/pyrenes 145 70.0 NA <5700 91.9 NA 66.7 373 127 109 NA NA NA NA 134 123 107 123

C2-fluoranthenes/pyrenes 62.3 42.7 NA <5700 55.3 NA 43.0 < 7.4 92.7 55.3 NA NA NA NA 67.1 59.1 59.3 59.3

C3-fluoranthenes/pyrenes 33.4 31.7 NA <5700 24.3 NA <40 57.9 52.3 33.4 NA NA NA NA 40.2 27.0 30.2 30.2

C4-fluoranthenes/pyrenes <15 12.6 NA NA NA NA NA NA <39 12.6 NA NA NA NA NA NA 15.2 15.2

C1-naphthobenzothiophenes NA 55.7 NA NA NA NA NA NA <39 55.7 NA NA NA NA 12.2 NA 18.9 15.5

C2-naphthobenzothiophenes NA 0.00 NA NA NA NA NA NA <39 NA NA NA NA 8.7 NA 15.9 12.3

C3-naphthobenzothiophenes NA 0.00 NA NA NA NA NA NA <39 NA NA NA NA 7.59 NA 9.75 8.7

C4-naphthobenzothiophenes NA 0.00 NA NA NA NA NA NA <39 NA NA NA NA 0.00 NA <0.707

C1-chrysenes 42.6 25.7 NA <5700 28.9 NA NA 35.5 43.5 35.5 NA NA NA NA 44.4 44.7 38.7 44.4

C2-chrysenes 25.7 21.3 NA <5700 16.2 NA NA 210 43.0 25.7 NA NA NA NA 32.2 19.5 23.9 23.9

C3-chrysenes <10 9.93 NA <5700 6.20 NA NA < 7.4 <39 8.07 NA NA NA NA 0.00 6.84 <0.595 6.84

C4-chrysenes <10 0.00 NA NA <40 NA NA < 7.4 <39 NA NA NA NA 0.00 2.93 <0.595 2.93

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus statistics
40

Table 14 (cont). Mussel Tissue (QA10TIS01): Laboratory means of three replicates summarzed by extraction method along with the median values for the extraction method - Alkylated PAHs (ng/g dry mass)

 (reported as if three figures were significant)

Sonication ASE base digestion microwave

Laboratory No. 3 17 19 25 30 31 median 5 11 14 18 21 24a 27 28 29 33 median 22 32

1-methylnaphthalene <294 <6.4 <78 <conc 16.1 7.90 12.0 21.0 27.4 29.8 19.9 25.6 58.3 <24.3 38.3 31.2 47.6 29.8 24.8 <52

2-methylnaphthalene 226 653 <78 <conc 70.5 6.90 70.5 37.1 43.8 47.6 31.8 42.3 94.0 <24.3 24.0 52.5 30.0 42.3 40.8 <52

2,6-dimethylnaphthalene 102 1062 <78 104 27.1 13.2 102 68.8 46.9 41.5 46.5 41.6 118 48.4 69.7 DL 87.5 48.4 76.2 <52

1,6,7-trimethylnaphthalene 112 325 <78 <conc NA 17.7 112 39.4 NA NA 41.4 NA NA 30.6 NA 46.0 NA 40.4 NA <52

1-methylphenanthrene <294 2465 <78 <conc NA <3.0 81.1 56.4 77.1 64.8 57.3 DL 35.1 <8.65 83.8 0.00 61.0 57.3 <52

C1-decalins NA 2467 NA <conc NA NA NA NA NA NA NA NA 30.6 NA DL NA NA <52

C2-decalins NA 14233 NA <conc NA NA NA NA NA NA NA NA 45.6 NA DL NA NA <52

C3-decalins NA 21200 NA <conc NA NA NA NA NA NA NA NA 310 NA DL NA NA <52

C4-decalins NA 24533 NA <conc NA NA NA NA NA NA NA NA 506 NA DL NA NA <52

C1-naphthalenes 596 862 <78 <conc NA 13.0 58.2 NA NA NA 63.4 NA <24.3 62.3 90.0 77.5 63.4 65.5 <52

C2-naphthalenes 378 2728 123 <conc NA 26.0 251 236 NA NA NA 277 508 102 263 229 321 263 298 <52

C3-naphthalenes 391 4270 200 <conc NA 27.0 295 606 NA NA NA 390 497 226 498 695 435 497 615 54.3

C4-naphthalenes 594 5307 227 <conc NA 18.3 410 600 NA NA NA 240 683 279 138 Other 313 296 554 76.0

C1-benzothiophenes NA <3.2 NA <conc NA NA NA NA NA NA NA NA 21.1 NA DL NA 21.1 NA <52

C2-benzothiophenes NA <3.2 NA <conc NA NA NA NA NA NA NA NA 12.4 NA DL NA 12.4 NA <52

C3-benzothiophenes NA <3.2 NA <conc NA NA NA NA NA NA NA NA 20.4 NA DL NA 20.4 NA <52

C4-benzothiophenes NA <3.2 NA <conc NA NA NA NA NA NA NA NA 37.8 NA DL NA 37.8 NA NA

C1-fluorenes <294 856 <78 <conc NA <3.0 68.6 NA NA NA 84.9 98.7 70.1 21.5 446 103 84.9 140 <52

C2-fluorenes <294 2563 147 <conc NA <3.0 147 186 NA NA NA 195 193 190 181 658 77.2 190 312 60.0

C3-fluorenes <294 <3.2 217 <conc NA <3.0 217 262 NA NA NA 48.4 DL 354 <6.89 558 277 277 530 67.0

C1-phenanthrenes/anthracenes <294 <3.2 190 <conc NA <3.0 190 425 NA NA NA 312 685 230 360 554 433 425 328 59.3

C2-phenanthrenes/anthracenes 662 2353 307 106 NA <3.0 484 626 NA NA NA 113 1457 393 536 934 639 626 546 93.3

C3-phenanthrenes/anthracenes <294 3257 263 <conc NA <3.0 1760.0 508 NA NA NA 155 469 307 356 837 482 469 547 77.0

C4-phenanthrenes/anthracenes <294 1380 117 <conc NA <3.0 117 209 NA NA NA NA 5.48 159 <9.48 426 237 209 590 <52

C1-dibenzothiophenes <294 385 <78 <conc NA <3.0 92.1 NA NA NA NA NA 71.6 NA 188 NA 92.1 103 <52

C2-dibenzothiophenes <294 946 107 <conc NA <3.0 107 245 NA NA NA NA NA 226 NA 651 NA 245 355 54.0

C3-dibenzothiophenes <294 1113 110 <conc NA <3.0 110 206 NA NA NA NA NA 234 NA 705 NA 234 321 <52

C4-dibenzothiophenes <294 877 <78 <conc NA <3.0 103 NA NA NA NA NA 108 NA 433 NA 108 132 NA

C1-fluoranthenes/pyrenes <294 717 99 <conc NA <3.0 98.7 114 NA NA NA 338 NA 115 NA 112 NA 115 376 <52

C2-fluoranthenes/pyrenes 166 <3.2 <78 <conc NA <3.0 166 68.3 NA NA NA 91.6 NA 71.7 NA 84.2 NA 78.0 291 <52

C3-fluoranthenes/pyrenes <294 <3.2 <78 <conc NA <3.0 37.1 NA NA NA NA NA 36.2 NA 40.9 NA 37.1 99.1 <52

C4-fluoranthenes/pyrenes NA <3.2 NA <conc NA <3.0 12.2 NA NA NA NA NA 16.9 NA 18.5 NA 16.9 22.4 NA

C1-naphthobenzothiophenes NA <3.2 NA <conc NA <3.0 20.4 NA NA NA NA NA 19.1 NA NA NA 19.7 NA <52

C2-naphthobenzothiophenes NA <3.2 NA <conc NA <3.0 13.8 NA NA NA NA NA 16.0 NA NA NA 14.9 NA <52

C3-naphthobenzothiophenes NA <3.2 NA <conc NA <3.0 6.97 NA NA NA NA NA <8.19 NA NA NA 6.97 NA <52

C4-naphthobenzothiophenes NA <3.2 NA <conc NA <3.0 3.10 NA NA NA NA NA <8.19 NA NA NA 3.10 NA NA

C1-chrysenes <294 308 <78 <conc NA <3.0 56.9 NA NA NA NA NA 41.6 NA 43.9 NA 43.9 60.9 <52

C2-chrysenes <294 <3.2 <78 <conc NA <3.0 31.2 NA NA NA NA NA 22.4 NA 21.8 NA 22.4 30.6 <52

C3-chrysenes <294 <3.2 <78 <conc NA <3.0 13.5 NA NA NA NA NA <13.8 NA 12.3 NA 12.9 6.74 <52

C4-chrysenes <294 <3.2 <78 <conc NA <3.0 <1.79 NA NA NA NA NA <13.8 NA 7.81 NA 7.81 0.540 <52

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus statistics
41

Table 15. Mussel Tissue (QA10TIS01): Laboratory means of three replicates summarzed by extraction method along with the median values for the extraction method - Biomarkers (ng/g dry mass) 

 (reported as if three figures were significant)

Soxhlet QuEChERS tissuemizer

Laboratory No. 1 4 7 10 12 13 15 20 26 median 2 6 8 9 24b median 16 23 34 median

Carbazole NA NA NA <40 NA Other NA <1.7 NA NA NA NA NA NA 6.85 6.85

18a(H)-22,29,30-Trisnorhopane NA NA <5700 <40 NA Other 131 NA 131 NA NA NA NA 15.3 NA 19.8 17.6

17a(H)-22,29,30-Trisnorhopane <25 NA <5700 <40 NA Other 79.6 NA 79.6 NA NA NA NA 15.7 NA 20.8 18.2

17α(H),21β(H)-30-Norhopane <25 NA <5700 <40 NA Other < 7.4 NA NA NA NA NA 0.00 NA 51.2 25.6

18a(H)-30-Norneohopane NA NA <5700 <40 NA Other < 7.4 NA NA NA NA NA 48.2 NA 18.1 33.2

17a(H)-Diahopane NA NA <5700 <40 NA Other < 7.4 NA NA NA NA NA 0.00 NA 5.48 2.74

17α(H),21β(H)-Hopane 65.7 NA <5700 <40 NA Other < 7.4 81.1 73.4 NA NA NA NA 59.8 NA 78.9 69.4

17α(H),21β(H)-22R-Homohopane <20 NA <5700 <40 NA Other < 7.4 NA NA NA NA NA 18.4 NA 20.5 19.4

17α(H),21β(H)-22S-Homohopane 23.1 NA <5700 <40 NA Other < 7.4 NA 23.1 NA NA NA NA 25.0 NA 24.4 24.7

13b(H)17a(H)-Diacholestane 20S NA NA <5700 <40 NA Other 50.6 NA 50.6 NA NA NA NA 18.2 NA 17.7 18.0

5a(H),14a(H),17a(H)-Cholestane 20S NA NA NA <40 NA Other < 7.4 NA NA NA NA NA 26.8 NA 29.1 28.0

5a(H),14a(H),17a(H)-Cholestane 20R 38.2 NA <5700 <40 NA Other < 7.4 NA 38.2 NA NA NA NA 47.1 NA 52.4 49.7

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S NA NA <5700 <40 NA Other 21.0 NA 21.0 NA NA NA NA 12.4 NA 11.3 11.9

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R 29.0 NA <5700 <40 NA Other 66.2 NA 47.6 NA NA NA NA 31.0 NA 32.4 31.7

5a(H),14b(H),17b(H)-Cholestane 20R <20 NA <5700 <40 NA Other < 7.4 NA NA NA NA NA 17.1 NA 17.7 17.4

5a(H),14b(H),17b(H)-Cholestane 20S NA NA <5700 <40 NA Other < 7.4 NA NA NA NA NA 18.5 NA 18.8 18.7

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R <20 NA <5700 <40 NA Other < 7.4 NA NA NA NA NA 19.8 NA 23.7 21.8

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S NA NA <5700 <40 NA Other < 7.4 NA NA NA NA NA 20.0 NA 18.1 19.1

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus statistics

Table 15 (cont). Mussel Tissue (QA10TIS01): Laboratory means of three replicates summarzed by extraction method along with the median values for the extraction method - Biomarkers (ng/g dry mass)

 (reported as if three figures were significant)

Sonication ASE base digestion microwave

Laboratory No. 3 17 19 25 30 31 median 5 11 14 18 21 24a 27 28 29 33 median 22 32

Carbazole NA 223 NA <conc NA NA 223 NA NA NA NA NA NA NA NA NA NA < 10 NA

18a(H)-22,29,30-Trisnorhopane <294 NA <78 <conc NA <3.0 NA NA NA NA NA NA NA NA NA NA NA NA

17a(H)-22,29,30-Trisnorhopane <294 NA <78 <conc NA <3.0 NA NA coelution NA NA NA NA NA NA NA 23.2 NA

17α(H),21β(H)-30-Norhopane <294 NA <78 <conc NA 112 112 NA NA 20.3 NA NA NA NA NA NA NA 20.3 60.2 NA

18a(H)-30-Norneohopane <294 NA <78 <conc NA 86.7 86.7 NA NA NA NA NA NA NA NA NA NA NA NA

17a(H)-Diahopane <294 NA <78 <conc NA <3.0 NA NA NA NA NA NA NA NA NA NA NA NA

17α(H),21β(H)-Hopane <294 558 <78 <conc NA <3.0 558 NA NA 65.3 NA NA NA NA NA NA NA 65.3 68.8 NA

17α(H),21β(H)-22R-Homohopane <294 NA <78 <conc NA <3.0 NA NA 12.4 NA NA NA NA NA NA NA 12.4 23.8 NA

17α(H),21β(H)-22S-Homohopane <294 NA <78 <conc NA <3.0 NA NA 20.8 NA NA NA NA NA NA NA 20.8 29.4 NA

13b(H)17a(H)-Diacholestane 20S <294 NA <78 <conc NA <3.0 NA NA NA NA NA NA NA NA NA NA NA NA

5a(H),14a(H),17a(H)-Cholestane 20S <294 NA <78 <conc NA <3.0 NA NA NA NA NA NA NA NA NA NA NA NA

5a(H),14a(H),17a(H)-Cholestane 20R <294 NA <78 <conc NA <3.0 NA NA 36.8 NA NA NA NA NA NA NA 36.8 36.4 NA

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S <294 NA <78 <conc NA <3.0 NA NA 16.8 NA NA NA NA NA NA NA 16.8 NA NA

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R <294 NA <78 <conc NA 24.7 24.7 NA NA NA NA NA NA NA NA NA NA 27.6 NA

5a(H),14b(H),17b(H)-Cholestane 20R <294 NA <78 <conc NA 67.3 67.3 NA NA 20.0 NA NA NA NA NA NA NA 20.0 < 30 NA

5a(H),14b(H),17b(H)-Cholestane 20S <294 NA <78 <conc NA 59.7 59.7 NA NA NA NA NA NA NA NA NA NA NA NA

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R <294 NA <78 <conc NA <3.0 NA NA 8.75 NA NA NA NA NA NA NA 8.75 13.0 NA

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S <294 NA <78 <conc NA <3.0 NA NA NA NA NA NA NA NA NA NA NA NA

NA=Not analyzed; DL=Detection limit; No value in space=nothing reported by lab: Bolded values were not used in the calculation of the consensus statistics
42

APPENDIX A

Interlaboratory Analytical Comparison Study to Support Deepwater Horizon Natural Resource 

Damage Assessment

Intercomparison Exercise: Mussel Tissue QA10TIS01

Description of Materials and Instructions

Intercomparison Exercise Materials:

Each of the three jars contains approximately 15 g (wet basis) of Mussel Tissue QA10TIS01. This 

cryogenically homogenized fresh frozen 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. This material can be obtained from the NIST Standard Reference Materials Program 

($798/5 x 8 g to 10 g bottles). See the following link for information on ordering on-line: https://wwws.nist.gov/srmors/view_detail.cfm?srm=1974B

Storage of Materials:

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 QA10TIS01 and SRM 1974b using your laboratory's and/or 

program's analytical protocols, for the concentrations (mass/mass [dry-mass basis]) of the parent 

polycyclic aromatic hydrocarbon (PAH) compounds, alkylated PAH compounds, and biomarkers 

currently being determined in your laboratory. A target list of compounds are presented in Table 1;

however, participants do not need to quantify all of these compounds and can add additional 

compounds when reporting data. 

The percentage of water in the mussel tissue 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 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 

QA10TIS01 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 
43

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 QA10TIS01 and at least one or more samples of 

SRM 1974b using your protocol for tissue samples. If time allows, we are asking that you analyze one 

sample of Mussel Tissue QA10TIS01 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 analytes quantified in each 

of the three replicates of the Mussel Tissue QA10TIS01 and of SRM 1974b. Report results in units of 

ng/g dry-mass 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 QA10TIS01.

If you know that a target or non-target compound is interfering (coeluting) with the determination of a 

target analyte, please identify this issue by qualifying the data and note the data qualifier used at the 

bottom of your table of results. 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, QA10TIS01.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 attached file. 

Submit your results by April 8, 2011 as an attached file via e-mail to: 

michele.schantz@nist.gov 
44

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
45

Table 1: Preliminary List of Analytes of Interest in the Interlaboratory Analytical 

Comparison Study to Support Deepwater Horizon Natural Resource Damage 

Assessment

PAHs

Naphthalene cis/trans-Decalin

Biphenyl Dibenzofuran

Acenaphthene Retene

Acenaphthylene Benzothiophene

Fluorene Dibenzothiophene

Phenanthrene Naphthobenzothiophene

Anthracene

Fluoranthene

Pyrene

Benzo[b]fluorene

Benz[a]anthracene

Chrysene

Triphenylene

Benzo[b]fluoranthene

Benzo[j]fluoranthene

Benzo[k]fluoranthene

Benzo[a]fluoranthene

Benzo[e]pyrene

Benzo[a]pyrene

Perylene

Indeno[1,2,3-cd]pyrene

Benzo[ghi]perylene

Dibenz[a,h]anthracene

Alkylated PAHs

1-Methylnaphthalene C1-Naphthalenes

2-Methylnaphthalene C2-Naphthalenes

2,6-Dimethylnaphthalene C3-Naphthalenes

1,6.7-Trimethylnaphthalene C4-Naphthalenes

1-Methylphenanthrene

C1-Benzothiophenes

C1-Decalins C2-Benzothiophenes

C2-Decalins C3-Benzothiophenes

C3-Decalins C4-Benzothiophenes

C4-Decalins
46

Table 1 (cont.)

C1-Fluorenes C1-Naphthobenzothiophenes

C2-Fluorenes C2-Naphthobenzothiophenes

C3-Fluorenes C3-Naphthobenzothiophenes

C4-Naphthobenzothiophenes

C1-Phenanthrenes/anthracenes

C2- Phenanthrenes/anthracenes C1-Chrysenes

C3- Phenanthrenes/anthracenes C2-Chrysenes

C4- Phenanthrenes/anthracenes C3-Chrysenes

C1-Dibenzothiophenes C4-Chrysenes

C2-Dibenzothiophenes

C3-Dibenzothiophenes

C4-Dibenzothiophenes

C1-Fluoranthenes/pyrenes

C2-Fluoranthenes/pyrenes

C3-Fluoranthenes/pyrenes

C4-Fluoranthenes/pyrenes

Biomarkers

Carbazole

18α(H)-22,29,30-Trisnorhopane

17α(H)-22,29,30-Trisnorhopane

17α(H),21β(H)-30-Norhopane

18α(H)-30-Norneohopane

17α(H)-Diahopane

17α(H),21β(H)-Hopane

17α(H),21β(H)-22R-Homohopane

17α(H),21β(H)-22S-Homohopane

13β(H) 17α(H)-Diacholestane 20S

5α(H),14α(H),17α(H)-Cholestane 20S

5α(H),14α(H),17α(H)-Cholestane 20R

5α(H),14α(H),17α(H)-24-Ethylcholestane 20S

5α(H),14α(H),17α(H)-24-Ethylcholestane 20R

5α(H),14β(H),17β(H)-Cholestane 20S

5α(H),14β(H),17β(H)-Cholestane 20R

5α(H),14β(H),17β(H)-24-Ethylcholestane 20S

5α(H),14β(H),17β(H)-24-Ethylcholestane 20R
47

Appendix B

Summary of Method Information Provided by the Participating Laboratories
48

Extraction parameters used by labs for tissue samples

g extracted g extracted % water Extraction Extraction Extraction Extraction

Lab # Reported QA10TIS01 SRM 1974b Determination Method Solvent Time other

1 3/22/2011 8 8 Oven drying at 110°C until stable mass Soxhlet dichloromethane (DCM) 20 h mixed with hydromatrix in the extraction cell

2 3/16/2011 5 5 Loss on drying 140°C for 12 h QuEChERS acetonitrile

3 3/28/2011 2.5 & 10 10 ASTM D2216 SW-846 3550B DCM 3 times at 3 min each

4 3/30/2011 5 5 Modified EPA 160.3 EPA 3541 DCM 4h

5 4/5/2011 2 2 Oven-drying at 120°C overnight.

Accelerated solvent extraction 

(ASE) DCM ~16 min.

ASE conditions: Pressure = 2000 psi (13.8 

Mpa), temperature = 100°C

6 4/6/2011 5 5

AOAC Official Method 952.08 Solids (Total) in 

Seafood QuEChERS Acetonitrile 1 min

15.00 mL to ~5g shake 1 min with ceramic 

homogenizers; used Genogrinder to shake (500 

SPM)

7 4/7/2011 5 5

Small amount of sample placed in 1 dram shell 

vial and heated to >1050C on a heating block 

for over 8 h. Soxhlet 1:1 DCM : Acetone 12 - 16 h 2 - 3 cycles per hour - overnight

8 4/5/2011 5 5

Weighed aliquot of sample before and after 

drying in vacuum oven at 90°C QuEChERS Acetonitrile shake 1 min, rotate 10 min

extraction with acetonitrile and HPLC water, 6g 

MgSO4 1.5g sodium bicarbinate in 50mL glass 

tubes; centrifuge at 2000rpm (210 rad/sec) for 8 

min, solvent exchange to hexane

9 4/7/2011 5 5

Weighed about 0.5 g and dried at 100°C for 24 

h. Repeated drying until constant weight. modified QuEChERS Acetonitrile (ACN) 2 min via Genogrinder

Added 15 mL ACN + ceramic homogenizer & 

mixed for 1 min, then add 6 g magnesium 

sulfate + 1.5 g sodium acetate & mixed for 1 

min, then centrifuged for 10 min & filtered top 

layer using 0.2 μm PTFE filter prior to analysis.

10 4/8/2011 15 0 2540G 8270 3541 DCM\ Acetone

2h program:starts at 150°C 

boils 15 min/4-15 min 

reductions/55min extraction/3-

15min reductions/ Cools for 45 

min/ pulled off/ N blow down.

11 4/7/2011 2 2

Gravimetric Determination of Water by Drying 

and Weighing Ruiz, R. P. 2001. Current 

Protocols in Food Analytical Chemistry. John 

Wiley & Sons

ASE (sample + sodium sulfate + 

magnesium sulfate) DCM 10 min per sample

12 4/8/2011 10 10 SW 846 Guidance 3540 DCM: Acetone 18 h

13 4/8/2011 5 5

Dried an aliquot of sample in the oven at 105°C 

for 24 h Soxhlet 50% hexane/acetone > 18 h

14 4/8/2011 5 4.5 Dry for 24 h at 110°C. ASE DCM 3 cycles at 5 min each

 The cell temperature was 100 °C, equilibration 

5 min, static time 5 min, cell pressure was 2000 

psi (13.8 Mpa) and there were three cycles 

15 4/7/2011 5.1 NA Oven dry 105°C-Gravimetric Modified EPA 3540 DCM Minimum 16 h

16 4/8/2011 5 to 10 5 to 10 Drying oven at 105°C overnight

 SOP 5-190 - tissumizer 

extraction DCM 2 x 2 min 30 min on orbital shaker table (third extraction)

17 4/8/2011 10 10 160.3 Modified / TS EPA 3550 DCM

Approx. 3 h extraction; 2 h 

silica cleanup; 1 h 

concentration

18 4/8/2011 5 5 gravimetric

ASE, KD, Silica Gel column, 

KD DCM, Hexane 1 day
49

Extraction parameters used by labs for tissue samples (cont)

g extracted g extracted % water Extraction Extraction Extraction Extraction

Lab # Reported QA10TIS01 SRM 1974b Determination Method Solvent Time other

19 4/8/2011 13.2 - 14.6 9.9 - 12.2 160.3 Sonication Acetone/DCM (50/50) 3 min in triplicate

20 4/8/2011 10.2 6.8 SM 2540G SW846 3541 DCM / Acetone 2.5 h

21 4/8/2011 5 5 Freeze drying 7 days at -20°C ACE-350 NOAA procedure DCM

21 min total time with two 

cycles extraction

22 4/8/2011 15 10 Gravimetric Base digest Pentane 4.5 h

23 4/7/2011 20 7

An aliquat (~1g) was removed and dried to a 

constent weight after drying at 40°C Tissuemizer with sodium sulfate DCM three times for 3 min each time

24a 4/8/2011 2.1 2 Microwave moisture analyzer

NOAA Technical Memorandum 

NMFS-NWFSC-59 isooctane 24 h

24b 4/6/2011 5 Microwave moisture analyzer

QuEChERS-based method for 

LC-FLD screening acetonitrile 1.5 h

25 4/8/2011 8 8

2g of each sample was dried in an oven set to 

105°C for 3 h. 3550B sonication extraction 1:1 DCM/Acetone

3x 3min with sonic disrupter 

horn

26 4/8/2011 10 5 EPA 160.3 EPA 3541 DCM 3:12

27 4/8/2011 9.6 5 oven drying at 105°C to constant weight ASE DCM 13 min per sample

1500 psi (10.4 Mpa), 100°C Celsius, 2 static 

extraction cycles/sample, reduction to 2.0 to 3.0 

mL using water bath

28 4/8/2011 2 2 Drying overnight in an oven set at 90°C NOAA Method (July 2010) DCM 20 min

29 4/4/2011 5 4 gravimetric: 1g dried at 120°C for 24 h ASE DCM ~30min ground w/ sodium sulfate

30 4/15/2001 6 6

aliquot weighed into aluminum dish then dried 

at 110°C for 4 h, then weighed again and % 

solids calculated sonic bath 50:50 acetone and DCM overnight

31 4/22/2011 15 3550C DCM 4/19/11 4:00pm

32 4/26/2011 17 4 Dry at 106°C SW3546 (Microwave) DCM/Acetone 90:10 20 min (2x) Exchanged to hexane

33 4/27/2011 2.5 2.5

University of Massachusetts - Determination of 

Moisture and Total Solids; Gravimetric drying 

at 100 °C for 8 h.

NOAA Technical Memorandum 

NMFS-NWFSC-59 ACE - DCM 30 min

34 5/6/2011 ~8 ~8 Gravimetric, SM2540G Tissuemizer, Lab SOP - OP-003 DCM

6 minutes total (3 x 2min serial 

extractions)
50

Sample clean-up and quantification methods used by laboratories for tissue study 

Method of 

Lab # Sample extract cleanup method quantification

1

concentrate extract to 0.5 mL with solvent change to hexane; pass through two aminoproyl solid phase extraction (SPE) columns in series using 20 mL of 20% 

methylene chloride in hexane (same solvent mixture and volume used to condition the SPE columns) concentrate fraction to 0.5 mL and transfer to autosampler vial IS

2 QuEChERS ES

3 Gel Permeation Column (GPC) IS

4 Silica Gel IS

5 Gravity flow column with silica gel and neutral alumina, followed by size-exclusion HPLC to elute fraction containing PAHs and alkyl-PAHs. IS

6

QuEChERS packet added (6 g magnesium sulfate and 1.5 g of sodium acetate), shake vigorously 1 min, centrifuge at 3000 rpm for 10 min, filter through 0.2 um 

PTFE syringe filter ES

7

1. SX-3 Size Exclusion Chromatography (SEC) with DCM Elution; 2. KOH-Impregnated Silica Gel 60 (SG-60; 5g) Flash Chromatography with 5% Methyl t Butyl 

Ether (MtBE) in Hexanes Elution; 3. Phenogel (Phenomenex) SEC with DCM Elution; 4. 3% Aqueous Deactivated SG-60 (5g) Flash Chromatography with Hexanes 

(Impurities - Discarded) Followed by 25% MtBE in Hexanes (PAHs) Elution IS

8

4.2g 60 mesh activated Silica gel with 1cm layer sodium sulfate. Column rinsed with 3:1 hexane:MeCl2 followed by additional Hexane rinse. Sample added followed 

by 40mL Hexane. PAHs eluted with 3:1 Hexane:MeCl2 Solvent exchange to Iso-octane for analysis IS

9 No post extraction sample cleanup. ES

10 GPC IS

11 Silica/Alumina Column Chromatography (gravity-flow); Gel Permeation Chromatography (GPC) - J2 Scientific IS

12 3640; 3630 IS

13 Gel Permeation Chromatography IS

14 Alumina solid phase extraction. IS

15 GPC followed by a neutral alumina/silica column cleanup IS for PAH; ES for biomarkers

16 Alumina cleanup followed by silica gel cleanup IS

17 Silica gel cleanup performed. IS

18 IS

19 filter through sodium sulfate, followed by GPC, followed by silica gel IS

20 None IS

21 GPC IS

22 Column chromatography; PAHs & bimarkers - 5% deactivated silica gel; PAHs-5% deactivated silica gel, 2%-deactivated alumina, biobead. IS

23 Silica gel/Alumina columns and HPLC Phenogel IS

24a GPC IS

24b None ES

25 None IS

26 EPA 3630 IS

27 silica/alumina column chromatography, HPLC (Phenogel 100A columns), reduction to 0.5 mL in water bath IS

28 Silica/Alumina Column Chromatography; Size Exclusion High-Performance Liquid Chromatography IS

29 Extracts were filtered through silicone-treated filter papers and sodium sulfate, GPCed, and cleaned with alumina. IS

30 SW 846 3630 modified - silica gel IS

31 IS

32 Silica Gel IS

33 Alumina/Silica Cleanup Column followed by J2 - GPC Cleanup IS

34

PAH: 3610 - alumina cleanup, followed by 3640 - GPC cleanup; Biomarker: 3610 - alumina cleanup, followed by 3640 - GPC cleanup, followed by 3630 Silica 

fractionation. F1 portion collected for Biomarkers. IS
51

Analytical methods used for PAHs

PAHs mode of injection 

Calibration 

Curve

Lab # Instrument Phase Dimensions (split/splitless/on-column) # points range*

1 GC/MS DB-17MS 60m x 0.25mm, 0.25μm film on-column 6 varied by compound

2 HPLC/FLD Zorbax PAH 5 cm x 4.6 mm, 1.8 um part 10 ul direct 3 2.5 ppb to 50 ppb

3 GC/MS DB-5 60m x 0.25mm, 0.25μm film splitless 6 0.1 ug/mL to 4.0 ug/mL

4 GC/MS ZB-5MS 30m x 0.25mm, 0.25μm film split/splitless 10 2 ppb to 2000ppb

5 GC/MS DB-5 60m x 0.25mm, 0.25μm film on-column 6 0.001ng/μL to 0.33 ng/μL

6 LC Zorbax Ecliple PAH Rapid Resolution HT 50 mm x 4.6 mm, 1.8 um part 3 2.5 ng/g to 50 ng/g

7 GC/MS DB-5 30m x 0.25mm, 0.25μm film on-column 7 10ng/mL to 4000ng/mL

8 GC/MS

Crossbond® silarylene phase; similar to 

50% phenyl/50% dimethyl polysiloxane 30m x 0.25mm, 0.25μm film LVI/ solvent vent 6

1ng/mL to 500 ng/mL (0.2 ng/g 

to100ng/g)

9 HPLC polymeric C18 50 mm x 4.6 mm, 1.8 um part on-column 3 2.5 ng/mL - 50 ng/mL

10 GC/MS ZB-MS-5si 60m x 0.25mm, 0.25μm film 6 0.1 ug/mL to 4.0 ug/mL

11 GC/MS DB-5MS 60m x 0.25mm, 0.25μm film on-column 6 1 ng/mL to 300ng/mL

12 GC/MS ZB-5MSi 60m x 0.25mm, 0.25μm film splitless 6 0.008 ug/mL to 0.80 ug/mL

13 GC/MS DB-5 30m x 0.25mm, 0.25μm film 6 5 ng/mL to 1000 ng/mL

14 GC/MS Rxi-17 sil 60m x 0.25mm, 0.25μm film splitless 6 0.1 ng/g to 1000 ng/g

15 GC/MS DB-5 30m x 0.25mm, 0.25μm film splitless 6 0.05 mg/L to 5.0 mg/L

16 GC/MS DB-5 60m x 0.25mm, 0.25μm film splitless 7 0.01 to 7.2

17 GC/MS Rtx-5MS 30m x 0.32mm, 0.25μm film split 8 4ug/g - 1000ug/g

18 GC/MS DB-EUPAH CF 20m x 0.18mm, 0.14μm film pulsed splitless 6 0.5pg/uL - 100pg/uL

19 GC/MS 5% phenylpolydimethyl 60m x 0.25mm, 0.25μm film splitless 6 0.1 ug/mL to 4 ug/mL

20 GC/MS ZB5MSi 60m x 0.25mm, 0.25μm film 6 0.02 ug/L to 0.8 ug/L

21

GC/MS 

QQQ HP-5MS 30m x 0.25mm, 0.25μm film pulsed splitless 7 or 8 1 ppb to 500 ppb

22 GC/MS RTX-5 30m x 0.25mm, 0.25μm film split/splitless 5 50 ng/mL to 5000ng/mL

23 GC/MS DB5-MS 30m x 0.25mm, 0.25μm film split/splitless 5 20 ng/mL to 1000 ng/mL

24a GC/MS DB-5MS 60m x 0.25mm, 0.25μm film on-column 6 1ng/mL to 330 ng/mL

24b LC-FLD C18 Rapid resolution 50 mm x 4.6 mm, 1.8 um part on-column 3 2.5 ng/mL to 50 ng/mL

25 GC/MS ZB-5MSI 60m x 0.25mm, 0.25μm film pulsed splitless 6 0.1 ug/m to -4.0ug/ml

26 GC/MS ZB-5MS 30m x 0.25mm, 0.25μm film splitless 10 2.0 ng/mL to 2000 ng/mL

27 GC/MS HP-5MS 60m x 0.25mm, 0.25μm film split 5 (20, 100, 250, 500,1000) 

28 GC/MS DB-5 60m x 0.25mm, 0.25μm film 6 3 ppm to 333 ppm

29 GC/MS DB-5MS 30m x 0.25mm, 0.25μm film PTV 6 10ng/ml to 5000ng/ml

30 GC/MS 5MS 30m x 0.25mm, 0.25μm film split/splitless 5 0.050 ug/mL to 10ug/mL

31 GC/MS ZB-5msi 60m x 0.25mm, 0.25μm film splitless 6 0.1 ppm to 4.0ppm

32 GC/MS ZB5 msi 30m x 0.25mm, 0.5μm film splitless 6 0.1-10

33 GC/MS DB-5 60m x 0.25mm, 0.25μm film on-column 6 1 ppb to 300 ppb

34 GC/MS-SIM ZB-5 60m x 0.25mm, 0.25μm film splitless 7 10 ng/mL to 20,000 ng/mL

*Units are those reported by the participating laboratory
52

Analytical methods used for Alkylated PAHs

Alkylated PAH mode of injection Calibration Curve

Lab # Instrument Phase Dimensions (split/splitless/on-column) # points range*

1 GC/MS DB-17MS 60m x 0.25mm, 0.25μm film on-column 6 varied by compound

2

3 GC/MS DB-5 60m x 0.25mm, 0.25μm film splitless 6 0.1 ug/mL to 4.0 ug/mL

4 GC/MS ZB-5MS 30m x 0.25mm, 0.25μm film split/splitless

5 GC/MS DB-5 60m x 0.25mm, 0.25μm film on-column 6 0.001ng/μL to 0.33 ng/μL

6

7 GC/MS DB-5 30m x 0.25mm, 0.25μm film on-column 7 10ng/mL to 4000ng/mL

8 GC/MS

Crossbond® silarylene phase; similar to 50% 

phenyl/50% dimethyl polysiloxane 30m x 0.25mm, 0.25μm film LVI/ solvent vent 6

1ng/mL to 500 ng/mL (0.2 ng/g to 

100ng/g)

9

10 GC/MS ZB-MS-5si 60m x 0.25mm, 0.25μm film 6 0.1 ug/mL to 4.0 ug/mL

11 GC/MS DB-5MS 60m x 0.25mm, 0.25μm film on-column 6 1 ng/mL to 300ng/mL

12 GC/MS ZB-5MSi 60m x 0.25mm, 0.25μm film splitless 6 0.008 ug/mL to 0.80 ug/mL

13 GC/MS DB-5 30m x 0.25mm, 0.25μm film 6 5 ng/mL to 1000 ng/mL

14 GC/MS Rxi-17 sil 60m x 0.25mm, 0.25μm film splitless 6 0.1 ng/g to 1000 ng/g

15 GC/MS DB-5 30m x 0.25mm, 0.25μm film splitless 6 0.05 mg/L to 5.0 mg/L

16 GC/MS DB-5 60m x 0.25mm, 0.25μm film splitless 7 0.01 to 7.2

17 GC/MS Rtx-5MS 30m x 0.32mm, 0.25μm film split 8 4ug/g to 1000ug/g

18 GC/MS DB-EUPAH CF 20m x 0.18mm, 0.14μm film pulsed splitless 6 0.5pg/uL to 100pg/uL

19 GC/MS 5% phenylpolydimethyl 60m x 0.25mm, 0.25μm film splitless 6 0.1 ug/mL to 4 ug/mL

20 GC/MS ZB5MSi 60m x 0.25mm, 0.25μm film 6 0.02 ug/L to 0.8 ug/L

21 GC/MS QQQ HP-5MS 30m x 0.25mm, 0.25μm film pulsed splitless 8 1ppb to 500 ppb

22 GC/MS RTX-5 30m x 0.25mm, 0.25μm film split/splitless 1 2000 ng/mL

23 GC/MS DB5-MS 30m x 0.25mm, 0.25μm film split/splitless 5 20ng/mL to 1000 ng/mL

24a GC/MS DB-5MS 60m x 0.25mm, 0.25μm film on-column 6 1 ng/mL to 330 ng/mL

24b

25 GC/MS ZB-5MSI 60m x 0.25mm, 0.25μm film pulsed splitless 6 0.1 ug/mL to 4.0ug/mL

26 GC/MS ZB-5MS 30m x 0.25mm, 0.25μm film splitless 10 2.0 ng/mL to 2000 ng/mL

27 GC/MS HP-5MS 60m x 0.25mm, 0.25μm film split 5 (20, 100, 250, 500,1000) ng/mL

28 GC/MS DB-5 60m x 0.25mm, 0.25μm film 6 3 ppm to 333 ppm

29 GC/MS DB-5MS 30m x 0.25mm, 0.25μm film PTV 6 10ng/mL to 5000ng/mL

30 GC/MS 5MS 30m x 0.25mm, 0.25μm film split/splitless 5 0.050 ug/mL to 10ug/mL

31 GC/MS ZB-5msi 60m x 0.25mm, 0.25μm film splitless 6 0.1ppm to 4.0ppm

32 GC/MS ZB5 msi 30m x 0.25mm, 0.5μm film splitless 6 0.1-10

33 GC/MS DB-5 60m x 0.25mm, 0.25μm film on-column 6 1ppb to 300 ppb

34 GC/MS-SIM ZB-5 60m x 0.25mm, 0.25μm film splitless 7 10 ng/mL to 20,000 ng/mL

*Units are those reported by the participating laboratory
53

Analytical methods used for Biomarkers

Biomarkers mode of injection Calibration Curve

Lab # Instrument Phase Dimensions (split/splitless/on-column) # points range*

1 GC/MS DB-17MS 60m x 0.25mm, 0.25μm film on-column 4 varied by compound

2

3 GC/MS DB-5 60m x 0.25mm, 0.25μm film splitless 6 0.1 ug/mL to 4.0 ug/mL

4

5

6

7

8

9

10 GC/MS ZB-MS-5si 60m x 0.25mm, 0.25μm film 6 0.1 ug/mL to 4.0 ug/mL

11

12 GC/MS ZB-5MSi 60m x 0.25mm, 0.25μm film splitless 6 0.008 ug/mL to 0.80 ug/mL

13

14 GC/MS Rxi-17 sil 60m x 0.25mm, 0.25μm film splitless 6 0.1 ng/g to 2000 ng/g

15 GC/MS DB-5 30m x 0.25mm, 0.25μm film splitless 1 SINTEF reference oil

16 GC/MS DB-5 60m x 0.25mm, 0.25μm film splitless 6 to 7 0.03 to 7.2 / 0.01 to 7.2

17 GC/MS Rtx-5MS 30m x 0.32mm, 0.25μm film split 8 4 ug/g to 1000 ug/g

18

19 GC/MS 5% phenylpolydimethyl 60m x 0.25mm, 0.25μm film splitless 6 0.1 ug/mL to 4 ug/mL

20 GC/MS ZB5MSi 60m x 0.25mm, 0.25μm film 6 0.02 ug/L to 0.8 ug/L

21

22 GC/MS RTX-5 30m x 0.25mm, 0.25μm film split/splitless 1 300 ng/mL to 11500ng/mL

23

24a

24b

25 GC/MS ZB-5MSI 60m x 0.25mm, 0.25μm film pulsed splitless 6 0.1 ug/mL to 4.0ug/mL

26

27

28

29

30

31 GC/MS ZB-5msi 60m x 0.25mm, 0.25μm film splitless 6 0.1ppm to 4.0ppm

32

33

34 GC/MS-SIM ZB-5 60m x 0.25mm, 0.25μm film splitless 6 10 ng/mL to 10,000 ng/mL

*Units are those reported by the participating laboratory
54

Quantification of PAHs

PAHs corrected for

Lab # IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery? others?

1

naphthalene-d8;biphenyl-d10; acenaphthalene-d10; phenanthrene-d10; fluoranthened10; pyrene-d10; B[a]A-d12; B[a]P-d12; perylene-d12; B[ghi]P-d12;DB[a,h]A-d14 x

2

3 Nitrobenzene-d5, 2-Fluorobiphenyl, Terphenyl-d14 Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, Chrysene-d10 x no

4 surrogates only Internal standards

5 NPH-d8, ACE-d10, BaP-d12 x HMB

PHN-d10 (prior to sizeexclusion LC)

6

7 Deuterated-Primary PAHs (16 total) x d10-2-Methylnaphthalene and d12-Benzo(e)pyrene

8 13C labeled EPA 16 PAH @10ng/g x

9

10 Nitrobenzene- d5; 2- Fluorobiphenyl; Terphenyl- d14 Naphthalene- d8; Acenapthene- d10; Chrysene- d12; Perylene- d12 x yes

11 Naphthalene-d8, Acenaphthene-d10 and Benzo[a]pyrene-d12 x

12 Naphthalene-d8, Acenaphtene-d10, Phenanthrene-d10, Chrysene-d12, Perylene-d12 Fluorene-d10, Benzo(a)pyrene-d12 x no

13

Acenaphthene-d10, Acenaphthylene-d8, Anthracene-d10, Benz[a]Anthracene-d12, 

Benzo[b]Fluoranthene-d12, Benzo[k]Fluoranthene-d12, Benzo[g,h,i]Perylene-d12, 

Benzo[a]Pyrene-d12, Chrysene-d12, Dibenz[a,h]Anthracene-d14, Fluoranthene-d10, 

Fluorene-d10, Indeno[l,2,3-cd]Pyrene-d12, Naphthalene-d8, Phenanthrene-d10, 

Pyrene-d10 x

14

Naphthalene-d8; Acenaphthene-d10; Phenanthrene-d10; Fluoranthene-d10; Pyrened10; Benz[a]anthracene-d12; Benzo[a]pyrene-d12; Perylene-d12; 

Bibenz[a,h]anthracene-d14; Benzo [[ghi]perylene-d12 x

15

naphthalene-d8, acenaphthylene-d8, phenanthrene-d10, pyrene-d10, benzo(a)pyrened12, benzo(ghi)perylene-d12 2-fluorobiphenyl, p-terphenyl-d14, chrysene-d12, dibenzo(ah)anthracene-d14 x

16 Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, Benzo(a)pyrene-d12 Fluorene-d10, Chrysene-d12 x yes

17

Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, 5 alpha-Androstane, 

Chrysene-d12, Perylene-d12 Fluorene-d10, Pyrene-d10, Benzo(a)pyrene-d12 x yes

18 Fluorene-d10, Fluoranthene-d10 Napthalene-d8, Acenaphthalene-d10, Phenanthrene-d10, Chrysene-d12, Perylene-d12 x no
55

Quantification of PAHs (cont)

PAHs corrected for

Lab # IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery?

19 surr - 2-fluorobiphenyl, nitrobenzene-d5, terphenyl-d14

IS - Naphthalene-d8, Acenaphthalene-d10, Phenanthrene-d10, Chrysene-d12, 

Perylene-d12 x no

20 Surrogates: Nitrobenzene-d5; 2-Fluorobiphenyl; Terphenyl-d14 Naphthalene-d8; Acenaphthene-d10; Phenanthrene-d10; Chrysene-d12; Perylene-d12

21 surrogates: Nitrobenzene-d5, 2-Fluorobiphenyl, Terphenyl-d14

Internal standards: Naphthalene-d8, Acenaphthene-d10, Phenathrene-d10, Chrysened12, Perylene-d12 x no

22

d8-naphthalene, d10-2-methylnaphthalene, d10-biphenyl, d12-2,6-

dimethylnaphthalene, d8-acenaphthylene, d10-phenanthrene, d10-fluoranthene, d12- 

benz[a]anthracene, d12-chrysene, d12-benzo[b,k]fluoranthenes, d12-benzo[a]pyrene, 

d12-perylene, d14-dibenz[a,h]anthracene, d12-indeno[123-cd]perylene, d12-

benzo(ghi)perylene x

d10-acenaphthene, d10-pyrene, d12-benzo[e]pyrene, used to quantify labeled 

surrogates only.

23 d8-Naphthalene, d10-Acenaphthene, d10-Phenanthrene, d12-Chrysene, d12-Perylene x d10-Fluorene, d12-Benzo(a)pyrene

24a Naphthalene-d8, Acenaphthene-d10, Benzo(a)-pyrene-d21 x Hexamethylbenzene

24b

25

2-Flourophenyl, phenol-d5, nitrobenzene-d5, 2,4,6-tribromophenol, Terphenyl-d14, 2-

Fluorobiphenyl

1,4-dichlorobenzene-d4, Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, 

Chrysene-d12, Perylene-d12 x yes

26 Fluorene-d10, Fluoranthene-d10, Terphenyl-d14 sur Naphthalene-d8, Acenapthene-d10, Phenanthrene-d10, Chrysene-d12, Perylene-d12 IS yes

27

SU-Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, Chrysene-d12, Perylened12 IS-Fluorene-d10, Pyrene-d10, Benzo(a)pyrene-d12 x yes

28 naphthalene-d8; acenaphthene-d10; benzo[a]pyrene-d12 x hexamethylbenzene

phenanthrene-d10 (prior 

to size-exclusion LC)

29

d8-Napthalene, d8-1-Methylnapthalene, d8-Acenaphthylene, d10-Acenaphthene, d10-

Fluorene, d8-Dibenzothiophene, 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-Benzo(g,h,i)perylene x d14-p-terphenyl

30 2-fluorobiphenyl, terphenyl d14 naph d8, acenaph d10, phenan d10, chry d12, pery d12 x no

31 Nitrobenzene-d5, 2-fluorobiphenyl, Terphenyl-d-14 x Naphthalene-d8, acenaphthalene-d10, phenanthrene-d10, chrysene-d12, perylene-d12

32 d8-Naphthalene, d10-Acenaphthene, d10-Phenanthrene, d12-Chrysene, d12-Perylene d10-Fluorene, d10-Pyrene, d12-Benzo(a)pyrene x no

33 D8Napthalene, D10Acenapthene, D12 BAP x Hexamethylbenzene

34 Surrogates: Naphthalene-d8, Phenanthrene-d10, Benzo[a]pyrene-d12, 5b(H)Cholane x IS: Acenaphthene-d10, Chrysene-d12 x yes
56

Quantification of Alkylated PAHs

Alkylated PAHs corrected for

Lab # IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery? others?

1

naphthalene-d8;biphenyl-d10; acenaphthalene-d10; phenanthrene-d10; fluoranthened10; pyrene-d10; B[a]A-d12; B[a]P-d12; perylene-d12; B[ghi]P-d12;DB[a,h]A-d14 x

2

3 Nitrobenzene-d5, 2-Fluorobiphenyl, Terphenyl-d14 Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, Chrysene-d10 x no

4 surrogates only Internal standards

5 NPH-d8, ACE-d10, BaP-d12 HMB

PHN-d10 (prior to sizeexclusion LC)

6 x

7 Deuterated-Primary PAHs (16 total) x d10-2-Methylnaphthalene and d12-Benzo(e)pyrene

8 13C labeled EPA 16 PAH @10ng/g x

9

10 Nitrobenzene- d5; 2- Fluorobiphenyl; Terphenyl- d14 Naphthalene- d8; Acenapthene- d10; Chrysene- d12; Perylene- d12 x yes

11 Naphthalene-d8, Acenaphthene-d10 and Benzo[a]pyrene-d12 x

12 Naphthalene-d8, Acenaphtene-d10, Phenanthrene-d10, Chrysene-d12, Perylene-d12 Fluorene-d10, Benzo(a)pyrene-d12 x no

13

14 Naphthalene-d8, Phenanthrene-d10, Fluoranthene-d10 x

15

naphthalene-d8, acenaphthylene-d8, phenanthrene-d10, pyrene-d10, benzo(a)pyrened12, benzo(ghi)perylene-d12 2-fluorobiphenyl, p-terphenyl-d14, chrysene-d12, dibenzo(ah)anthracene-d14 x

16 Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, Benzo(a)pyrene-d12 Fluorene-d10, Chrysene-d12 x yes

17

Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, 5 alpha-Androstane, 

Chrysene-d12, Perylene-d12 Fluorene-d10, Pyrene-d10, Benzo(a)pyrene-d12 x yes

18 1-methyl Napthalene-d10 x no
57

Quantification of Alkylated PAHs (cont)

Alkylated PAHs corrected for

Lab # IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery?

19 surr - 2-fluorobiphenyl, nitrobenzene-d5, terphenyl-d14

IS - Naphthalene-d8, Acenaphthalene-d10, Phenanthrene-d10, Chrysene-d12, 

Perylene-d12 x no

20 Surrogates: Nitrobenzene-d5; 2-Fluorobiphenyl; Terphenyl-d14 Naphthalene-d8; Acenaphthene-d10; Phenanthrene-d10; Chrysene-d12; Perylene-d12

21 surrogates: Nitrobenzene-d5, 2-Fluorobiphenyl, Terphenyl-d14

Internal standards: Naphthalene-d8, Acenaphthene-d10, Phenathrene-d10, Chrysened12, x no

22

d10-2-methylnaphthalene, d12-2,6-dimethylnaphthalene, d8-acenaphthylene, d10-

phenanthrene, d10-fluoranthene, d12-chrysene x

d10-acenaphthene, d10-pyrene, d12-benzo[e]pyrene, used to quantify labeled 

surrogates only.

23 d8-Naphthalene, d10-Acenaphthene, d10-Phenanthrene, d12-Chrysene, d12-Perylene x d10-Fluorene, d12-Benzo(a)pyrene

24a Naphthalene-d8, Acenaphthene-d10, Benzo(a)-pyrene-d21 x Hexamethylbenzene

24b

25

2-Flourophenyl, phenol-d5, nitrobenzene-d5, 2,4,6-tribromophenol, Terphenyl-d14, 2-

Fluorobiphenyl

1,4-dichlorobenzene-d4, Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, 

Chrysene-d12, Perylene-d12 x yes

26 Fluorene-d10, Fluoranthene-d10, Terphenyl-d14 sur Naphthalene-d8, Acenapthene-d10, Phenanthrene-d10, Chrysene-d12, Perylene-d12 IS yes

27

SU-Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, Chrysene-d12, Perylened12 IS-Fluorene-d10, Pyrene-d10, Benzo(a)pyrene-d12 x yes

28 naphthalene-d8; acenaphthene-d10; benzo[a]pyrene-d12 x hexamethylbenzene

phenanthrene-d10 (prior 

to size-exclusion LC)

29

d8-Napthalene, d8-1-Methylnapthalene, d10-Acenaphthene, d10-Fluorene, d8-

Dibenzothiophene, d10-Anthracene, d10-Fluoranthene, d12-Chrysene, d12-

Benzo(e)pyrene x d14-p-terphenyl

30 2-fluorobiphenyl, terphenyl d14 naph d8, acenaph d10, phenan d10, chry d12, pery d12 x no

31 Nitrobenzene-d5, 2-fluorobiphenyl, Terphenyl-d-14 x Naphthalene-d8, acenaphthalene-d10, phenanthrene-d10, chrysene-d12, perylene-d12

32 d8-Naphthalene, d10-Acenaphthene, d10-Phenanthrene, d12-Chrysene, d12-Perylene d10-Fluorene, d10-Pyrene, d12-Benzo(a)pyrene x no

33 D8Napthalene, D10Acenapthene, D12 BAP x

34 Surrogates: Naphthalene-d8, Phenanthrene-d10, Benzo[a]pyrene-d12, 5b(H)Cholane x IS: Acenaphthene-d10, Chrysene-d12 x yes
58

Quantification of Biomarkers

Biomarkers corrected for

Lab # IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery? others?

1

naphthalene-d8;biphenyl-d10; acenaphthalene-d10; phenanthrene-d10; fluoranthened10; pyrene-d10; B[a]A-d12; B[a]P-d12; perylene-d12; B[ghi]P-d12;DB[a,h]A-d14 x

2

3 Nitrobenzene-d5, 2-Fluorobiphenyl, Terphenyl-d14 Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, Chrysene-d10 x no

4

5

6

7

8

9

10 Nitrobenzene- d5; 2- Fluorobiphenyl; Terphenyl- d14 Naphthalene- d8; Acenapthene- d10; Chrysene- d12; Perylene- d12 x yes

11

12 Naphthalene-d8, Acenaphtene-d10, Phenanthrene-d10, Chrysene-d12, Perylene-d12 Fluorene-d10, Benzo(a)pyrene-d12 x no

13

14 n-triacontane-d62 x

15

16 5b(H)-Cholane Chrysene-d12 x yes

17

Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, 5 alpha-Androstane, 

Chrysene-d12, Perylene-d12 Fluorene-d10, Pyrene-d10, Benzo(a)pyrene-d12 x yes

18
59

Quantification of Biomarkers (cont)

Biomarkers corrected for

Lab # IS/surrogate added prior to extraction Used? added prior to analysis Used? recovery?

19 surr - 2-fluorobiphenyl, nitrobenzene-d5, terphenyl-d14

IS - Naphthalene-d8, Acenaphthalene-d10, Phenanthrene-d10, Chrysene-d12, 

Perylene-d12 x no

20 Surrogates: Nitrobenzene-d5; 2-Fluorobiphenyl; Terphenyl-d14 Naphthalene-d8; Acenaphthene-d10; Phenanthrene-d10; Chrysene-d12; Perylene-d12

21

22 d10-phenanthrene, d50-tetracosane x d10-pyrene, used to quantify labeled surrogates only

23

24

25

2-Flourophenyl, phenol-d5, nitrobenzene-d5, 2,4,6-tribromophenol, Terphenyl-d14, 2-

Fluorobiphenyl

1,4-dichlorobenzene-d4, Naphthalene-d8, Acenaphthene-d10, Phenanthrene-d10, 

Chrysene-d12, Perylene-d12 x yes

26 Fluorene-d10, Fluoranthene-d10, Terphenyl-d14 sur Naphthalene-d8, Acenapthene-d10, Phenanthrene-d10, Chrysene-d12, Perylene-d12 IS yes

27

28

29

30

31 Nitrobenzene-d5, 2-fluorobiphenyl, Terphenyl-d-14 x Naphthalene-d8, acenaphthalene-d10, phenanthrene-d10, chrysene-d12, perylene-d12

32

33

34 Surrogates: Naphthalene-d8, Phenanthrene-d10, Benzo[a]pyrene-d12, 5b(H)Cholane x IS: Acenaphthene-d10, Chrysene-d12 x yes
60

PAHs - IS/surrogate used for quantitation

Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6

naphthalene naphthalene-d8 Naphthalene-d8 Naphthalene-D8 NPH-d8

biphenyl biphenyl-d10 Naphthalene-d8 Naphthalene-D8 ACE-d10

acenaphthene acenaphthene-d10 Acenaphthene-d10 Acenapthene-D10 ACE-d10

acenaphthylene acenaphthene-d10 Acenaphthene-d10 Acenapthene-D10 ACE-d10

fluorene phenanthrene-d10 Acenaphthene-d10 Acenapthene-D10 ACE-d10

phenanthrene phenanthrene-d10 Phenanthrene-d10 Phenanthrene-D10 ACE-d10

anthracene phenanthrene-d10 Phenanthrene-d10 Phenanthrene-D10 ACE-d10

fluoranthene fluoranathene-d10 Phenanthrene-d10 Phenanthrene-D10 BaP-d12

pyrene pyrene-d10 Chrysene-d12 Chrysene-D12 BaP-d12

benzo[b]fluorene NA NA Perylene-D12

benz[a]anthracene B[a]A-d12 Chrysene-d12 Chrysene-D12 BaP-d12

chrysene B[a]A-d12 Chrysene-d12 Chrysene-D12 BaP-d12

triphenylene B[a]A-d12 NA

benzo[b ]fluoranthene B[a]P-d12 Chrysene-d12 Perylene-D12 BaP-d12

benzo[j ]fluoranthene B[a]P-d12 NA

benzo[k ]fluoranthene B[a]P-d12 Chrysene-d12 Perylene-D12 BaP-d12

benzo[a]fluoranthene B[a]P-d12 NA Perylene-D12

benzo[e]pyrene B[a]P-d12 Chrysene-d12 Perylene-D12 BaP-d12

benzo[a]pyrene B[a]P-d12 Chrysene-d12 Perylene-D12 BaP-d12

perylene perylene-d12 Chrysene-d12 Perylene-D12 BaP-d12

indeno[1,2,3-cd]pyrene B[ghi]P-d12 Chrysene-d12 Perylene-D12 BaP-d12

benzo[ghi]perylene B[ghi]P-d12 Chrysene-d12 Perylene-D12 BaP-d12

dibenz[a,h]anthracene DB[a,h]A-d14 Chrysene-d12 Perylene-D12 BaP-d12

cis/trans-decalin NA NA Naphthalene-D8

dibenzofuran NA Acenaphthene-d10 Acenapthene-D10

retene NA NA Chrysene-D12 ACE-d10

benzothiophene NA NA Naphthalene-D8

dibenzothiophene fluoranathene-d10 Acenaphthene-d10 Phenanthrene-D10 ACE-d10

naphthobenzothiophene NA NA Chrysene-D12
61

PAHs - IS/surrogate used for quantitation

Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12

naphthalene d8-Naphthalene 13C naphthalene Napthalene- d8 Naphthalene-d8 Fluorene-d10

biphenyl d10-Acenaphthylene NA Acenapthene- d10 Fluorene-d10

acenaphthene d10-Acenaphthene 13C acenaphthene Acenapthene- d10 Fluorene-d10

acenaphthylene d10-Acenaphthylene 13C acenaphthylene Acenapthene- d10 Fluorene-d10

fluorene d10-Fluorene 13C Fluorene Acenapthene- d10 Acenaphthene-d10 Fluorene-d10

phenanthrene d10-Phenanthrene 13C phenathrene Phananthrene- d10 Acenaphthene-d10 Fluorene-d10

anthracene d10-Anthracene 13C anthracene Phananthrene- d10 Acenaphthene-d10 Fluorene-d10

fluoranthene d10-Fluoranthene 13C Fluoranthen Phananthrene- d10 Acenaphthene-d10 Fluorene-d10

pyrene d10-Pyrene 13C pyrene Chyrsene- 12 Acenaphthene-d10 Benzo(a)pyrene-d12

benzo[b]fluorene NA NA Benzo(a)pyrene-d12

benz[a]anthracene d12-Benz[a]anthracene 13C ben[a]anthracene Chyrsene- 12 Benzo[a]pyrene-d12 Benzo(a)pyrene-d12

chrysene d12-Chrysene 13C chrysene Chyrsene- 12 Benzo[a]pyrene-d12 Benzo(a)pyrene-d12

triphenylene NA NA

benzo[b ]fluoranthene d12-Benzo[b ]fluoranthene 13C benzo[b]fluoranthene Chyrsene- 12 Benzo[a]pyrene-d12 Benzo(a)pyrene-d12

benzo[j ]fluoranthene NA NA

benzo[k ]fluoranthene d12-Benzo[k ]fluoranthene 13C benzo[k]fluoranthene Chyrsene- 12 Benzo[a]pyrene-d12 Benzo(a)pyrene-d12

benzo[a]fluoranthene NA NA

benzo[e]pyrene d12-Benzo[a]pyrene 13C benzo[a]pyrene Chyrsene- 12 Benzo(a)pyrene-d12

benzo[a]pyrene d12-Benzo[a]pyrene 13C benzo[a]pyrene Chyrsene- 12 Benzo[a]pyrene-d12 Benzo(a)pyrene-d12

perylene d12-Benzo[a]pyrene NA Chyrsene- 12 Benzo(a)pyrene-d12

indeno[1,2,3-cd]pyrene d12-Indeno[1,2,3-cd]pyrene 13C indeno[1,2,3-cd]pyrene Chyrsene- 12 Benzo[a]pyrene-d12 Benzo(a)pyrene-d12

benzo[ghi]perylene d12-Benzo[ghi]perylene 13C benzo[ghi]perylene Chyrsene- 12 Benzo(a)pyrene-d12

dibenz[a,h]anthracene d14-Dibenz[a,h]anthracene 13C dibenz[a,h]anthracene Chyrsene- 12 Benzo[a]pyrene-d12 Benzo(a)pyrene-d12

cis/trans-decalin NA NA Fluorene-d10

dibenzofuran NA NA Fluorene-d10

retene NA NA

benzothiophene d8-Naphthalene NA NA Fluorene-d10

dibenzothiophene d10-Fluorene NA Phananthrene- d10 Fluorene-d10

naphthobenzothiophene NA NA Benzo(a)pyrene-d12
62

PAHs - IS/surrogate used for quantitation

Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18

naphthalene naphthalene-d8 2-fluorobiphenyl Fluorene-d10 / Naphthalene-d8 Fluorene-d10 / Naphthalene-d8 Naphthalene-d8

biphenyl naphthalene-d8 2-fluorobiphenyl Fluorene-d10 / Acenaphthene-d10 Fluorene-d10 / Acenaphthene-d10 Naphthalene-d8

acenaphthene acenaphthene-d10 napthalene-d8 2-fluorobiphenyl Fluorene-d10 / Acenaphthene-d10 Fluorene-d10 / Acenaphthene-d10 Acenaphthene-d10

acenaphthylene acenaphthylene-d8 napthalene-d8 2-fluorobiphenyl Fluorene-d10 / Acenaphthene-d10 Fluorene-d10 / Acenaphthene-d10 Naphthalene-d8

fluorene fluorene-d10 napthalene-d8 2-fluorobiphenyl Fluorene-d10 / Acenaphthene-d10 Fluorene-d10 / Acenaphthene-d10 Acenaphthene-d10

phenanthrene phenanthrene-d10 phenanthrene-d10 2-fluorobiphenyl Fluorene-d10 / Phenanthrene-d10 Pyrene-d10 / Phenanthrene-d10 Phenanthrene-d10

anthracene anthracene-d10 phenanthrene-d10 2-fluorobiphenyl Fluorene-d10 / Phenanthrene-d10 Pyrene-d10 / Phenanthrene-d10 Phenanthrene-d10

fluoranthene fluoranthene-d10 fluoranthene-d10 p-terphenyl-d14 Fluorene-d10 / Phenanthrene-d10 Pyrene-d10 / Chrysene-d12 Phenanthrene-d10

pyrene pyrene-d10 pyrene-d10 p-terphenyl-d14 Fluorene-d10 / Phenanthrene-d10 Pyrene-d10 / Chrysene-d12 Phenanthrene-d10

benzo[b]fluorene NA Pyrene-d10 / Chrysene-d12

benz[a]anthracene benz[a]anthracene-d12 benz[a]anthracene-d12 chrysene-d12 Chrysene-d12 / Phenanthrene-d10 Pyrene-d10 / Chrysene-d12 Phenanthrene-d10

chrysene chrysene-d12 benz[a]anthracene-d12 chrysene-d12 Chrysene-d12 / Phenanthrene-d10 Pyrene-d10 / Chrysene-d12 Chrysene-d12

triphenylene benz[a]anthracene-d12 NA Pyrene-d10 / Chrysene-d12 Chrysene-d12

benzo[b ]fluoranthene benzo[b ]fluoranthene-d12 benzo[a]pyrene-d12 chrysene-d12

Chrysene-d12 / Benzo(a)pyrened12Benzo(a)pyrene-d12 / Perylened12 Chrysene-d12

benzo[j ]fluoranthene benzo[a]pyrene-d12 chrysene-d12

Benzo(a)pyrene-d12 / Perylened12

benzo[k ]fluoranthene benzo[k ]fluoranthene-d12 benzo[a]pyrene-d12 chrysene-d12

Chrysene-d12 / Benzo(a)pyrened12Benzo(a)pyrene-d12 / Perylened12 Chrysene-d12

benzo[a]fluoranthene benzo[a]pyrene-d12 NA

Benzo(a)pyrene-d12 / Perylened12

benzo[e]pyrene benzo[k ]fluoranthene-d12 benzo[a]pyrene-d12 NA

Chrysene-d12 / Benzo(a)pyrened12Benzo(a)pyrene-d12 / Perylened12 Chrysene-d12

benzo[a]pyrene benzo[a]pyrene-d12 benzo[a]pyrene-d12 chrysene-d12

Chrysene-d12 / Benzo(a)pyrened12Benzo(a)pyrene-d12 / Perylened12 Chrysene-d12

perylene benzo[a]pyrene-d12 perylene-d12 chrysene-d12

Chrysene-d12 / Benzo(a)pyrened12Benzo(a)pyrene-d12 / Perylened12 Perylene-d12

indeno[1,2,3-cd]pyrene indeno[1,2,3-cd]pyrene-d12 benzo[ghi]perylene-d12 dibenzo(ah)anthracene-d14

Chrysene-d12 / Benzo(a)pyrened12Benzo(a)pyrene-d12 / Perylened12 Perylene-d12

benzo[ghi]perylene benzo[ghi]perylene-d12 perylene-d12 dibenzo(ah)anthracene-d14

Chrysene-d12 / Benzo(a)pyrened12Benzo(a)pyrene-d12 / Perylened12 Perylene-d12

dibenz[a,h]anthracene dibenz[a,h]anthracene-d14 dibenz[a,h]anthracene-d14 dibenzo(ah)anthracene-d14

Chrysene-d12 / Benzo(a)pyrened12Benzo(a)pyrene-d12 / Perylened12 Perylene-d12

cis/trans-decalin NA Fluorene-d10 / Naphthalene-d8 Fluorene-d10 / Naphthalene-d8

dibenzofuran acenaphthylene-d8 NA Fluorene-d10 / Acenaphthene-d10 Fluorene-d10 / Acenaphthene-d10

retene fluoranthene-d10 p-terphenyl-d14 Fluorene-d10 / Phenanthrene-d10 Pyrene-d10 / Chrysene-d12

benzothiophene NA Fluorene-d10 / Acenaphthene-d10 Fluorene-d10 / Naphthalene-d8

dibenzothiophene fluorene-d10 phenanthrene-d10 p-terphenyl-d14 Fluorene-d10 / Phenanthrene-d10 Pyrene-d10 / Phenanthrene-d10 Acenaphthene-d10

naphthobenzothiophene NA Fluorene-d10 / Phenanthrene-d10 Pyrene-d10 / Chrysene-d12
63

PAHs - IS/surrogate used for quantitation

Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24a Lab 24b

naphthalene Naphthalene-d8 Naphthalene-d8 naphthalene-d8 d8-naphthalene d8-Naphthalene NA

biphenyl Naphthalene-d8 Acenaphthene-d10 d10-biphenyl d10-Acenaphthene NA

acenaphthene Acenaphthalene-d10 Acenaphthene-d10 acenaphthene-d10 d8-acenaphthylene d10-Acenaphthene NA

acenaphthylene Acenaphthalene-d10 Acenaphthene-d10 acenaphthene-d10 d8-acenaphthylene d10-Acenaphthene Acenaphthene-d10

fluorene Acenaphthalene-d10 Acenaphthene-d10 acenaphthene-d10 d10-phenanthrene d10-Acenaphthene Acenaphthene-d10

phenanthrene Phenanthrene-d10 Phenanthrene-d10 phenanthrene-d10 d10-phenanthrene d10-Phenanthrene Acenaphthene-d10

anthracene Phenanthrene-d10 Phenanthrene-d10 phenanthrene-d10 d10-phenanthrene d10-Phenanthrene Acenaphthene-d10

fluoranthene Phenanthrene-d10 Phenanthrene-d10 phenanthrene-d10 d10-fluoranthene d10-Phenanthrene Acenaphthene-d10

pyrene Chrysene-d12 Chrysene-d12 chrysene-d12 d10-fluoranthene d10-Phenanthrene Acenaphthene-d10

benzo[b]fluorene __________ NA Benzo(a)pyrene-d12

benz[a]anthracene Chrysene-d12 Chrysene-d12 chrysene-d12 d12-benz[a]anthracene d12-Chrysene Benzo(a)pyrene-d12

chrysene Chrysene-d12 Chrysene-d12 chrysene-d12 d12-chrysene d12-Chrysene NA

triphenylene __________ other Benzo(a)pyrene-d12

benzo[b ]fluoranthene Chrysene-d12 Chrysene-d12 perylene-d12 d12-benzo[b]fluoranthene d12-Chrysene NA

benzo[j ]fluoranthene __________ other Benzo(a)pyrene-d12

benzo[k ]fluoranthene Chrysene-d12 Chrysene-d12 perylene-d12 d12-benzo[k]fluoranthene d12-Chrysene NA

benzo[a]fluoranthene __________ NA NA

benzo[e]pyrene Chrysene-d12 Chrysene-d12 d12-benzo[a]pyrene d12-Chrysene Benzo(a)pyrene-d12

benzo[a]pyrene Chrysene-d12 Chrysene-d12 perylene-d12 d12-benzo[a]pyrene d12-Chrysene NA

perylene Chrysene-d12 Chrysene-d12 d12-perylene d12-Perylene Benzo(a)pyrene-d12

indeno[1,2,3-cd]pyrene Chrysene-d12 Chrysene-d12 perylene-d12 d12-indeno[1,2,3-cd]pyrene d12-Chrysene NA

benzo[ghi]perylene Chrysene-d12 Chrysene-d12 perylene-d12 d12-benzo[ghi]perylene d12-Chrysene Benzo(a)pyrene-d12

dibenz[a,h]anthracene Chrysene-d12 Chrysene-d12 perylene-d12 d14-dibenz[a,h]anthracene d12-Chrysene NA

cis/trans-decalin __________ NA NA

dibenzofuran Acenaphthalene-d10 Acenaphthene-d10 NA NA

retene __________ d10-fluoranthene NA

benzothiophene __________ NA NA

dibenzothiophene Acenaphthalene-d10 Phenanthrene-d10 d10-phenanthrene d10-Phenanthrene NA

naphthobenzothiophene __________ NA
64

PAHs - IS/surrogate used for quantitation

Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30

naphthalene Naphthalene-d8 Naphthalene-d8/Fluorene-d10 Fluorene-d10/Naphthalene-d8 naphthalene-d8 d8-Naphthalene naphthalene d8

biphenyl Naphthalene-d8 Naphthalene-d8/Fluorene-d10 Fluorene-d10/Acenaphthene-d10 d8-1-Methylnaphthalene naphthalene d8

acenaphthene Acenaphthene-d10 Acenaphthene-d10/Fluorene-d10 Fluorene-d10/Acenaphthene-d10 d10Acenapthene acenaphthene d10

acenaphthylene Acenaphthene-d10 Acenaphthene-d10/Fluorene-d10 Fluorene-d10/Acenaphthene-d10 d8-Acenapthylene acenaphthene d10

fluorene Acenaphthene-d10 Acenaphthene-d10/Fluorene-d10 Fluorene-d10/Acenaphthene-d10 acenaphthene-d10 d10-Fluorene acenaphthene d10

phenanthrene Phenanthrene-d10

Phenanthrene-d10/Fluoranthened10 Pyrene-d10/Phenanthrene-d10 acenaphthene-d10 d10-Phenanthrene phenanthrene d10

anthracene Phenanthrene-d10

Phenanthrene-d10/Fluoranthened10 Pyrene-d10/Phenanthrene-d10 acenaphthene-d10 d10-Anthracene phenanthrene d10

fluoranthene Phenanthrene-d10

Phenanthrene-d10/Fluoranthened10 Pyrene-d10/Phenanthrene-d10 acenaphthene-d10 d10-Fluoranthene phenanthrene d10

pyrene Chrysene-d12 Chrysene-d12/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 acenaphthene-d10 d10-Pyrene phenanthrene d10

benzo[b]fluorene Chrysene-d12 Chrysene-d12/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 d12-Benzo(b)fluoranthene phenanthrene d10

benz[a]anthracene Chrysene-d12 Chrysene-d12/Terphenyl-d14 Pyrene-d10/Chrysene-d12 benzo[a]pyrene-d12 d12-Benz(a)anthracene chrysene d12

chrysene Chrysene-d12 Chrysene-d12/Terphenyl-d14 Pyrene-d10/Chrysene-d12 benzo[a]pyrene-d12 d12-Chrysene chrysene d12

triphenylene Chrysene-d12/Terphenyl-d14 NA d12-Chrysene NA

benzo[b ]fluoranthene Chrysene-d12 Perylene-d12Terphenyl-d14

Benzo(a)pyrene-d12/Chrysened12 benzo[a]pyrene-d12 d12-Benzo(b)fluoranthene perylene d12

benzo[j ]fluoranthene Perylene-d12Terphenyl-d14

Benzo(a)pyrene-d12/Chrysened12 d12-Benzo(k)fluoranthene perylene d12

benzo[k ]fluoranthene Chrysene-d12 Perylene-d12Terphenyl-d14 NA benzo[a]pyrene-d12 d12-Benzo(k)fluoranthene perylene d12

benzo[a]fluoranthene Perylene-d12Terphenyl-d14

Benzo(a)pyrene-d12/Chrysened12 d12-Benzo(e)pyrene NA

benzo[e]pyrene Chrysene-d12 Perylene-d12Terphenyl-d14

Benzo(a)pyrene-d12/Chrysened12 d12-Benzo(e)pyrene perylene d12

benzo[a]pyrene Chrysene-d12 Perylene-d12Terphenyl-d14

Benzo(a)pyrene-d12/Chrysened12 benzo[a]pyrene-d12 d12benzo(a)pyrene perylene d12

perylene Chrysene-d12 Perylene-d12Terphenyl-d14 Benzo(a)pyrene-d12/Perylene-d12 d12-perylene perylene d12

indeno[1,2,3-cd]pyrene Chrysene-d12 Perylene-d12Terphenyl-d14

Benzo(a)pyrene-d12/Chrysened12 benzo[a]pyrene-d12 d12-benzo(ghi)perylene perylene d12

benzo[ghi]perylene Chrysene-d12 Perylene-d12Terphenyl-d14

Benzo(a)pyrene-d12/Chrysened12 d12-benzo(ghi)perylene perylene d12

dibenz[a,h]anthracene Chrysene-d12 Perylene-d12Terphenyl-d14

Benzo(a)pyrene-d12/Chrysened12 benzo[a]pyrene-d12 d12-benzo(ghi)perylene perylene d12

cis/trans-decalin Naphthalene-d8/Fluorene-d10 Fluorene-d10/Naphthalene-d8 d8-Naphthalene naphthalene d8

dibenzofuran Acenaphthene-d10 Acenaphthene-d10/Fluorene-d10 Fluorene-d10/Acenaphthene-d10 d10-Acenapthene acenaphthene d10

retene Chrysene-d12/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 d10-Pyrene NA

benzothiophene Naphthalene-d8/Fluorene-d10 Fluorene-d10/Acenaphthene-d10 d8-Naphthalene naphthalene d8

dibenzothiophene Acenaphthene-d10

Phenanthrene-d10/Fluoranthened10 Pyrene-d10/Phenanthrene-d10 d10-Phenanthrene acenaphthene d10

naphthobenzothiophene Chrysene-d12/Terphenyl-d14 Pyrene-d10/Phenanthrene-d10
65

PAHs - IS/surrogate used for quantitation

Lab 31 Lab 32 Lab 33 Lab 34

naphthalene d10-Fluorene D8 Napthalene Acenaphthene-d10

biphenyl d10-Fluorene D10 Acenapthene Acenaphthene-d10

acenaphthene d10-Fluorene D12 Benzo a pyrene Acenaphthene-d10

acenaphthylene d10-Fluorene Acenaphthene-d10

fluorene d10-Fluorene Acenaphthene-d10

phenanthrene d10-Fluorene Acenaphthene-d10

anthracene d10-Fluorene Acenaphthene-d10

fluoranthene d10-Pyrene Acenaphthene-d10

pyrene d10-Pyrene Acenaphthene-d10

benzo[b]fluorene Acenaphthene-d10

benz[a]anthracene d12-Benzo(a)pyrene Chrysene-d12

chrysene d12-Benzo(a)pyrene Chrysene-d12

triphenylene Chrysene-d12

benzo[b ]fluoranthene Chrysene-d12

benzo[j ]fluoranthene Chrysene-d12

benzo[k ]fluoranthene d12-Benzo(a)pyrene Chrysene-d12

benzo[a]fluoranthene Chrysene-d12

benzo[e]pyrene d12-Benzo(a)pyrene Chrysene-d12

benzo[a]pyrene d12-Benzo(a)pyrene Chrysene-d12

perylene d12-Benzo(a)pyrene Chrysene-d12

indeno[1,2,3-cd]pyrene d12-Benzo(a)pyrene Chrysene-d12

benzo[ghi]perylene d12-Benzo(a)pyrene Chrysene-d12

dibenz[a,h]anthracene d12-Benzo(a)pyrene Chrysene-d12

cis/trans-decalin d10-Fluorene Acenaphthene-d10

dibenzofuran d10-Fluorene Acenaphthene-d10

retene d10-Pyrene Acenaphthene-d10

benzothiophene d10-Fluorene Acenaphthene-d10

dibenzothiophene d10-Fluorene Acenaphthene-d10

naphthobenzothiophene d10-Pyrene Acenaphthene-d10
66

Alkylated PAHs - IS/surrogate used for quantitation

Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6

1-methylnaphthalene naphthalene-d8 Naphthalene-d8 Naphthalene-D8 NPH-d8

2-methylnaphthalene naphthalene-d8 Naphthalene-d8 Naphthalene-D8 NPH-d8

2,6-dimethylnaphthalene naphthalene-d8 Naphthalene-d8 Naphthalene-D8 ACE-d10

1,6,7-trimethylnaphthalene naphthalene-d8 Acenaphthene-d10 Naphthalene-D8 ACE-d10

1-methylphenanthrene phenanthrene-d10 Phenanthrene-d10 Phenanthrene-D10 ACE-d10

C1-decalins NA NA Naphthalene-D8

C2-decalins NA NA Naphthalene-D8

C3-decalins NA NA Naphthalene-D8

C4-decalins NA NA Naphthalene-D8

C1-naphthalenes naphthalene-d8 Naphthalene-d8 Naphthalene-D8 ACE-d10

C2-naphthalenes naphthalene-d8 Naphthalene-d8 Naphthalene-D8 ACE-d10

C3-naphthalenes naphthalene-d8 Naphthalene-d8 Naphthalene-D8 ACE-d10

C4-naphthalenes naphthalene-d8 Naphthalene-d8 Naphthalene-D8 ACE-d10

C1-benzothiophenes NA NA Naphthalene-D8

C2-benzothiophenes NA NA Naphthalene-D8

C3-benzothiophenes NA NA Naphthalene-D8

C4-benzothiophenes NA NA Naphthalene-D8

C1-fluorenes phenanthrene-d10 Acenaphthene-d10 Acenapthene-D10 ACE-d10

C2-fluorenes phenanthrene-d10 Acenaphthene-d10 Acenapthene-D10 ACE-d10

C3-fluorenes phenanthrene-d10 Acenaphthene-d10 Acenapthene-D10 ACE-d10

C1-phenanthrenes/anthracenes phenanthrene-d10 Phenanthrene-d10 Phenanthrene-D10 ACE-d10

C2-phenanthrenes/anthracenes phenanthrene-d10 Phenanthrene-d10 Phenanthrene-D10 ACE-d10

C3-phenanthrenes/anthracenes phenanthrene-d10 Phenanthrene-d10 Phenanthrene-D10 ACE-d10

C4-phenanthrenes/anthracenes phenanthrene-d10 Phenanthrene-d10 Phenanthrene-D10 ACE-d10

C1-dibenzothiophenes phenanthrene-d10 Acenaphthene-d10 Phenanthrene-D10 ACE-d10

C2-dibenzothiophenes phenanthrene-d10 Acenaphthene-d10 Phenanthrene-D10 ACE-d10

C3-dibenzothiophenes phenanthrene-d10 Acenaphthene-d10 Phenanthrene-D10 ACE-d10

C4-dibenzothiophenes phenanthrene-d10 Acenaphthene-d10 Phenanthrene-D10 ACE-d10

C1-fluoranthenes/pyrenes fluoranthene-d10 Chrysene-d12 Phenanthrene-D10 BaP-d12

C2-fluoranthenes/pyrenes fluoranthene-d10 Chrysene-d12 Phenanthrene-D10 BaP-d12

C3-fluoranthenes/pyrenes fluoranthene-d10 Chrysene-d12 Phenanthrene-D10 BaP-d12

C4-fluoranthenes/pyrenes fluoranthene-d10 NA Phenanthrene-D10 BaP-d12

C1-naphthobenzothiophenes NA NA Chrysene-D12 ACE-d10

C2-naphthobenzothiophenes NA NA Chrysene-D12 ACE-d10

C3-naphthobenzothiophenes NA NA Chrysene-D12 ACE-d10

C4-naphthobenzothiophenes NA NA Chrysene-D12 ACE-d10

C1-chrysenes B[a]A-d12 Chrysene-d12 Chrysene-D12 BaP-d12

C2-chrysenes B[a]A-d12 Chrysene-d12 Chrysene-D12 BaP-d12

C3-chrysenes B[a]A-d12 Chrysene-d12 Chrysene-D12 BaP-d12

C4-chrysenes B[a]A-d12 Chrysene-d12 Chrysene-D12 BaP-d12
67

Alkylated PAHs - IS/surrogate used for quantitation

Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12

1-methylnaphthalene d8-Naphthalene 13C Acenaphthylene Napthalene- d8 Naphthalene-d8 Fluorene-d10

2-methylnaphthalene d8-Naphthalene 13C Acenaphthylene Napthalene- d8 Naphthalene-d8 Fluorene-d10

2,6-dimethylnaphthalene 13C Acenaphthylene NA Naphthalene-d8 Fluorene-d10

1,6,7-trimethylnaphthalene NA NA Fluorene-d10

1-methylphenanthrene 13C Phenanthrene NA Acenaphthene-d10 Fluorene-d10

C1-decalins NA NA

C2-decalins NA NA

C3-decalins NA NA

C4-decalins NA NA

C1-naphthalenes NA Napthalene- d8 Fluorene-d10

C2-naphthalenes NA Napthalene- d8 Fluorene-d10

C3-naphthalenes NA Napthalene- d8 Fluorene-d10

C4-naphthalenes NA Napthalene- d8 Fluorene-d10

C1-benzothiophenes NA NA

C2-benzothiophenes NA NA

C3-benzothiophenes NA NA

C4-benzothiophenes NA NA

C1-fluorenes NA Acenapthene- d10 Fluorene-d10

C2-fluorenes NA Acenapthene- d10 Fluorene-d10

C3-fluorenes NA Acenapthene- d10 Fluorene-d10

C1-phenanthrenes/anthracenes NA Phananthrene- d10 Fluorene-d10

C2-phenanthrenes/anthracenes NA Phananthrene- d10 Fluorene-d10

C3-phenanthrenes/anthracenes NA Phananthrene- d10 Fluorene-d10

C4-phenanthrenes/anthracenes NA Phananthrene- d10 Fluorene-d10

C1-dibenzothiophenes NA Phananthrene- d10 Fluorene-d10

C2-dibenzothiophenes NA Phananthrene- d10 Fluorene-d10

C3-dibenzothiophenes NA Phananthrene- d10 Fluorene-d10

C4-dibenzothiophenes NA Phananthrene- d10 Fluorene-d10

C1-fluoranthenes/pyrenes NA Chyrsene- 12 Benzo(a)pyrene-d12

C2-fluoranthenes/pyrenes NA Chyrsene- 12 Benzo(a)pyrene-d12

C3-fluoranthenes/pyrenes NA Chyrsene- 12 Benzo(a)pyrene-d12

C4-fluoranthenes/pyrenes NA NA

C1-naphthobenzothiophenes NA NA

C2-naphthobenzothiophenes NA NA

C3-naphthobenzothiophenes NA NA

C4-naphthobenzothiophenes NA NA

C1-chrysenes NA Chyrsene- 12 Benzo(a)pyrene-d12

C2-chrysenes NA Chyrsene- 12 Benzo(a)pyrene-d12

C3-chrysenes NA Chyrsene- 12 Benzo(a)pyrene-d12

C4-chrysenes NA NA Benzo(a)pyrene-d12
68

Alkylated PAHs - IS/surrogate used for quantitation

Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18

1-methylnaphthalene naphthalene-d8 napthalene-d8 2-fluorobiphenyl

Fluorene-d10 / 

Naphthalene-d8

Fluorene-d10 / 

Naphthalene-d8 Naphthalene-d8

2-methylnaphthalene naphthalene-d8 napthalene-d8 2-fluorobiphenyl

Fluorene-d10 / 

Naphthalene-d8

Fluorene-d10 / 

Naphthalene-d8 Naphthalene-d8

2,6-dimethylnaphthalene naphthalene-d8 napthalene-d8 NA

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Acenaphthene-d10 Naphthalene-d8

1,6,7-trimethylnaphthalene acenaphthylene-d8 NA

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Acenaphthene-d10 Acenphthene-d10

1-methylphenanthrene phenanthrene-d10 phenanthrene-d10 NA

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12 Phenanthrene-d10

C1-decalins NA

Fluorene-d10 / 

Naphthalene-d8

Fluorene-d10 / 

Naphthalene-d8

C2-decalins NA

Fluorene-d10 / 

Naphthalene-d8

Fluorene-d10 / 

Naphthalene-d8

C3-decalins NA

Fluorene-d10 / 

Naphthalene-d8

Fluorene-d10 / 

Naphthalene-d8

C4-decalins NA

Fluorene-d10 / 

Naphthalene-d8

Fluorene-d10 / 

Naphthalene-d8

C1-naphthalenes NA

Fluorene-d10 / 

Naphthalene-d8

Fluorene-d10 / 

Naphthalene-d8

C2-naphthalenes 2-fluorobiphenyl

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Naphthalene-d8

C3-naphthalenes 2-fluorobiphenyl

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Naphthalene-d8

C4-naphthalenes 2-fluorobiphenyl

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Naphthalene-d8

C1-benzothiophenes NA

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Naphthalene-d8

C2-benzothiophenes NA

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Naphthalene-d8

C3-benzothiophenes NA

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Naphthalene-d8

C4-benzothiophenes NA

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Naphthalene-d8

C1-fluorenes 2-fluorobiphenyl

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Acenaphthene-d10

C2-fluorenes 2-fluorobiphenyl

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Phenanthrene-d10

C3-fluorenes 2-fluorobiphenyl

Fluorene-d10 / 

Acenaphthene-d10

Fluorene-d10 / 

Phenanthrene-d10

C1-phenanthrenes/anthracenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / 

Phenanthrene-d10

C2-phenanthrenes/anthracenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / 

Phenanthrene-d10

C3-phenanthrenes/anthracenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / 

Phenanthrene-d10

C4-phenanthrenes/anthracenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / 

Phenanthrene-d10

C1-dibenzothiophenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / 

Phenanthrene-d10

C2-dibenzothiophenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / 

Phenanthrene-d10

C3-dibenzothiophenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / 

Phenanthrene-d10

C4-dibenzothiophenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / 

Phenanthrene-d10

C1-fluoranthenes/pyrenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12

C2-fluoranthenes/pyrenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12

C3-fluoranthenes/pyrenes p-terphenyl-d14

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12

C4-fluoranthenes/pyrenes NA

Pyrene-d10 / Chrysened12

C1-naphthobenzothiophenes NA

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12

C2-naphthobenzothiophenes NA

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12

C3-naphthobenzothiophenes NA

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12

C4-naphthobenzothiophenes NA

Fluorene-d10 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12

C1-chrysenes NA

Chrysene-d12 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12

C2-chrysenes NA

Chrysene-d12 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12

C3-chrysenes NA

Chrysene-d12 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12

C4-chrysenes NA

Chrysene-d12 / 

Phenanthrene-d10

Pyrene-d10 / Chrysened12
69

Alkylated PAHs - IS/surrogate used for quantitation

Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24a Lab 24b

1-methylnaphthalene Naphthalene-d8 Naphthalene-d8 naphthalene-d8

d10-2-

methylnaphthalene d8-Naphthalene Naphthalene-d8

2-methylnaphthalene Naphthalene-d8 Acenaphthene-d10 acenaphthene-d10

d10-2-

methylnaphthalene d8-Naphthalene Naphthalene-d8

2,6-dimethylnaphthalene Naphthalene-d8 Acenaphthene-d10 naphthalene-d8

d12-2,6-

dimethylnaphthalene d10-Acenaphthene Naphthalene-d8

1,6,7-trimethylnaphthalene Phenanthrene-d10 Acenaphthene-d10 NA d10-Acenaphthene NA

1-methylphenanthrene Phenanthrene-d10 Phenanthrene-d10 phenanthrene-d10 d10-phenanthrene d10-Phenanthrene Acenaphthene-d10

C1-decalins __________ NA NA

C2-decalins __________ NA NA

C3-decalins __________ NA NA

C4-decalins __________ NA NA

C1-naphthalenes Naphthalene-d8 Naphthalene-d8 naphthalene-d8

d10-2-

methylnaphthalene Naphthalene-d8

C2-naphthalenes Naphthalene-d8 Acenaphthene-d10 naphthalene-d8

d12-2,6-

dimethylnaphthalene Naphthalene-d8

C3-naphthalenes Naphthalene-d8 Acenaphthene-d10 naphthalene-d8

d12-2,6-

dimethylnaphthalene Acenaphthene-d10

C4-naphthalenes Naphthalene-d8 Phenanthrene-d10 naphthalene-d8

d12-2,6-

dimethylnaphthalene Acenaphthene-d10

C1-benzothiophenes __________ NA NA

C2-benzothiophenes __________ NA NA

C3-benzothiophenes __________ NA NA

C4-benzothiophenes __________ NA NA

C1-fluorenes Acenaphthalene-d10 Phenanthrene-d10 acenaphthene-d10 d10-phenanthrene Acenaphthene-d10

C2-fluorenes Acenaphthalene-d10 Phenanthrene-d10 acenaphthene-d10 d10-phenanthrene Acenaphthene-d10

C3-fluorenes Acenaphthalene-d10 Phenanthrene-d10 acenaphthene-d10 d10-phenanthrene Acenaphthene-d10

C1-phenanthrenes/anthracenes Phenanthrene-d10 Phenanthrene-d10 phenanthrene-d10 d10-phenanthrene Acenaphthene-d10

C2-phenanthrenes/anthracenes Phenanthrene-d10 Phenanthrene-d10 phenanthrene-d10 d10-fluoranthene Acenaphthene-d10

C3-phenanthrenes/anthracenes Phenanthrene-d10 Chrysene-d12 phenanthrene-d10 d10-fluoranthene Acenaphthene-d10

C4-phenanthrenes/anthracenes Phenanthrene-d10 Chrysene-d12 d10-fluoranthene Acenaphthene-d10

C1-dibenzothiophenes Phenanthrene-d10 Phenanthrene-d10 d10-phenanthrene NA

C2-dibenzothiophenes Phenanthrene-d10 Phenanthrene-d10 d10-phenanthrene NA

C3-dibenzothiophenes Phenanthrene-d10 Phenanthrene-d10 d10-phenanthrene NA

C4-dibenzothiophenes Phenanthrene-d10 Chrysene-d12 d10-phenanthrene NA

C1-fluoranthenes/pyrenes Chrysene-d12 Chrysene-d12 chrysene-d12 d10-fluoranthene Acenaphthene-d10

C2-fluoranthenes/pyrenes Chrysene-d12 Chrysene-d12 chrysene-d12 d10-fluoranthene Acenaphthene-d10

C3-fluoranthenes/pyrenes Chrysene-d12 Chrysene-d12 d10-fluoranthene Acenaphthene-d10

C4-fluoranthenes/pyrenes __________ d10-fluoranthene Acenaphthene-d10

C1-naphthobenzothiophenes __________ NA NA

C2-naphthobenzothiophenes __________ NA NA

C3-naphthobenzothiophenes __________ NA NA

C4-naphthobenzothiophenes __________ NA NA

C1-chrysenes Chrysene-d12 Chrysene-d12 d12-chrysene NA

C2-chrysenes Chrysene-d12 Chrysene-d12 d12-chrysene NA

C3-chrysenes Chrysene-d12 Chrysene-d12 d12-chrysene NA

C4-chrysenes Chrysene-d12 Chrysene-d12 d12-chrysene NA
70

Alkylated PAHs - IS/surrogate used for quantitation

Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30

1-methylnaphthalene Naphthalene-d8

Naphthalene-d8/Fluorened10 Fluorene-d10/Naphthalene-d8 naphthalene-d8 d8-1-Methylnaphthalene naphthalene d8

2-methylnaphthalene Naphthalene-d8

Naphthalene-d8/Fluorened10 Fluorene-d10/Naphthalene-d8 naphthalene-d8 d8-1-Methylnaphthalene naphthalene d8

2,6-dimethylnaphthalene Naphthalene-d8

Naphthalene-d8/Fluorened10Fluorene-d10/Acenaphthened10 naphthalene-d8 d8-1-Methylnaphthalene naphthalene d8

1,6,7-trimethylnaphthalene

Naphthalene-d8/Fluorened10Fluorene-d10/Acenaphthened10 d10-Fluorene NA

1-methylphenanthrene Phenanthrene-d10

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 acenaphthene-d10 d8-Dibenzothiophene NA

C1-decalins

Naphthalene-d8/Fluorened10 Fluorene-d10/Naphthalene-d8 d8-1-Methylnaphthalene NA

C2-decalins

Naphthalene-d8/Fluorened10 Fluorene-d10/Naphthalene-d8 d8-1-Methylnaphthalene NA

C3-decalins

Naphthalene-d8/Fluorened10 Fluorene-d10/Naphthalene-d8 d8-1-Methylnaphthalene NA

C4-decalins

Naphthalene-d8/Fluorened10 Fluorene-d10/Naphthalene-d8 d8-1-Methylnaphthalene NA

C1-naphthalenes Naphthalene-d8

Naphthalene-d8/Fluorened10 Fluorene-d10/Naphthalene-d8 naphthalene-d8 d8-1-Methylnaphthalene NA

C2-naphthalenes Naphthalene-d8

Naphthalene-d8/Fluorened10Fluorene-d10/Acenaphthened10 naphthalene-d8 d10Acenapthene NA

C3-naphthalenes Naphthalene-d8

Naphthalene-d8/Fluorened10Fluorene-d10/Acenaphthened10 acenaphthene-d10 d10Fluorene NA

C4-naphthalenes Naphthalene-d8

Naphthalene-d8/Fluorened10Fluorene-d10/Acenaphthened10 acenaphthene-d10 d10Fluorene NA

C1-benzothiophenes

Naphthalene-d8/Fluorened10Fluorene-d10/Acenaphthened10 d8-1-Methylnaphthalene NA

C2-benzothiophenes

Naphthalene-d8/Fluorened10Fluorene-d10/Acenaphthened10 d8-1-Methylnaphthalene NA

C3-benzothiophenes

Naphthalene-d8/Fluorened10Fluorene-d10/Acenaphthened10 d8-1-Methylnaphthalene NA

C4-benzothiophenes

Naphthalene-d8/Fluorened10Fluorene-d10/Acenaphthened10 d8-1-Methylnaphthalene NA

C1-fluorenes Acenaphthene-d10

Acenaphthened10/Fluorene-d10Fluorene-d10/Acenaphthened10 acenaphthene-d10 d10-Fluorene NA

C2-fluorenes Acenaphthene-d10

Acenaphthened10/Fluorene-d10Fluorene-d10/Acenaphthened10 acenaphthene-d10 d10-Fluorene NA

C3-fluorenes Acenaphthene-d10

Acenaphthened10/Fluorene-d10Fluorene-d10/Acenaphthened10 acenaphthene-d10 d10-Fluorene NA

C1-phenanthrenes/anthracenes Phenanthrene-d10

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 acenaphthene-d10 d10-Anthracene NA

C2-phenanthrenes/anthracenes Phenanthrene-d10

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 acenaphthene-d10 d10-Anthracene NA

C3-phenanthrenes/anthracenes Phenanthrene-d10

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 acenaphthene-d10 d10-Anthracene NA

C4-phenanthrenes/anthracenes Phenanthrene-d10

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 acenaphthene-d10 d10-Anthracene NA

C1-dibenzothiophenes Phenanthrene-d10

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 d8-Dibenzothiophene NA

C2-dibenzothiophenes Phenanthrene-d10

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 d8-Dibenzothiophene NA

C3-dibenzothiophenes Phenanthrene-d10

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 d8-Dibenzothiophene NA

C4-dibenzothiophenes Phenanthrene-d10

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 d8-Dibenzothiophene NA

C1-fluoranthenes/pyrenes Chrysene-d12

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 d10-Fluoranthene NA

C2-fluoranthenes/pyrenes Chrysene-d12

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 d10-Fluoranthene NA

C3-fluoranthenes/pyrenes Chrysene-d12

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 d10-Fluoranthene NA

C4-fluoranthenes/pyrenes

Phenanthrened10/Fluoranthene-d10 Pyrene-d10/Phenanthrene-d10 d10-Fluoranthene NA

C1-naphthobenzothiophenes

Chrysene-d12/Terphenyld14 Pyrene-d10/Phenanthrene-d10 NA

C2-naphthobenzothiophenes

Chrysene-d12/Terphenyld14 Pyrene-d10/Phenanthrene-d10 NA

C3-naphthobenzothiophenes

Chrysene-d12/Terphenyld14 Pyrene-d10/Phenanthrene-d10 NA

C4-naphthobenzothiophenes

Chrysene-d12/Terphenyld14 Pyrene-d10/Phenanthrene-d10 NA

C1-chrysenes Chrysene-d12

Chrysene-d12/Terphenyld14 Pyrene-d10/Chrysene-d12 d12-Chrysene NA

C2-chrysenes Chrysene-d12

Chrysene-d12/Terphenyld14 Pyrene-d10/Chrysene-d12 d12-Chrysene NA

C3-chrysenes Chrysene-d12

Chrysene-d12/Terphenyld14 Pyrene-d10/Chrysene-d12 d12-Chrysene NA

C4-chrysenes Chrysene-d12

Chrysene-d12/Terphenyld14 Pyrene-d10/Chrysene-d12 d12-Chrysene NA
71

Alkylated PAHs - IS/surrogate used for quantitation

Lab 31 Lab 32 Lab 33 Lab 34

1-methylnaphthalene d10-Fluorene Acenaphthene-d10

2-methylnaphthalene d10-Fluorene Acenaphthene-d10

2,6-dimethylnaphthalene d10-Fluorene Acenaphthene-d10

1,6,7-trimethylnaphthalene d10-Fluorene Acenaphthene-d10

1-methylphenanthrene d10-Pyrene Acenaphthene-d10

C1-decalins d10-Fluorene Acenaphthene-d10

C2-decalins d10-Fluorene Acenaphthene-d10

C3-decalins d10-Fluorene Acenaphthene-d10

C4-decalins d10-Fluorene Acenaphthene-d10

C1-naphthalenes d10-Fluorene Acenaphthene-d10

C2-naphthalenes d10-Fluorene Acenaphthene-d10

C3-naphthalenes d10-Fluorene Acenaphthene-d10

C4-naphthalenes d10-Fluorene Acenaphthene-d10

C1-benzothiophenes d10-Fluorene Acenaphthene-d10

C2-benzothiophenes d10-Fluorene Acenaphthene-d10

C3-benzothiophenes d10-Fluorene Acenaphthene-d10

C4-benzothiophenes Acenaphthene-d10

C1-fluorenes d10-Fluorene Acenaphthene-d10

C2-fluorenes d10-Fluorene Acenaphthene-d10

C3-fluorenes d10-Fluorene Acenaphthene-d10

C1-phenanthrenes/anthracenes d10-Pyrene Acenaphthene-d10

C2-phenanthrenes/anthracenes d10-Pyrene Acenaphthene-d10

C3-phenanthrenes/anthracenes d10-Pyrene Acenaphthene-d10

C4-phenanthrenes/anthracenes d10-Pyrene Acenaphthene-d10

C1-dibenzothiophenes d10-Fluorene Acenaphthene-d10

C2-dibenzothiophenes d10-Fluorene Acenaphthene-d10

C3-dibenzothiophenes d10-Fluorene Acenaphthene-d10

C4-dibenzothiophenes Acenaphthene-d10

C1-fluoranthenes/pyrenes d10-Pyrene Acenaphthene-d10

C2-fluoranthenes/pyrenes d10-Pyrene Acenaphthene-d10

C3-fluoranthenes/pyrenes d10-Pyrene Acenaphthene-d10

C4-fluoranthenes/pyrenes Acenaphthene-d10

C1-naphthobenzothiophenes d10-Pyrene Acenaphthene-d10

C2-naphthobenzothiophenes d10-Pyrene Acenaphthene-d10

C3-naphthobenzothiophenes d10-Pyrene Acenaphthene-d10

C4-naphthobenzothiophenes Acenaphthene-d10

C1-chrysenes Chrysene-d12

C2-chrysenes d12-Benzo(a)pyrene Chrysene-d12

C3-chrysenes d12-Benzo(a)pyrene Chrysene-d12

C4-chrysenes d12-Benzo(a)pyrene Chrysene-d12
72

Biomarkers - IS/surrogate used for quantitation

Lab 1 Lab 3 Lab 10 Lab 12 Lab 14 Lab 16 Lab 17 Lab 19 Lab 20 Lab 22 Lab 25 Lab 26 Lab 30 Lab 34

Carbazole NA NA NA

Pyrene-d10 / 

Phenanthrened10d10-

phenanthrene Chrysene-d12

Phenanthrened10/Fluoranthened10

phenanthrene 

d10 Chrysene-d12

18a(H)-22,29,30-Trisnorhopane NA Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 NA Chrysene-d12 NA Chrysene-d12

17a(H)-22,29,30-Trisnorhopane B[a]A-d12 Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Benz[a]anthrace

ne-d12

Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 d50-tetracosane Chrysene-d12 NA Chrysene-d12

17α(H),21β(H)-30-Norhopane B[a]A-d12 Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Benz[a]anthrace

ne-d12

Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 d50-tetracosane Chrysene-d12 NA Chrysene-d12

18a(H)-30-Norneohopane NA Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 NA Chrysene-d12 NA Chrysene-d12

17a(H)-Diahopane NA Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 NA Chrysene-d12 NA Chrysene-d12

17α(H),21β(H)-Hopane B[a]A-d12 Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Benz[a]anthrace

ne-d12

Chrysene-d12 / 

5b(H)-Cholane

Benzo(a)pyrened12 / 5-alpha 

Androstane Chrysene-d12 Chrysene-d12 d50-tetracosane Chrysene-d12

Chrysened12/Terphenyld14 NA Chrysene-d12

17α(H),21β(H)-22R-Homohopane B[a]A-d12 Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Benz[a]anthrace

ne-d12

Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 d50-tetracosane Chrysene-d12 NA Chrysene-d12

17α(H),21β(H)-22S-Homohopane B[a]A-d12 Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Benz[a]anthrace

ne-d12

Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 d50-tetracosane Chrysene-d12 NA Chrysene-d12

13b(H)17a(H)-Diacholestane 20S NA Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 NA Chrysene-d12 NA Chrysene-d12

5a(H),14a(H),17a(H)-Cholestane 20S NA Chrysene-d12 NA

Benzo(a)pyrened12Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 NA Chrysene-d12 NA Chrysene-d12

5a(H),14a(H),17a(H)-Cholestane 20R B[a]A-d12 Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Benz[a]anthrace

ne-d12

Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 d50-tetracosane Chrysene-d12 NA Chrysene-d12

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S NA Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Benz[a]anthrace

ne-d12

Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 NA Chrysene-d12 NA Chrysene-d12

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R B[a]A-d12 Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 d50-tetracosane Chrysene-d12 NA Chrysene-d12

5a(H),14b(H),17b(H)-Cholestane 20R B[a]A-d12 Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Benz[a]anthrace

ne-d12

Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 d50-tetracosane Chrysene-d12 NA Chrysene-d12

5a(H),14b(H),17b(H)-Cholestane 20S NA Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 NA Chrysene-d12 NA Chrysene-d12

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R B[a]A-d12 Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Benz[a]anthrace

ne-d12

Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 d50-tetracosane Chrysene-d12 NA Chrysene-d12

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S NA Chrysene-d12 Chyrsene- 12

Benzo(a)pyrened12Chrysene-d12 / 

5b(H)-Cholane Chrysene-d12 Chrysene-d12 NA Chrysene-d12 NA Chrysene-d12
73

PAHs - Associated % recovery / acceptance ranges

Lab 3 Lab 10 Lab 16 Lab 17 Lab 19 Lab 20 Lab 21 Lab 23 Lab 25 Lab 26 Lab 27 Lab 28 Lab 30 Lab 33 Lab 34

naphthalene 60-140

minus 50 to 

plus 100 40 to 120 1%-33% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 60-130% 40-120

biphenyl 60-140

minus 50 to 

plus 100 40 to 120 1%-42% 60-140 50-120

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

acenaphthene 60-140

minus 50 to 

plus 100 40 to 120 1%-42% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

acenaphthylene 60-140

minus 50 to 

plus 100 40 to 120 1%-42% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

fluorene 60-140

minus 50 to 

plus 100 40 to 120 1%-42% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

phenanthrene 60-140

minus 50 to 

plus 100 40 to 120 4%-54% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

anthracene 60-140

minus 50 to 

plus 100 40 to 120 4%-54% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

fluoranthene 60-140

minus 50 to 

plus 100 40 to 120 24%-68% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

pyrene 60-140

minus 50 to 

plus 100 40 to 120 24%-68% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

benzo[b]fluorene NA

minus 50 to 

plus 100 24%-68%

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

benz[a]anthracene 60-140

minus 50 to 

plus 100 40 to 120 24%-68% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

chrysene 60-140

minus 50 to 

plus 100 40 to 120 24%-68% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

triphenylene NA

minus 50 to 

plus 100 24%-68%

50-200% of IS 

value in CCV 40-120 NA NA 40-120

benzo[b ]fluoranthene 60-140

minus 50 to 

plus 100 40 to 120 1%-73% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

benzo[j ]fluoranthene NA

minus 50 to 

plus 100 1%-73%

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

benzo[k ]fluoranthene 60-140

minus 50 to 

plus 100 40 to 120 1%-73% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 NA +/-30% NA 40-120

benzo[a]fluoranthene NA

minus 50 to 

plus 100 1%-73%

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

benzo[e]pyrene 60-140

minus 50 to 

plus 100 40 to 120 1%-73% 60-140 50-120

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

benzo[a]pyrene 60-140

minus 50 to 

plus 100 40 to 120 1%-73% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

perylene 60-140

minus 50 to 

plus 100 40 to 120 1%-73% 60-140 50-120

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

indeno[1,2,3-cd]pyrene 60-140

minus 50 to 

plus 100 40 to 120 1%-73% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

benzo[ghi]perylene 60-140

minus 50 to 

plus 100 40 to 120 1%-73% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

dibenz[a,h]anthracene 60-140

minus 50 to 

plus 100 40 to 120 1%-73% 60-140 60 - 140 50-200 50-120

50-200% of IS 

value in CCV 40-120 60-120 +/-30% NA 40-120

cis/trans-decalin NA

minus 50 to 

plus 100 40 to 120 1%-33%

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

dibenzofuran 60-140

minus 50 to 

plus 100 40 to 120 1%-42% 60-140

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

retene NA

minus 50 to 

plus 100 40 to 120 24%-68%

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

benzothiophene NA

minus 50 to 

plus 100 40 to 120 1%-33%

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

dibenzothiophene 60-140

minus 50 to 

plus 100 40 to 120 4%-54% 60-140 50-120

50-200% of IS 

value in CCV 40-120 60-120 NA 40-120

naphthobenzothiophene NA

minus 50 to 

plus 100 40 to 120 24%-68% 40-120 60-120 40-120
74

AlkylatedPAHs - Associated % recovery / acceptance ranges

Lab 3 Lab 10 Lab 16 Lab 17 Lab 19 Lab 20 Lab 21 Lab 23 Lab 25 Lab 26 Lab 27 Lab 28 Lab 34

1-methylnaphthalene 60-140 - 50 to +100 40 to 120 1%-33% 60-140 50-200 50-120 50-200% of IS value in CCV 40-120 60-120 +/-30% 40-120

2-methylnaphthalene 60-140 - 50 to +100 40 to 120 1%-33% 60-140 60 - 140 50-200 50-120 50-200% of IS value in CCV 40-120 60-120 +/-30% 40-120

2,6-dimethylnaphthalene 60-140 - 50 to +100 40 to 120 1%-42% 60-140 50-200 50-120 50-200% of IS value in CCV 40-120 60-120 +/-30% 40-120

1,6,7-trimethylnaphthalene 60-140 - 50 to +100 40 to 120 1%-42% 60-140 50-120 50-200% of IS value in CCV 40-120 60-120 40-120

1-methylphenanthrene 60-140 - 50 to +100 40 to 120 24%-68% 60-140 50-200 50-120 50-200% of IS value in CCV 40-120 60-120 +/-30% 40-120

C1-decalins NA - 50 to +100 40 to 120 1%-33% 50-200% of IS value in CCV 40-120 NA 40-120

C2-decalins NA - 50 to +100 40 to 120 1%-33% 50-200% of IS value in CCV 40-120 NA 40-120

C3-decalins NA - 50 to +100 40 to 120 1%-33% 50-200% of IS value in CCV 40-120 NA 40-120

C4-decalins NA - 50 to +100 40 to 120 1%-33% 50-200% of IS value in CCV 40-120 NA 40-120

C1-naphthalenes NA - 50 to +100 40 to 120 1%-33% 60-140 50-200 50-200% of IS value in CCV 40-120 NA N/A 40-120

C2-naphthalenes NA - 50 to +100 40 to 120 1%-33% 60-140 50-200 50-200% of IS value in CCV 40-120 NA N/A 40-120

C3-naphthalenes NA - 50 to +100 40 to 120 1%-33% 60-140 50-200 50-200% of IS value in CCV 40-120 NA N/A 40-120

C4-naphthalenes NA - 50 to +100 40 to 120 1%-33% 60-140 50-200 50-200% of IS value in CCV 40-120 NA N/A 40-120

C1-benzothiophenes NA - 50 to +100 40 to 120 1%-33% 50-200% of IS value in CCV 40-120 NA 40-120

C2-benzothiophenes NA - 50 to +100 40 to 120 1%-33% 50-200% of IS value in CCV 40-120 NA 40-120

C3-benzothiophenes NA - 50 to +100 40 to 120 1%-33% 50-200% of IS value in CCV 40-120 NA 40-120

C4-benzothiophenes NA - 50 to +100 40 to 120 1%-33% 50-200% of IS value in CCV 40-120 NA 40-120

C1-fluorenes NA - 50 to +100 40 to 120 1%-42% 60-140 50-200 50-200% of IS value in CCV 40-120 NA N/A 40-120

C2-fluorenes NA - 50 to +100 40 to 120 4%-54% 60-140 50-200 50-200% of IS value in CCV 40-120 NA N/A 40-120

C3-fluorenes NA - 50 to +100 40 to 120 4%-54% 60-140 50-200 50-200% of IS value in CCV 40-120 NA N/A 40-120

C1-phenanthrenes/anthracenes NA - 50 to +100 40 to 120 4%-54% 60-140 50-200 50-200% of IS value in CCV 40-120 NA N/A 40-120

C2-phenanthrenes/anthracenes NA - 50 to +100 40 to 120 4%-54% 60-140 50-200 50-200% of IS value in CCV 40-120 NA N/A 40-120

C3-phenanthrenes/anthracenes NA - 50 to +100 40 to 120 4%-54% 60-140 50-200 50-200% of IS value in CCV 40-120 NA N/A 40-120

C4-phenanthrenes/anthracenes NA - 50 to +100 40 to 120 4%-54% 60-140 50-200% of IS value in CCV 40-120 NA N/A 40-120

C1-dibenzothiophenes NA - 50 to +100 40 to 120 4%-54% 60-140 50-200% of IS value in CCV 40-120 NA 40-120

C2-dibenzothiophenes NA - 50 to +100 40 to 120 4%-54% 60-140 50-200% of IS value in CCV 40-120 NA 40-120

C3-dibenzothiophenes NA - 50 to +100 40 to 120 4%-54% 60-140 50-200% of IS value in CCV 40-120 NA 40-120

C4-dibenzothiophenes NA - 50 to +100 40 to 120 4%-54% 60-140 50-200% of IS value in CCV 40-120 NA 40-120

C1-fluoranthenes/pyrenes NA - 50 to +100 40 to 120 24%-68% 60-140 50-200 50-200% of IS value in CCV 40-120 NA 40-120

C2-fluoranthenes/pyrenes NA - 50 to +100 40 to 120 24%-68% 60-140 50-200 50-200% of IS value in CCV 40-120 NA 40-120

C3-fluoranthenes/pyrenes NA - 50 to +100 40 to 120 24%-68% 60-140 50-200% of IS value in CCV 40-120 NA 40-120

C4-fluoranthenes/pyrenes NA - 50 to +100 24%-68% 60-140 50-200% of IS value in CCV 40-120 NA 40-120

C1-naphthobenzothiophenes NA - 50 to +100 40 to 120 24%-68% 50-200% of IS value in CCV 40-120 NA 40-120

C2-naphthobenzothiophenes NA - 50 to +100 40 to 120 24%-68% 50-200% of IS value in CCV 40-120 NA 40-120

C3-naphthobenzothiophenes NA - 50 to +100 40 to 120 24%-68% 50-200% of IS value in CCV 40-120 NA 40-120

C4-naphthobenzothiophenes NA - 50 to +100 40 to 120 24%-68% 50-200% of IS value in CCV 40-120 NA 40-120

C1-chrysenes NA - 50 to +100 40 to 120 24%-68% 60-140 50-200% of IS value in CCV 40-120 NA 40-120

C2-chrysenes NA - 50 to +100 40 to 120 24%-68% 60-140 50-200% of IS value in CCV 40-120 NA 40-120

C3-chrysenes NA - 50 to +100 40 to 120 24%-68% 60-140 50-200% of IS value in CCV 40-120 NA 40-120

C4-chrysenes NA - 50 to +100 40 to 120 24%-68% 60-140 50-200% of IS value in CCV 40-120 NA 40-120
75

Biomarkers - Associated % recovery / acceptance ranges

Lab 3 Lab 10 Lab 16 Lab 17 Lab 19 Lab 25 Lab 26 Lab 27 Lab 30 Lab 34

Carbazole NA

minus 50 to plus 

100 4%-54%

50-200% of IS value 

in CCV 40-120 NA NA 50-130

18a(H)-22,29,30-Trisnorhopane NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

17a(H)-22,29,30-Trisnorhopane NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

17α(H),21β(H)-30-Norhopane NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

18a(H)-30-Norneohopane NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

17a(H)-Diahopane NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

17α(H),21β(H)-Hopane 60-140

minus 50 to plus 

100 40 to 120 17%-60% 60-140

50-200% of IS value 

in CCV 40-120 NA NA 50-130

17α(H),21β(H)-22R-Homohopane NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

17α(H),21β(H)-22S-Homohopane NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

13b(H)17a(H)-Diacholestane 20S NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

5a(H),14a(H),17a(H)-Cholestane 20S NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

5a(H),14a(H),17a(H)-Cholestane 20R NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

5a(H),14b(H),17b(H)-Cholestane 20R NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

5a(H),14b(H),17b(H)-Cholestane 20S NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S NA

minus 50 to plus 

100 40 to 120 60-140

50-200% of IS value 

in CCV NA NA 50-130
76

PAHs -If "representative compound" used for quantitation, list the compound

Lab 5 Lab 8 Lab 18 Lab 19 Lab 27

naphthalene naphthalene NA

biphenyl biphenyl NA

acenaphthene acenaphthene NA

acenaphthylene acenaphthylene NA

fluorene fluorene NA

phenanthrene phenanthrene NA

anthracene anthracene NA

fluoranthene fluoranthene NA

pyrene pyrene NA

benzo[b]fluorene NA

benz[a]anthracene benz[a]anthracene NA

chrysene chrysene NA

triphenylene Chrysene chrysene

benzo[b ]fluoranthene benzo[b]fluoranthene NA

benzo[j ]fluoranthene benzo[k]fluoranthene

benzo[k ]fluoranthene benzo[k]fluoranthene NA

benzo[a]fluoranthene benzo[k]fluoranthene

benzo[e]pyrene 13C benzo[a]pyrene benzo[e]pyrene NA

benzo[a]pyrene benzo[a]pyrene NA

perylene perylene NA

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

benzo[ghi]perylene benzo[ghi]perylene NA

dibenz[a,h]anthracene dibenz[a,h]anthracene NA

cis/trans-decalin NA

dibenzofuran dibenzofuran NA

retene 1-methylphenanthrene NA

benzothiophene NA

dibenzothiophene dibenzothiophene NA

naphthobenzothiophene dibenzothiophene NA
77

Alkylated PAHs -If "representative compound" used for quantitation, list the compound

Lab 1 Lab 3 Lab 4 Lab 5 Lab 8 Lab 10 Lab 12 Lab 15

1-methylnaphthalene NA 13C Acenaphthylene NA

2-methylnaphthalene NA 13C Acenaphthylene NA

2,6-dimethylnaphthalene NA 13C Acenaphthylene NA

1,6,7-trimethylnaphthalene NA NA

1-methylphenanthrene NA 13C Phenanthrene NA

C1-decalins NA cis/trans-decalin NA

C2-decalins NA cis/trans-decalin NA

C3-decalins NA cis/trans-decalin NA

C4-decalins NA cis/trans-decalin NA

C1-naphthalenes 1-me and 2-menaphthalene Naphthalene Naphthalene Napthalene Naphthalene

C2-naphthalenes 2,6-dimehtylnaphthalene Naphthalene Naphthalene 2,6-dimethylnaphthalene Napthalene Naphthalene

C3-naphthalenes 2,3,5-trimethylnaphthalene Naphthalene Naphthalene 1,6,7-trimethylnaphthalene Napthalene Naphthalene

C4-naphthalenes 2,3,5-trimethylnaphthalene Naphthalene Naphthalene 1,6,7-trimethylnaphthalene Napthalene Naphthalene C3-naphthalenes

C1-benzothiophenes NA benzothiophene NA

C2-benzothiophenes NA benzothiophene NA

C3-benzothiophenes NA benzothiophene NA

C4-benzothiophenes NA benzothiophene NA

C1-fluorenes fluorene Fluorene Fluorene fluorene Flourene Fluorene fluorene

C2-fluorenes Fluorene Fluorene fluorene Flourene Fluorene fluorene

C3-fluorenes Fluorene Fluorene fluorene Flourene Fluorene fluorene

C1-phenanthrenes/anthracenes

1-me, 2-me, 3-me, and 9-

mephenanthrene plus 2-

meanthracene Phenanthrene Phenanthrene 1-methylphenanthrene Phenanthrene Phenanthrene

C2-phenanthrenes/anthracenes 1,7-dimethylphenanthrene Phenanthrene Phenanthrene 1-methylphenanthrene Phenanthrene Phenanthrene C1-phenanthrenes/anthracenes

C3-phenanthrenes/anthracenes 1,7-dimethylphenanthrene Phenanthrene Phenanthrene 1-methylphenanthrene Phenanthrene Phenanthrene C1-phenanthrenes/anthracenes

C4-phenanthrenes/anthracenes 1,7-dimethylphenanthrene Phenanthrene Phenanthrene 1-methylphenanthrene Phenanthrene Phenanthrene retene

C1-dibenzothiophenes dibenzothiophene Dibenzothiophene Dibenzothiophene dibenzothiophene Dibenzothiophene Dibenzothiophene dibenzothiophene

C2-dibenzothiophenes dibenzothiophene Dibenzothiophene Dibenzothiophene dibenzothiophene Dibenzothiophene Dibenzothiophene dibenzothiophene

C3-dibenzothiophenes dibenzothiophene Dibenzothiophene Dibenzothiophene dibenzothiophene Dibenzothiophene Dibenzothiophene dibenzothiophene

C4-dibenzothiophenes dibenzothiophene Dibenzothiophene Dibenzothiophene dibenzothiophene Dibenzothiophene Dibenzothiophene dibenzothiophene

C1-fluoranthenes/pyrenes

1-me and 3-mefluoranthene plus 1-

me and 4-mepyrene Pyrene Fluoranthene fluoranthene Pyrene Pyrene pyrene

C2-fluoranthenes/pyrenes

1-me and 3-mefluoranthene plus 1-

me and 4-mepyrene Pyrene Fluoranthene fluoranthene Pyrene Pyrene pyrene

C3-fluoranthenes/pyrenes

1-me and 3-mefluoranthene plus 1-

me and 4-mepyrene Pyrene Fluoranthene fluoranthene Pyrene Pyrene pyrene

C4-fluoranthenes/pyrenes

1-me and 3-mefluoranthene plus 1-

me and 4-mepyrene NA Fluoranthene fluoranthene NA

C1-naphthobenzothiophenes NA naphthobenzothiophene dibenzothiophene NA

C2-naphthobenzothiophenes NA naphthobenzothiophene dibenzothiophene NA

C3-naphthobenzothiophenes NA naphthobenzothiophene dibenzothiophene NA

C4-naphthobenzothiophenes NA naphthobenzothiophene dibenzothiophene NA

C1-chrysenes 3-me and 6-mechyrsne Chrysene Chysene chrysene Chyrsene Chrysene

C2-chrysenes 3-me and 6-mechyrsne Chrysene Chysene chrysene Chyrsene Chrysene

C3-chrysenes 3-me and 6-mechyrsne Chrysene Chysene chrysene Chyrsene Chrysene

C4-chrysenes 3-me and 6-mechyrsne Chrysene Chysene chrysene NA Chrysene
78

Alkylated PAHs -If "representative compound" used for quantitation, list the compound

Lab 16 Lab 17 Lab 19 Lab 20 Lab 21 Lab 22 Lab 26 Lab 27

1-methylnaphthalene 1-methylnaphthalene NA

2-methylnaphthalene 2-methylnaphthalene NA

2,6-dimethylnaphthalene 2,6-dimethylnaphthalene NA

1,6,7-trimethylnaphthalene 1,6,7-trimethylnaphthalene NA

1-methylphenanthrene phenanthrene 1-methylphenanthrene Phenanthrene phenanthrene

C1-decalins trans-decalin cis/trans-decalin Decalin cis/trans-decalin

C2-decalins trans-decalin cis/trans-decalin Decalin cis/trans-decalin

C3-decalins trans-decalin cis/trans-decalin Decalin cis/trans-decalin

C4-decalins trans-decalin cis/trans-decalin Decalin cis/trans-decalin

C1-naphthalenes naphthalene naphthalene Naphthalene Naphthalene 1-methylnaphthalene 1- & 2-methylnaphthalene Naphthalene naphthalene

C2-naphthalenes naphthalene naphthalene Naphthalene Naphthalene 2,6-dimethylnaphthalene 2,6- & 1,2-dimethylnaphthalene Naphthalene naphthalene

C3-naphthalenes naphthalene naphthalene Naphthalene Naphthalene 1,3,5-trimethylnaphthalene

2,3,5- & 2,3,6-

trimethylnaphthalene Naphthalene naphthalene

C4-naphthalenes naphthalene naphthalene Naphthalene Naphthalene 1,3,5-trimethylnaphthalene 1,4,6,7-tetramethylnaphthalene Naphthalene naphthalene

C1-benzothiophenes benzo(b)thiophene benzothiophene Benzothiophene benzothiophene

C2-benzothiophenes benzo(b)thiophene benzothiophene Benzothiophene benzothiophene

C3-benzothiophenes benzo(b)thiophene benzothiophene Benzothiophene benzothiophene

C4-benzothiophenes benzo(b)thiophene benzothiophene Benzothiophene benzothiophene

C1-fluorenes Fluorene fluorene fluorene Fluorene fluorene 2-methylfluorene Fluorene fluorene

C2-fluorenes Fluorene fluorene fluorene Fluorene fluorene 1,7-dimethylfluorene Fluorene fluorene

C3-fluorenes Fluorene fluorene fluorene Fluorene fluorene 1,7-dimethylfluorene Fluorene fluorene

C1-phenanthrenes/anthracenes phenanthrene phenanthrene phenanthrene Phenanthrene 1-methylphenenthrene

1- & 2-methylphenanthrene & 2-

methylanthracene Phenanthrene phenanthrene

C2-phenanthrenes/anthracenes phenanthrene phenanthrene phenanthrene Phenanthrene 1-methylphenenthrene 3,6- & 1,7-dimethylphenanthrene Phenanthrene phenanthrene

C3-phenanthrenes/anthracenes phenanthrene phenanthrene phenanthrene Phenanthrene 1-methylphenenthrene 1,2,6-trimethylphenanthrene Phenanthrene phenanthrene

C4-phenanthrenes/anthracenes phenanthrene phenanthrene phenanthrene Phenanthrene retene Phenanthrene phenanthrene

C1-dibenzothiophenes dibenzothiophene dibenzothiophene dibenzothiophene Dibenzothiophene 2/3-methyldibenzothiophenes Dibenzothiophene dibenzothiophene

C2-dibenzothiophenes dibenzothiophene dibenzothiophene dibenzothiophene Dibenzothiophene 2,4-dimethyldibenzothiophene Dibenzothiophene dibenzothiophene

C3-dibenzothiophenes dibenzothiophene dibenzothiophene dibenzothiophene Dibenzothiophene 2,4-dimethyldibenzothiophene Dibenzothiophene dibenzothiophene

C4-dibenzothiophenes dibenzothiophene dibenzothiophene dibenzothiophene Dibenzothiophene 2,4-dimethyldibenzothiophene Dibenzothiophene dibenzothiophene

C1-fluoranthenes/pyrenes pyrene pyrene pyrene Pyrene pyrene 3-methylfluoranthene Fluoranthene fluoranthene

C2-fluoranthenes/pyrenes pyrene pyrene pyrene Pyrene pyrene 3-methylfluoranthene Fluoranthene fluoranthene

C3-fluoranthenes/pyrenes pyrene pyrene pyrene Pyrene 3-methylfluoranthene Fluoranthene fluoranthene

C4-fluoranthenes/pyrenes pyrene pyrene 3-methylfluoranthene Fluoranthene fluoranthene

C1-naphthobenzothiophenes benzo(b)naphtho(2,1-d)thiophene naphthobenzothiophene Naphthobenzothiophene naphthobenzothiophene

C2-naphthobenzothiophenes benzo(b)naphtho(2,1-d)thiophene naphthobenzothiophene Naphthobenzothiophene naphthobenzothiophene

C3-naphthobenzothiophenes benzo(b)naphtho(2,1-d)thiophene naphthobenzothiophene Naphthobenzothiophene naphthobenzothiophene

C4-naphthobenzothiophenes benzo(b)naphtho(2,1-d)thiophene naphthobenzothiophene Naphthobenzothiophene naphthobenzothiophene

C1-chrysenes Chrysene chrysene/triphenylene chrysene Chrysene 1- & 6-methylchrysene Chrysene chrysene

C2-chrysenes Chrysene chrysene/triphenylene chrysene Chrysene 5,9-dimethylchrysene Chrysene chrysene

C3-chrysenes Chrysene chrysene/triphenylene chrysene Chrysene 5,9-dimethylchrysene Chrysene chrysene

C4-chrysenes Chrysene chrysene/triphenylene chrysene Chrysene 5,9-dimethylchrysene Chrysene chrysene
79

Alkylated PAHs -If "representative compound" used for quantitation, list the compound

Lab 28 Lab 29 Lab 32 Lab 33 Lab 34

1-methylnaphthalene

2-methylnaphthalene

2,6-dimethylnaphthalene

1,6,7-trimethylnaphthalene

1-methylphenanthrene

C1-decalins cis+trans decalin Decalin trans-decalin

C2-decalins cis+trans decalin Decalin trans-decalin

C3-decalins cis+trans decalin Decalin trans-decalin

C4-decalins cis+trans decalin Decalin trans-decalin

C1-naphthalenes

1-methylnaphthalene/2-

methylnaphthalene 1+2-methylnaphthalene Naphthalene 1 methyl napthalene naphthalene

C2-naphthalenes 2,6-dimethylnaphthalene Sum of five DMNs Naphthalene 2,6 dimethyl napthalene naphthalene

C3-naphthalenes 2,3,5-trimethylnaphthalene 1,6,7-TMN Naphthalene 2,3,5 trimethyl napthalene naphthalene

C4-naphthalenes 1,2,5,6-tetramethylnaphthalene 1,6,7-TMN 1,2,5,6 tetramethylnapthalene naphthalene

C1-benzothiophenes benzothiophene Benzothiophene benzothiophene

C2-benzothiophenes benzothiophene Benzothiophene benzothiophene

C3-benzothiophenes benzothiophene Benzothiophene benzothiophene

C4-benzothiophenes benzothiophene benzothiophene

C1-fluorenes 1-methylfluorene 1-methylfluorene Fluorene 1 methyl fluorene fluorene

C2-fluorenes 1,7-dimethylfluorene 1-methylfluorene Fluorene 1,7 dimethyl fluorene fluorene

C3-fluorenes 9-n-propylfluorene 1-methylfluorene Fluorene 9-n propyl fluorene fluorene

C1-phenanthrenes/anthracenes 1-methylphenanthrene

Sum of five methylphenanthrenes 

and anthracenes Anthracene 1-methylphenanthrene phenanthrene

C2-phenanthrenes/anthracenes 1,3-dimethylphenanthrene 9,10-dimethylanthracene Anthracene 1,3 dimethylphenanthrene phenanthrene

C3-phenanthrenes/anthracenes 1,2,6-trimethylphenanthrene 9,10-dimethylanthracene Anthracene 1,2,6 trimethylphenanthrene phenanthrene

C4-phenanthrenes/anthracenes 1,2,6,9-tetramethylphenanthrene 9,10-dimethylanthracene Anthracene 1,2,6,9 tetramethylphenanthrene phenanthrene

C1-dibenzothiophenes 2+4-methyldibenzothiophene Dibenzothiophene dibenzothiophene

C2-dibenzothiophenes 2+4-methyldibenzothiophene Dibenzothiophene dibenzothiophene

C3-dibenzothiophenes 2+4-methyldibenzothiophene Dibenzothiophene dibenzothiophene

C4-dibenzothiophenes 2+4-methyldibenzothiophene dibenzothiophene

C1-fluoranthenes/pyrenes benzo(a+b)fluorene Fluoranthene pyrene

C2-fluoranthenes/pyrenes benzo(a+b)fluorene Fluoranthene pyrene

C3-fluoranthenes/pyrenes benzo(a+b)fluorene Fluoranthene pyrene

C4-fluoranthenes/pyrenes benzo(a+b)fluorene pyrene

C1-naphthobenzothiophenes Naphthobenzothiophene naphthobenzothiophene

C2-naphthobenzothiophenes Naphthobenzothiophene naphthobenzothiophene

C3-naphthobenzothiophenes Naphthobenzothiophene naphthobenzothiophene

C4-naphthobenzothiophenes naphthobenzothiophene

C1-chrysenes Chrysene+Triphenylene chrysene

C2-chrysenes Chrysene+Triphenylene Chrysene chrysene

C3-chrysenes Chrysene+Triphenylene Chrysene chrysene

C4-chrysenes Chrysene+Triphenylene Chrysene chrysene
80

Biomarkers -If "representative compound" used for quantitation, list the compound

Lab 3 Lab 10 Lab 12 Lab 16 Lab 19 Lab 20 Lab 34

Carbazole NA

18a(H)-22,29,30-Trisnorhopane 17β(H),21β(H)-Hopane 17α(H),21β(H)-Hopane 17b(H)21b(H) Hopane 17B(h),21B(h)-hopane 17b(H)21b(H) Hopane 17b(H)21b(H)Hopane 17α(H),21β(H)-Hopane

17a(H)-22,29,30-Trisnorhopane 17β(H),21β(H)-Hopane 17α(H),21β(H)-Hopane 17b(H)21b(H) Hopane 17B(h),21B(h)-hopane 17b(H)21b(H) Hopane 17b(H)21b(H)Hopane 17α(H),21β(H)-Hopane

17α(H),21β(H)-30-Norhopane 17β(H),21β(H)-Hopane 17α(H),21β(H)-Hopane 17b(H)21b(H) Hopane 17B(h),21B(h)-hopane 17b(H)21b(H) Hopane 17b(H)21b(H)Hopane 17α(H),21β(H)-Hopane

18a(H)-30-Norneohopane 17β(H),21β(H)-Hopane 17α(H),21β(H)-Hopane 17b(H)21b(H) Hopane 17B(h),21B(h)-hopane 17b(H)21b(H) Hopane 17b(H)21b(H)Hopane 17α(H),21β(H)-Hopane

17a(H)-Diahopane 17β(H),21β(H)-Hopane 17α(H),21β(H)-Hopane 17b(H)21b(H) Hopane 17B(h),21B(h)-hopane 17b(H)21b(H) Hopane 17b(H)21b(H)Hopane 17α(H),21β(H)-Hopane

17α(H),21β(H)-Hopane 17β(H),21β(H)-Hopane 17α(H),21β(H)-Hopane 17b(H)21b(H) Hopane 17B(h),21B(h)-hopane 17b(H)21b(H) Hopane 17b(H)21b(H)Hopane

17α(H),21β(H)-22R-Homohopane 17β(H),21β(H)-Hopane 17α(H),21β(H)-Hopane 17b(H)21b(H) Hopane 17B(h),21B(h)-hopane 17b(H)21b(H) Hopane 17b(H)21b(H)Hopane 17α(H),21β(H)-Hopane

17α(H),21β(H)-22S-Homohopane 17β(H),21β(H)-Hopane 17α(H),21β(H)-Hopane 17b(H)21b(H) Hopane 17B(h),21B(h)-hopane 17b(H)21b(H) Hopane 17b(H)21b(H)Hopane 17α(H),21β(H)-Hopane

13b(H)17a(H)-Diacholestane 20S 5α - Cholestane 5(a) Cholestane 5a-Cholestane Cholestane 5a-Cholestane 5a-Cholestane 5b(H)Cholane

5a(H),14a(H),17a(H)-Cholestane 20S 5α - Cholestane 5a-Cholestane Cholestane 5a-Cholestane 5a-Cholestane 5b(H)Cholane

5a(H),14a(H),17a(H)-Cholestane 20R 5α - Cholestane 5(a) Cholestane 5a-Cholestane Cholestane 5a-Cholestane 5a-Cholestane 5b(H)Cholane

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S 5α - Cholestane 5(a) Cholestane 5a-Cholestane Cholestane 5a-Cholestane 5a-Cholestane 5b(H)Cholane

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R 5α - Cholestane 5(a) Cholestane 5a-Cholestane Cholestane 5a-Cholestane 5a-Cholestane 5b(H)Cholane

5a(H),14b(H),17b(H)-Cholestane 20R 5α - Cholestane 5(a) Cholestane 5a-Cholestane Cholestane 5a-Cholestane 5a-Cholestane 5b(H)Cholane

5a(H),14b(H),17b(H)-Cholestane 20S 5α - Cholestane 5(a) Cholestane 5a-Cholestane Cholestane 5a-Cholestane 5a-Cholestane 5b(H)Cholane

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R 5α - Cholestane 5(a) Cholestane 5a-Cholestane Cholestane 5a-Cholestane 5a-Cholestane 5b(H)Cholane

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S 5α - Cholestane 5(a) Cholestane 5a-Cholestane Cholestane 5a-Cholestane 5a-Cholestane 5b(H)Cholane
81

APPENDIX C

Laboratory Notes Submitted with the Data
82

Lab Notes including data for additional analytes

1 QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 IS/surrogate 

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used 

chrysene + triphenylene 145 140 146 111 100 103 B[a]A-d12

5 QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 IS/surrogate "reprentative compound" 

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used used for quantitation

benzo[b]naphtho[2,1-d]thiophene 16.0 16.1 16.3 23.4 24.0 23.7 ACE-d10 dibenzothiophene

benzo[b]naphtho[1,2-d]thiophene 3.31 3.27 3.07 5.72 5.90 5.70 ACE-d10 dibenzothiophene

benzo[b]naphtho[2,3-d]thiophene 2.70 2.45 2.38 5.26 5.41 4.99 ACE-d10 dibenzothiophene

chrysene + triphenylene 130 139 147 155 156 168 BaP-d12

benzo[j+k]fluoranthene 31.6 33.6 33.2 62.3 62.2 61.9 BaP-d12

dibenz[a,h+a,c]anthracene 2.36 2.37 2.32 7.17 6.64 6.70 BaP-d12

1,6,7-trimethylnapthalene (also known as 2,3,5-trimethylnaphthalene, CAS # 2245-38-7), partially coelutes with another C3-naphthalene; this coeluting peak was split off during peak integration.

biphenyl is not reported due to the presence of an interference in the chromatograms introduced from the ASE.

NPH-d8 recovery range 92-96%

ACE-d10 recovery range 99-102%

BaP-d12 recovery range 91-103%

These recoveries were within the acceptable range of 60-130%

6 Benzo[ghi]perylene results (wet tissue) is below MDL of 0.60 ng/g (wet tissue) for oyster tissue 

acenaphthene MDL (wet tissue) is 0.18 ng/g

dibenz[a,h]anthracene MDL (wet tissue) is 0.55 ng/g

indeno[1,2,3-cd]pyrene MDL (wet tissue) is 0.07 ng/g

Conservative Estimate of total PAH dry basis Sample 1 5824 ng/g, sample 2 5318 ng/g, sample 3 5744 ng/g

Benzo[ghi]perylene has a consistent interferring peak, the peak area is corrected for the interference in standards and samples.

7 ALKYLATED PAH ANALYSES QA10TIS01 QA10TIS01 QA10TIS01 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

IS/surrogate 

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used 

4-methylbiphenyl 25.1 22.2 20.4 <14.8 <14.8 NA d10-Acenaphthylene

2,3,5-trimethylnaphthalene 44.2 41.7 37 <14.8 <14.8 NA d10-Acenaphthylene

1-methylfluorene 42.9 44.1 39.9 <14.8 <14.8 NA d10-Fluorene

2-methylphenanthrene 92.3 96.8 82.5 <14.8 <14.8 NA d10-Phenanthrene

3,6-dimethylphenanthrene 60.4 63.8 51.4 <14.8 <14.8 NA d10-Phenanthrene

8 Other: QA10TIS01 anthracene coeluting with an interfering peak at both quantitation and confirmation ions 178 and 177 respectively. Ion ratios out of range.

note: calibration is based on wet weight basis.

9 other = interference noted for naphthalene and benz[a]anthracene 
83

Lab Notes including data for additional analytes

10 Any values less than RL will be considered as estimated "J" values.

NA are compounds not calibrated for

Samples were analyzed at a dilution due to the matrix of the sample

11 Other = Blank contaminated with naphthalene.

12 * Percent moisture value used for the SRM Material (89.9%) was taken from the SRM Certificate of analysis.

13 (NOTES: Typical quantitation limit for all analytes in samples and SRM in this matix are <30 ng/g)

Other = An unknown interferent peak did not allow for quantitation 

14 QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass)

abb 20R 24R-methylcholestane 19.6 18.8 19.2 59.8 68.6 67.2

1,2-dimethylnaphthalene 13.7 15.4 14.3 coelution coelution coelution

3-methylphenanthrene 116 124 116 11.6 11.5 12.6

2-methylphenanthrene 143 158 140 16.9 17.6 20.3

2-methylanthracene 17.8 19.0 17.9 9.6 9.8 10.5

9-methylphenanthrene 76.1 79.4 79.0 13.0 11.7 12.7

3-methy+1-methylfluoranthene 12.5 13.8 13.2 14.0 13.5 15.0

1-methylpyrene 24.8 26.4 24.2 24.1 26.5 25.7

4-methylpyrene 13.6 14.3 13.8 15.1 16.7 16.2

3-methylchrysene 3.47 3.96 3.86 4.65 4.71 5.00

6-methylchrysene 2.97 3.20 2.98 3.60 3.85 3.69

benzo[ghi]fluoranthene 19.7 21.3 19.9 20.7 23.2 23.4

benzo[c]phenanthrene 14.8 15.4 15.1 19.1 19.6 21.2

dibenz[aj]anthracene <1.5 <1.5 <1.5 4.64 4.58 5.32

dibenz[ac]anthracene <1.5 <1.5 <1.5 4.24 4.59 3.86

benzo[b]chrysene <1.5 <1.5 <1.5 4.02 4.00 3.88

picene <1.5 <1.5 <1.5 7.98 7.78 7.98
84

Lab Notes including data for additional analytes

15 Unable to obtain SRM 1974b as NIST could not ship it across the border to Canada.

QA10TIS01 QA10TIS01 QA10TIS01

Sample 1 Sample 2 Sample 3

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass)

benzo[b&j]fluoranthene 0.031 0.021 0.029

Biomarkers calculated as ratios only:

SUMMARY 301004 1001012 1601021 601007

Terpanes Source Source Source Source Mean Std Dev RSD%

DR-27Ts/27Tm - (DR-27Ts) 1.190246359 1.228033753 1.093023256 1.284924116 1.199056871 0.080692 6.7

DR-29ab/30ab - (DR-29ab) 0.492225719 0.481056548 0.481349995 0.48606703 0.485174823 0.0052313 1.1

DR-31abS/31abR - (DR-31ab) 1.438697831 1.442665855 1.377923908 1.385527025 1.411203655 0.0342181 2.4

DR-32abS/32abR - (DR-32ab) 1.510096344 1.46006357 1.613340105 1.434011665 1.504377921 0.0792057 5.3

DR-33abS/33abR - (DR-33ab) 1.318269399 1.352325746 1.245795021 1.293989136 1.302594825 0.0447926 3.4

Steranes Source Source Source Source

DR-(27bbR + 27bbS)/(28bbR + 28bbS + 29bbR +29bbS) - (DR-27bbR) 0.706424785 0.721822493 0.723710502 0.719873991 0.717957943 0.0078467 1.1

DR-(28bbR + 28bbS)/(27bbR + 27bbS + 29bbR + 29bbS) - (DR-28bbR) 0.366375776 0.368973186 0.357914677 0.364834552 0.364524548 0.004726 1.3

DR-(29bbR + 29bbS)/(27bbR + 27bbS + 28bbR + 28bbS) - (DR-29bbR) 0.466025548 0.451915025 0.463201472 0.4579969 0.459784736 0.0062116 1.4

Triaromatic steranes Source Source Source Source

DR-C26TA(20S)/C28TA(20S) - (DR-C26TA) 0.652599192 0.632985279 0.641149081 0.627700133 0.638608421 0.0108445 1.7

DR-C27TA(20R)/C28TA(20R) - (DR-C27TA) 0.9359524 0.965588774 0.965805785 0.940931607 0.952069641 0.0158668 1.7

DR-C28TA(20R)/C28TA(20S) - (DR-C28TA) 0.764082782 0.762307853 0.763949175 0.793219152 0.770889741 0.0149081 1.9

PAHs

C3-D/C3-P - (DR-C3D/C3P) 0.199698226 0.201890811 0.200803525 0.200797521 0.0010963 0.5

C2-D/C2-P - (DR-C2D/C2P) 0.155768311 0.160931939 0.156201044 0.157633764 0.0028645 1.8

DR-27Ts DR-29ab DR-31ab DR-32ab DR-33ab DR-27bbR DR-28bbR DR-29bbR DR-C26TA DR-C27-TA DR-C28TA C3-D/C3-P C2-D/C2-P

L981972-1 1.140323092 0.809296365 1.22763466 1.942802669 1.44149766 0.6355281 0.3721401 0.5156381 0.6980482 1.2392996 0.5901263 0.1394943 0.2543507

Difference 0.058733779 -0.324121542 0.183568994 -0.438424748 -0.138902834 0.0824298 -0.007616 -0.055853 -0.05944 -0.28723 0.1807634 0.0613032 -0.096717

Critical Difference 0.163756597 0.090612983 0.184718682 0.241302641 0.192086474 0.094744 0.0515665 0.0682796 0.093566 0.1533958 0.0952711 0.0238204 0.0288389

Conclusion Match No Match Match No Match Match Match Match Match Match No Match No Match No Match No Match

L981972-2 1.350643777 0.787543882 1.169922762 1.574833174 1.461805556 0.6183365 0.3655331 0.5390136 0.866129 1.4419263 0.5693548 0.1687429 0.3083067

Difference -0.151586906 -0.865468954 0.241280892 -0.070455253 -0.15921073 0.0996214 -0.001009 -0.079229 -0.227521 -0.489857 0.2015349 0.0320546 -0.150673

Critical Difference 0.178479045 0.089090309 0.180678849 0.215544777 0.193508027 0.0935406 0.051104 0.0699159 0.1053316 0.1675797 0.0938171 0.0258678 0.0326158

Conclusion Match No Match No Match Match Match No Match Match No Match No Match No Match No Match No Match No Match

L981972-3 1.211646838 0.791306183 1.221881838 1.673452769 1.236477987 0.6592533 0.3662597 0.502869 0.8145859 1.4906977 0.5315204 0.142206 0.276259

Difference -0.012589967 -0.30613136 0.189321817 -0.169074848 0.066116838 0.0587047 -0.001735 -0.043084 -0.175977 -0.538628 0.2393693 0.0585915 -0.118625

Critical Difference 0.16874926 0.08935367 0.184315984 0.222448148 0.177735097 0.0964048 0.0511549 0.0673858 0.1017236 0.1709937 0.0911687 0.0240102 0.0303725

Conclusion Match No Match No Match Match Match Match Match Match No Match No Match No Match No Match No Match

CRITICAL DIFFERENCE ANALYSIS
85

Lab Notes including data for additional analytes

16 cis/trans decalin were calculated seperately, the sum of the isomers is reported above.

Benzo(j)fluoranthene and Benzo(k)fluoranthene co-elute - both are reported together as Benzo(k) in the tables above

Chrysene and tryphenylin co-elute, if present in both samples (as in the SRM), the amounts are a combination of the two

Dates of measurements listed above are the extraction dates of the samples - these were used as they are the start of the process.

QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 IS/surrogate % recovery

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used acceptance 

chrysene/triphenylene 106 119 99.9 112 119 110 Chrysene-d12 / Phenanthrene-d10 40 to 120

benzo[j+k ]fluoranthene 31.1 35.8 28.2 57 54.8 54.3 Chrysene-d12 / Benzo(a)pyrene-d12 40 to 120

17 Chrysene and Triphenylene cannot be chromatographically separated.

Benzo(j)fluoranthene and Benzo(k)fluoranthene cannot be chromatographically separated.

No laboratory control data exists for surrogate recoveries in this matrix; control charts from a sediment matrix utilizing the same extraction procedure were used.

Matrix interference is evident at the retention time of 1-Methylphenanthrene; results may be biased high.

QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 IS/surrogate % recovery

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used acceptance 

chrysene+triphenylene 365 392 507 120 __________ __________ Pyrene-d10 / Chrysene-d12 24%-68%

benzo[j+k ]fluoranthene 141 144 296 63.8 __________ __________ Benzo(a)pyrene-d12 / Perylene-d12 1%-73%

22 "other" = analyte co-elutes with another reported analyte. Triphenylene co-elutes with chrysene. Benzo[j]fluoranthene co-elutes with benzo[k]fluoranthene. Dibenz[a,h]anthracene co-elutes with dibenz[a,c]anthracene

QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 IS/surrogate 

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used 

chrysene + triphenylene 85.3 86.3 81.5 106 105 __________ d12-chrysene

benzo[j+k ]fluoranthene 24 25.6 24.4 48.7 50.1 __________ d12-benzo[k]fluoranthene

dibenz[a,c+a,h]anthracene 2.00 1.94 1.81 5.80 5.60 __________ d14-dibenz[a,h]anthracene

23 QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 IS/surrogate % recovery

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used acceptance 

chrysene + triphenylene 70.3 70.7 67.8 108 __________ __________ d12-Chrysene 50-120

24a Triphenylene interferes with benzo(a)anthracene and chrysene quantitation

Benzo(j)fluoranthene interferes with benzo(b)fluoranthene quantitation

26 * Triphenylene cannot be resolved from Chrysene under the chromatographic conditions used

** Benzo(j)fluoranthene cannot be resolved from Benzo(k)fluoranthene under the chromatographic condition used

QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 IS/surrogate % recovery

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used acceptance 

chrysene + triphenylene 75.9 78.3 83.7 91.5 __________ __________ Chrysene-d12/Terphenyl-d14 40-120

benzo[j+k ]fluoranthene 9.69 9.61 10.60 21.0 __________ __________ Perylene-d12Terphenyl-d14 40-120
86

Lab Notes including data for additional analytes

27 <symbol refers to values less than our MDL

The reported value of chrysene is the sum of chrysene and triphenylene

The reported value of benzo(j)fluoranthene is the sum of benzo(k)fluoranthene and benzo(j)fluoranthene

QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 IS/surrogate % recovery "reprentative compound" 

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used acceptance used for quantitation

chrysene+triphenylene 90.9 86 98 116 102 NA Pyrene-d10/Chrysene-d12 60-120 NA

benzo[j+k ]fluoranthene 15.8 14.5 13.9 55.4 55.4 NA Benzo(a)pyrene-d12/Chrysene-d12 60-120 benzo[k]fluoranthene

29 Most of our detection limits ranged ~10 to 50 ng/g dry; some were lower or as high as ~200.

Other = We used a methyl PAH cocktail to calibrate and assess recoveries. Although it did not contain C4-Naphthalenes, we measured significant amounts using the standard protocol. 

Our numbers were DL in 1974b and ~1300ng/g dry in QATISS10.

We also analyzed a suite of 28 MethylPAHs; only the above were detected.

Figures lacking three significant figures should be assumed to have lost trailing zeroes.

Chrysene and triphenylene quantified together as one chromatographic peak.

Benzo[j]fluoranthene and benzo[k]fluoranthene quantified together as one chromatographic peak.

2,6- and 2,7-methylnaphthalene were quantified together (although we do not assume both are present in samples) as one chromatographic peak.

Other Analytes:

QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 IS/surrogate 

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used 

3-MePhenanthrene 126 137 137 15.0 16.5 12.9 d10-Anthracene

benzo[g,h,i]fluoranth+cyclopenta[c,d]pyr 32.1 30.3 31.3 41.3 43.7 42.8 d10-Pyrene

Benzo[c]phenanthrene 20.1 20.7 20.0 27.5 28.7 26.8 d10-Pyrene

chrysene + triphenylene 107 106 109 123 126 118 d12-Chrysene

benzo[j+k ]fluoranthene 32.0 32.5 33.8 62.7 61.3 56.8 d12-Benzo(k)fluoranthene

32 QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass)

benzo[b+j+k]fluoranthenes <25 <26 <25 106

34 1) chrysene is reported as a coelution of both chrysene and triphenylene.

2) benzo[k]fluoranthene is reported as a coelution of both benzo[j]fluoranthene and benzo[k]fluoranthene.

3) Dibenz[a,h]anthracene is reported as a coelution of both Dibenz[a,h]anthracene and Dibenz[a,c]anthracene

QA10TIS01 QA10TIS01 QA10TIS01 SRM 1974b SRM 1974b SRM 1974b

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 IS/surrogate % recovery

(ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass) (ng/g dry mass)(ng/g dry mass) used acceptance 

chrysene/triphenylene 107 96.4 104 106 113 115 Chrysene-d12 40-120

benzo[j+k]fluoranthene 41.1 26.6 34 54 53.1 58.3 Chrysene-d12 40-120

dibenz[a,h+a,c]anthracene 4.04 2.72 4.14 7.21 4.83 4.84 Chrysene-d12 40-120
87

APPENDIX D

Charts of QA10TIS01 and SRM 1974b

Results by Analyte

See Tables 1 through 3 for results reported as <number, detection limit, etc. 

For QA10TIS01 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)
88

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

140

160

laboratory number

 mass fraction (% by mass)

Percent Water QA10TIS01

Assigned value = 86.7 % by mass s = 1.1 % by mass 95% CI = 0.4 % by mass Median value = 

86.8 % by mass

Reported Results: 34 Quantitative Results: 34 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

20

40

60

80

100

120

140

laboratory number

mass fraction (% by mass)

Percent Water SRM 1974b

Target Value = 89.9 % by mass ; 95% CI 0.1 % by mass: Median value = 89.9 % by mass

Reported Results: 29 Quantitative Results: 29 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
89

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

laboratory number

 mass fraction (ng/g dry mass)

naphthalene QA10TIS01

Assigned value = 27.2 ng/g dry mass s = 9.2 ng/g dry mass 95% CI = 4.1 ng/g dry mass Median 

value = 30.2 ng/g dry mass

Reported Results: 33 Quantitative Results: 27 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

10

20

30

40

50

60

70

80

laboratory number

mass fraction (ng/g dry mass)

naphthalene SRM 1974b

Certified Value = 24.0 ng/g dry mass ; 95% CI 1.2 ng/g dry mass: Median value = 20.7 ng/g dry mass

Reported Results: 29 Quantitative Results: 25 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
90

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

40

laboratory number

 mass fraction (ng/g dry mass)

biphenyl QA10TIS01

Assigned value = 16.6 ng/g dry mass s = 6.4 ng/g dry mass 95% CI = 3.5 ng/g dry mass Median 

value = 16.1 ng/g dry mass

Reported Results: 22 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

2

4

6

8

10

12

14

16

laboratory number

mass fraction (ng/g dry mass)

biphenyl SRM 1974b

Reference Value = 6.0 ng/g dry mass ; 95% CI 1.4 ng/g dry mass: Median value = 8.0 ng/g dry mass

Reported Results: 18 Quantitative Results: 12 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
91

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

2

4

6

8

10

12

14

16

18

laboratory number

 mass fraction (ng/g dry mass)

acenaphthene QA10TIS01

Assigned value = 9.63 ng/g dry mass s = 2.13 ng/g dry mass 95% CI = 1.11 ng/g dry mass 

Median value = 9.67 ng/g dry mass

Reported Results: 30 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

2

4

6

8

10

12

laboratory number

mass fraction (ng/g dry mass)

acenaphthene SRM 1974b

Reference Value = 2.70 ng/g dry mass ; 95% CI 0.53 ng/g dry mass: Median value = 2.66 ng/g dry 

mass

Reported Results: 22 Quantitative Results: 12 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
92

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

2

4

6

8

10

12

14

16

18

laboratory number

 mass fraction (ng/g dry mass)

acenaphthylene QA10TIS01

Assigned value = 8.88 ng/g dry mass s = 3.76 ng/g dry mass 95% CI = 1.90 ng/g dry mass 

Median value = 8.08 ng/g dry mass

Reported Results: 26 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

2

4

6

8

10

12

14

16

18

20

laboratory number

mass fraction (ng/g dry mass)

acenaphthylene SRM 1974b

Reference Value = 4.70 ng/g dry mass ; 95% CI 1.20 ng/g dry mass: Median value = 5.60 ng/g dry 

mass

Reported Results: 21 Quantitative Results: 11 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
93

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

40

45

50

laboratory number

 mass fraction (ng/g dry mass)

fluorene QA10TIS01

Assigned value = 23.4 ng/g dry mass s = 6.6 ng/g dry mass 95% CI = 2.5 ng/g dry mass Median 

value = 21.5 ng/g dry mass

Reported Results: 33 Quantitative Results: 27 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

2

4

6

8

10

12

14

16

laboratory number

mass fraction (ng/g dry mass)

fluorene SRM 1974b

Certified Value = 4.88 ng/g dry mass ; 95% CI 0.36 ng/g dry mass: Median value = 4.53 ng/g dry 

mass

Reported Results: 30 Quantitative Results: 23 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
94

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

50

100

150

200

250

laboratory number

 mass fraction (ng/g dry mass)

phenanthrene QA10TIS01

Assigned value = 120 ng/g dry mass s = 24 ng/g dry mass 95% CI = 9 ng/g dry mass Median 

value = 119 ng/g dry mass

Reported Results: 34 Quantitative Results: 33 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

10

20

30

40

50

60

70

laboratory number

mass fraction (ng/g dry mass)

phenanthrene SRM 1974b

Certified Value = 25.5 ng/g dry mass ; 95% CI 1.1 ng/g dry mass: Median value = 24.2 ng/g dry mass

Reported Results: 31 Quantitative Results: 29 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
95

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

laboratory number

 mass fraction (ng/g dry mass)

anthracene QA10TIS01

Assigned value = 12.6 ng/g dry mass s = 5.7 ng/g dry mass 95% CI = 2.4 ng/g dry mass Median 

value = 12.1 ng/g dry mass

Reported Results: 32 Quantitative Results: 25 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

2

4

6

8

10

12

14

laboratory number

mass fraction (ng/g dry mass)

anthracene SRM 1974b

Certified Value = 5.20 ng/g dry mass ; 95% CI 0.71 ng/g dry mass: Median value = 6.77 ng/g dry 

mass

Reported Results: 30 Quantitative Results: 24 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
96

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

50

100

150

200

250

300

350

400

laboratory number

 mass fraction (ng/g dry mass)

fluoranthene QA10TIS01

Assigned value = 217 ng/g dry mass s = 50 ng/g dry mass 95% CI = 17 ng/g dry mass Median 

value = 218 ng/g dry mass

Reported Results: 34 Quantitative Results: 34 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

50

100

150

200

250

300

350

400

450

laboratory number

mass fraction (ng/g dry mass)

fluoranthene SRM 1974b

Certified Value = 169 ng/g dry mass ; 95% CI 7 ng/g dry mass: Median value = 184 ng/g dry mass

Reported Results: 31 Quantitative Results: 31 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
97

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

50

100

150

200

250

300

laboratory number

 mass fraction (ng/g dry mass)

pyrene QA10TIS01

Assigned value = 146 ng/g dry mass s = 38 ng/g dry mass 95% CI = 13 ng/g dry mass Median 

value = 149 ng/g dry mass

Reported Results: 34 Quantitative Results: 34 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

50

100

150

200

250

300

350

400

450

laboratory number

mass fraction (ng/g dry mass)

pyrene SRM 1974b

Certified Value = 178 ng/g dry mass ; 95% CI 6 ng/g dry mass: Median value = 175 ng/g dry mass

Reported Results: 31 Quantitative Results: 31 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
98

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

40

laboratory number

 mass fraction (ng/g dry mass)

benzo[b]fluorene QA10TIS01

Assigned value = 20.9 ng/g dry mass s = 9.7 ng/g dry mass 95% CI = 8.5 ng/g dry mass Median 

value = 17.3 ng/g dry mass

Reported Results: 8 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

10

20

30

40

50

60

70

laboratory number

mass fraction (ng/g dry mass)

benzo[b]fluorene SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 26.7 ng/g dry mass

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
99

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

laboratory number

 mass fraction (ng/g dry mass)

benz[a]anthracene QA10TIS01

Assigned value = 36.6 ng/g dry mass s = 12.1 ng/g dry mass 95% CI = 4.7 ng/g dry mass 

Median value = 34.0 ng/g dry mass

Reported Results: 33 Quantitative Results: 28 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

20

40

60

80

100

120

140

laboratory number

mass fraction (ng/g dry mass)

benz[a]anthracene SRM 1974b

Certified Value = 46.8 ng/g dry mass ; 95% CI 5.2 ng/g dry mass: Median value = 46.5 ng/g dry mass

Reported Results: 30 Quantitative Results: 28 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
100

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

20

40

60

80

100

120

laboratory number

 mass fraction (ng/g dry mass)

chrysene QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 65.2 ng/g dry mass

Reported Results: 25 Quantitative Results: 22 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

20

40

60

80

100

120

140

laboratory number

mass fraction (ng/g dry mass)

chrysene SRM 1974b

Certified Value = 62.2 ng/g dry mass ; 95% CI 9.9 ng/g dry mass: Median value = 74.6 ng/g dry mass

Reported Results: 21 Quantitative Results: 19 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
101

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

10

20

30

40

50

60

70

80

90

laboratory number

 mass fraction (ng/g dry mass)

triphenylene QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 60.4 ng/g dry mass

Reported Results: 2 Quantitative Results: 2 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

10

20

30

40

50

60

70

80

90

100

laboratory number

mass fraction (ng/g dry mass)

triphenylene SRM 1974b

Certified Value = 42.7 ng/g dry mass ; 95% CI 7.1 ng/g dry mass: Median value = 68.9 ng/g dry mass

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
102

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

140

160

180

200

laboratory number

 mass fraction (ng/g dry mass)

chrysene/triphenylene QA10TIS01

Assigned value = 103 ng/g dry mass s = 25 ng/g dry mass 95% CI = 17 ng/g dry mass Median 

value = 105 ng/g dry mass

Reported Results: 10 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

20

40

60

80

100

120

140

160

180

laboratory number

mass fraction (ng/g dry mass)

chrysene/triphenylene SRM 1974b

Target Value = 105 ng/g dry mass ; 95% CI 10 ng/g dry mass: Median value = 110 ng/g dry mass

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
103

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

laboratory number

 mass fraction (ng/g dry mass)

benzo[b]fluoranthene QA10TIS01

Assigned value = 32.4 ng/g dry mass s = 10.5 ng/g dry mass 95% CI = 4.0 ng/g dry mass 

Median value = 30.9 ng/g dry mass

Reported Results: 33 Quantitative Results: 28 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

20

40

60

80

100

120

140

160

180

laboratory number

mass fraction (ng/g dry mass)

benzo[b]fluoranthene SRM 1974b

Certified Value = 63.8 ng/g dry mass ; 95% CI 5.8 ng/g dry mass: Median value = 58.5 ng/g dry mass

Reported Results: 31 Quantitative Results: 27 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
104

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

5

10

15

20

25

30

35

laboratory number

 mass fraction (ng/g dry mass)

benzo[j]fluoranthene QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 22.6 ng/g dry mass

Reported Results: 2 Quantitative Results: 2 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

5

10

15

20

25

30

35

40

45

laboratory number

mass fraction (ng/g dry mass)

benzo[j]fluoranthene SRM 1974b

Certified Value = 29.5 ng/g dry mass ; 95% CI 2.9 ng/g dry mass: Median value = 29.5 ng/g dry mass

Reported Results: 3 Quantitative Results: 2 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
105

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

laboratory number

 mass fraction (ng/g dry mass)

benzo[k]fluoranthene QA10TIS01

Assigned value = 15.8 ng/g dry mass s = 6.2 ng/g dry mass 95% CI = 2.8 ng/g dry mass Median 

value = 14.7 ng/g dry mass

Reported Results: 25 Quantitative Results: 21 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

10

20

30

40

50

60

70

laboratory number

mass fraction (ng/g dry mass)

benzo[k]fluoranthene SRM 1974b

Certified Value = 31.2 ng/g dry mass ; 95% CI 1.8 ng/g dry mass: Median value = 28.4 ng/g dry mass

Reported Results: 23 Quantitative Results: 19 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
106

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

laboratory number

 mass fraction (ng/g dry mass)

benzo[j+k]fluoranthene QA10TIS01

Assigned value = 28.4 ng/g dry mass s = 7.5 ng/g dry mass 95% CI = 6.0 ng/g dry mass Median 

value = 32.2 ng/g dry mass

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

20

40

60

80

100

120

laboratory number

mass fraction (ng/g dry mass)

benzo[j+k]fluoranthene SRM 1974b

Target Value = 60.7 ng/g dry mass ; 95% CI 18.0 ng/g dry mass: Median value = 55.4 ng/g dry mass

Reported Results: 8 Quantitative Results: 8 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
107

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0.0

1.0

2.0

3.0

4.0

5.0

6.0

laboratory number

 mass fraction (ng/g dry mass)

benzo[a]fluoranthene QA10TIS01

Assigned value = 3.17 ng/g dry mass s = 1.88 ng/g dry mass 95% CI = 1.84 ng/g dry mass 

Median value = 2.97 ng/g dry mass

Reported Results: 7 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

2

4

6

8

10

12

laboratory number

mass fraction (ng/g dry mass)

benzo[a]fluoranthene SRM 1974b

Certified Value = 6.26 ng/g dry mass ; 95% CI 0.73 ng/g dry mass: Median value = 6.28 ng/g dry 

mass

Reported Results: 7 Quantitative Results: 6 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
108

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

80

laboratory number

 mass fraction (ng/g dry mass)

benzo[e]pyrene QA10TIS01

Assigned value = 38.6 ng/g dry mass s = 5.9 ng/g dry mass 95% CI = 2.9 ng/g dry mass Median 

value = 39.4 ng/g dry mass

Reported Results: 25 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

20

40

60

80

100

120

140

160

laboratory number

mass fraction (ng/g dry mass)

benzo[e]pyrene SRM 1974b

Certified Value = 102 ng/g dry mass ; 95% CI 11 ng/g dry mass: Median value = 100 ng/g dry mass

Reported Results: 23 Quantitative Results: 20 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
109

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

laboratory number

 mass fraction (ng/g dry mass)

benzo[a]pyrene QA10TIS01

Assigned value = 12.3 ng/g dry mass s = 5.3 ng/g dry mass 95% CI = 2.0 ng/g dry mass Median 

value = 11.4 ng/g dry mass

Reported Results: 35 Quantitative Results: 28 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

10

20

30

40

50

60

70

laboratory number

mass fraction (ng/g dry mass)

benzo[a]pyrene SRM 1974b

Certified Value = 27.6 ng/g dry mass ; 95% CI 3.8 ng/g dry mass: Median value = 24.2 ng/g dry mass

Reported Results: 31 Quantitative Results: 27 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
110

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

2

4

6

8

10

12

14

laboratory number

 mass fraction (ng/g dry mass)

perylene QA10TIS01

Assigned value = 5.38 ng/g dry mass s = 1.64 ng/g dry mass 95% CI = 0.93 ng/g dry mass 

Median value = 5.68 ng/g dry mass

Reported Results: 25 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

2

4

6

8

10

12

14

16

laboratory number

mass fraction (ng/g dry mass)

perylene SRM 1974b

Certified Value = 9.8 ng/g dry mass ; 95% CI 1.4 ng/g dry mass: Median value = 9.85 ng/g dry mass

Reported Results: 22 Quantitative Results: 16 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
111

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

laboratory number

 mass fraction (ng/g dry mass)

indeno[1,2,3-cd]pyrene QA10TIS01

Assigned value = 8.05 ng/g dry mass s = 4.00 ng/g dry mass 95% CI = 1.85 ng/g dry mass 

Median value = 7.45 ng/g dry mass

Reported Results: 32 Quantitative Results: 22 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

10

20

30

40

50

60

70

laboratory number

mass fraction (ng/g dry mass)

indeno[1,2,3-cd]pyrene SRM 1974b

Certified Value = 21.1 ng/g dry mass ; 95% CI 1.1 ng/g dry mass: Median value = 20.6 ng/g dry mass

Reported Results: 30 Quantitative Results: 24 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
112

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

2

4

6

8

10

12

14

16

18

laboratory number

 mass fraction (ng/g dry mass)

benzo[ghi]perylene QA10TIS01

Assigned value = 8.92 ng/g dry mass s = 2.25 ng/g dry mass 95% CI = 1.04 ng/g dry mass 

Median value = 8.75 ng/g dry mass

Reported Results: 29 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

10

20

30

40

50

60

laboratory number

mass fraction (ng/g dry mass)

benzo[ghi]perylene SRM 1974b

Certified Value = 30.8 ng/g dry mass ; 95% CI 3.3 ng/g dry mass: Median value = 30.9 ng/g dry mass

Reported Results: 27 Quantitative Results: 23 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
113

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

1

2

3

4

5

6

7

8

9

laboratory number

 mass fraction (ng/g dry mass)

dibenz[a,h]anthracene QA10TIS01

Assigned value = 3.00 ng/g dry mass s = 2.07 ng/g dry mass 95% CI = 1.43 ng/g dry mass 

Median value = 2.54 ng/g dry mass

Reported Results: 28 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)

 } -30% 95% CI

 from CI

 +30%

 from CI

0

5

10

15

20

25

30

laboratory number

mass fraction (ng/g dry mass)

dibenz[a,h]anthracene SRM 1974b

Certified Value = 3.23 ng/g dry mass ; 95% CI 0.31 ng/g dry mass: Median value = 6.75 ng/g dry 

mass

Reported Results: 27 Quantitative Results: 18 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
114

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

laboratory number

 mass fraction (ng/g dry mass)

dibenz[a,h+a,c]anthracene QA10TIS01

Assigned value = 2.63 ng/g dry mass s = 0.89 ng/g dry mass 95% CI = 1.01 ng/g dry mass 

Median value = 2.35 ng/g dry mass

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

laboratory number

mass fraction (ng/g dry mass)

dibenz[a,h+a,c]anthracene SRM 1974b

Target Value = 5.32 ng/g dry mass ; 95% CI 0.13 ng/g dry mass: Median value = 5.70 ng/g dry mass

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
115

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

20

40

60

80

100

120

140

160

laboratory number

 mass fraction (ng/g dry mass)

cis/trans-decalin QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 77.6 ng/g dry mass

Reported Results: 8 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

40

45

laboratory number

mass fraction (ng/g dry mass)

cis/trans-decalin SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 2.72 ng/g dry mass

Reported Results: 7 Quantitative Results: 4 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
116

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

laboratory number

 mass fraction (ng/g dry mass)

dibenzofuran QA10TIS01

Assigned value = 17.4 ng/g dry mass s = 2.6 ng/g dry mass 95% CI = 1.9 ng/g dry mass Median 

value = 17.7 ng/g dry mass

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

laboratory number

mass fraction (ng/g dry mass)

dibenzofuran SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 8.20 ng/g dry mass

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
117

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

laboratory number

 mass fraction (ng/g dry mass)

retene QA10TIS01

Assigned value = 34.4 ng/g dry mass s = 14.4 ng/g dry mass 95% CI = 10.0 ng/g dry mass 

Median value = 30.7 ng/g dry mass

Reported Results: 12 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

10

20

30

40

50

60

laboratory number

mass fraction (ng/g dry mass)

retene SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 25.2 ng/g dry mass

Reported Results: 10 Quantitative Results: 8 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
118

 z = +1 asg value 0.0 z = -3 z = -1 z = -2 z = +3 z = +2

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

1.8

laboratory number

 mass fraction (ng/g dry mass)

benzothiophene QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 1.30 ng/g dry mass

Reported Results: 10 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

laboratory number

mass fraction (ng/g dry mass)

benzothiophene SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 0.29 ng/g dry mass

Reported Results: 8 Quantitative Results: 2 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
119

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

laboratory number

 mass fraction (ng/g dry mass)

dibenzothiophene QA10TIS01

Assigned value = 15.7 ng/g dry mass s = 3.0 ng/g dry mass 95% CI = 1.5 ng/g dry mass Median 

value = 15.8 ng/g dry mass

Reported Results: 26 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

1

2

3

4

5

6

7

laboratory number

mass fraction (ng/g dry mass)

dibenzothiophene SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 2.76 ng/g dry mass

Reported Results: 21 Quantitative Results: 12 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
120

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

laboratory number

 mass fraction (ng/g dry mass)

naphthobenzothiophene QA10TIS01

Assigned value = 14.0 ng/g dry mass s = 4.6 ng/g dry mass 95% CI = 3.7 ng/g dry mass Median 

value = 13.1 ng/g dry mass

Reported Results: 8 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

40

laboratory number

mass fraction (ng/g dry mass)

naphthobenzothiophene SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 19.0 ng/g dry mass

Reported Results: 7 Quantitative Results: 6 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
121

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

laboratory number

 mass fraction (ng/g dry mass)

1-methylnaphthalene QA10TIS01

Assigned value = 31.7 ng/g dry mass s = 11.1 ng/g dry mass 95% CI = 4.8 ng/g dry mass 

Median value = 30.1 ng/g dry mass

Reported Results: 31 Quantitative Results: 24 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

2

4

6

8

10

12

14

laboratory number

mass fraction (ng/g dry mass)

1-methylnaphthalene SRM 1974b

Reference Value = 6.06 ng/g dry mass ; 95% CI 0.49 ng/g dry mass: Median value = 4.73 ng/g dry 

mass

Reported Results: 22 Quantitative Results: 17 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
122

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

80

90

100

laboratory number

 mass fraction (ng/g dry mass)

2-methylnaphthalene QA10TIS01

Assigned value = 43.6 ng/g dry mass s = 15.3 ng/g dry mass 95% CI = 6.6 ng/g dry mass 

Median value = 43.1 ng/g dry mass

Reported Results: 31 Quantitative Results: 26 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

2

4

6

8

10

12

14

16

18

laboratory number

mass fraction (ng/g dry mass)

2-methylnaphthalene SRM 1974b

Reference Value = 12.3 ng/g dry mass ; 95% CI 0.9 ng/g dry mass: Median value = 8.93 ng/g dry 

mass

Reported Results: 22 Quantitative Results: 18 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
123

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

140

laboratory number

 mass fraction (ng/g dry mass)

2,6-dimethylnaphthalene QA10TIS01

Assigned value = 70.7 ng/g dry mass s = 24.9 ng/g dry mass 95% CI = 10.2 ng/g dry mass 

Median value = 69.7 ng/g dry mass

Reported Results: 27 Quantitative Results: 25 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

1

2

3

4

5

6

7

8

9

laboratory number

mass fraction (ng/g dry mass)

2,6-dimethylnaphthalene SRM 1974b

Reference Value = 3.3 ng/g dry mass ; 95% CI 1.6 ng/g dry mass: Median value = 5.02 ng/g dry mass

Reported Results: 20 Quantitative Results: 16 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
124

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

140

160

180

laboratory number

 mass fraction (ng/g dry mass)

1,6,7-trimethylnaphthalene QA10TIS01

Assigned value = 63.6 ng/g dry mass s = 37.6 ng/g dry mass 95% CI = 19.7 ng/g dry mass 

Median value = 46.4 ng/g dry mass

Reported Results: 19 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

1

2

3

4

5

6

7

8

9

laboratory number

mass fraction (ng/g dry mass)

1,6,7-trimethylnaphthalene SRM 1974b

Reference Value = 3.95 ng/g dry mass ; 95% CI 0.32 ng/g dry mass: Median value = 3.95 ng/g dry 

mass

Reported Results: 16 Quantitative Results: 11 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
125

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

laboratory number

 mass fraction (ng/g dry mass)

1-methylphenanthrene QA10TIS01

Assigned value = 58.5 ng/g dry mass s = 16.4 ng/g dry mass 95% CI = 8.0 ng/g dry mass 

Median value = 58.3 ng/g dry mass

Reported Results: 25 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

5

10

15

20

25

laboratory number

mass fraction (ng/g dry mass)

1-methylphenanthrene SRM 1974b

Certified Value = 9.66 ng/g dry mass ; 95% CI 1.30 ng/g dry mass: Median value = 9.32 ng/g dry 

mass

Reported Results: 22 Quantitative Results: 17 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
126

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

200

400

600

800

1000

1200

laboratory number

 mass fraction (ng/g dry mass)

C1-decalins QA10TIS01

Assigned value = 582 ng/g dry mass s = 183 ng/g dry mass 95% CI = 179 ng/g dry mass 

Median value = 554 ng/g dry mass

Reported Results: 7 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

2

4

6

8

10

12

14

16

18

20

laboratory number

mass fraction (ng/g dry mass)

C1-decalins SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 11.7 ng/g dry mass

Reported Results: 7 Quantitative Results: 4 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
127

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

500

1000

1500

2000

2500

3000

3500

laboratory number

 mass fraction (ng/g dry mass)

C2-decalins QA10TIS01

Assigned value = 1639 ng/g dry mass s = 379 ng/g dry mass 95% CI = 372 ng/g dry mass 

Median value = 1543 ng/g dry mass

Reported Results: 8 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

50

100

150

200

250

300

350

400

450

laboratory number

mass fraction (ng/g dry mass)

C2-decalins SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 82.9 ng/g dry mass

Reported Results: 8 Quantitative Results: 4 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
128

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

500

1000

1500

2000

2500

3000

3500

4000

laboratory number

 mass fraction (ng/g dry mass)

C3-decalins QA10TIS01

Assigned value = 1930 ng/g dry mass s = 766 ng/g dry mass 95% CI = 751 ng/g dry mass 

Median value = 1813 ng/g dry mass

Reported Results: 8 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

50

100

150

200

250

laboratory number

mass fraction (ng/g dry mass)

C3-decalins SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 155 ng/g dry mass

Reported Results: 8 Quantitative Results: 4 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
129

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

500

1000

1500

2000

2500

3000

3500

4000

4500

5000

laboratory number

 mass fraction (ng/g dry mass)

C4-decalins QA10TIS01

Assigned value = 2567 ng/g dry mass s = 838 ng/g dry mass 95% CI = 821 ng/g dry mass 

Median value = 2620 ng/g dry mass

Reported Results: 8 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

50

100

150

200

250

300

350

400

450

500

laboratory number

mass fraction (ng/g dry mass)

C4-decalins SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 398.8 ng/g dry mass

Reported Results: 8 Quantitative Results: 4 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
130

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

laboratory number

 mass fraction (ng/g dry mass)

C1-naphthalenes QA10TIS01

Assigned value = 59.3 ng/g dry mass s = 17.0 ng/g dry mass 95% CI = 8.9 ng/g dry mass 

Median value = 63.4 ng/g dry mass

Reported Results: 22 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

5

10

15

20

25

30

laboratory number

mass fraction (ng/g dry mass)

C1-naphthalenes SRM 1974b

Target Value = 18.4 ng/g dry mass ; 95% CI 0.9 ng/g dry mass: Median value = 9.50 ng/g dry mass

Reported Results: 16 Quantitative Results: 11 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
131

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

100

200

300

400

500

600

laboratory number

 mass fraction (ng/g dry mass)

C2-naphthalenes QA10TIS01

Assigned value = 232 ng/g dry mass s = 106 ng/g dry mass 95% CI = 47 ng/g dry mass Median 

value = 229 ng/g dry mass

Reported Results: 24 Quantitative Results: 21 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

laboratory number

mass fraction (ng/g dry mass)

C2-naphthalenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 13.6 ng/g dry mass

Reported Results: 16 Quantitative Results: 11 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
132

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

100

200

300

400

500

600

700

800

laboratory number

 mass fraction (ng/g dry mass)

C3-naphthalenes QA10TIS01

Assigned value = 386 ng/g dry mass s = 165 ng/g dry mass 95% CI = 72 ng/g dry mass Median 

value = 390 ng/g dry mass

Reported Results: 24 Quantitative Results: 23 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

20

40

60

80

100

120

140

160

laboratory number

mass fraction (ng/g dry mass)

C3-naphthalenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 29.7 ng/g dry mass

Reported Results: 17 Quantitative Results: 12 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
133

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

200

400

600

800

1000

1200

laboratory number

 mass fraction (ng/g dry mass)

C4-naphthalenes QA10TIS01

Assigned value = 552 ng/g dry mass s = 173 ng/g dry mass 95% CI = 76 ng/g dry mass Median 

value = 316 ng/g dry mass

Reported Results: 23 Quantitative Results: 22 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

50

100

150

200

250

300

350

laboratory number

mass fraction (ng/g dry mass)

C4-naphthalenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 39.9 ng/g dry mass

Reported Results: 17 Quantitative Results: 12 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
134

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

laboratory number

 mass fraction (ng/g dry mass)

C1-benzothiophenes QA10TIS01

Assigned value = 17.5 ng/g dry mass s = 3.4 ng/g dry mass 95% CI = 3.8 ng/g dry mass Median 

value = 15.7 ng/g dry mass

Reported Results: 8 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

1

2

3

4

5

6

7

8

laboratory number

mass fraction (ng/g dry mass)

C1-benzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 3.56 ng/g dry mass

Reported Results: 8 Quantitative Results: 2 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
135

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

40

45

laboratory number

 mass fraction (ng/g dry mass)

C2-benzothiophenes QA10TIS01

Assigned value = 22.2 ng/g dry mass s = 11.3 ng/g dry mass 95% CI = 12.8 ng/g dry mass 

Median value = 15.9 ng/g dry mass

Reported Results: 8 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

1

2

3

4

5

6

7

8

laboratory number

mass fraction (ng/g dry mass)

C2-benzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 3.43 ng/g dry mass

Reported Results: 8 Quantitative Results: 2 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
136

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

80

laboratory number

 mass fraction (ng/g dry mass)

C3-benzothiophenes QA10TIS01

Assigned value = 41.8 ng/g dry mass s = 18.9 ng/g dry mass 95% CI = 21.4 ng/g dry mass 

Median value = 34.9 ng/g dry mass

Reported Results: 8 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

2

4

6

8

10

12

14

laboratory number

mass fraction (ng/g dry mass)

C3-benzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 5.92 ng/g dry mass

Reported Results: 8 Quantitative Results: 2 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
137

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

80

90

laboratory number

 mass fraction (ng/g dry mass)

C4-benzothiophenes QA10TIS01

Assigned value = 45.9 ng/g dry mass s = 7.5 ng/g dry mass 95% CI = 7.3 ng/g dry mass Median 

value = 41.6 ng/g dry mass

Reported Results: 7 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

2

4

6

8

10

12

14

16

laboratory number

mass fraction (ng/g dry mass)

C4-benzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 7.05 ng/g dry mass

Reported Results: 7 Quantitative Results: 2 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
138

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

140

160

laboratory number

 mass fraction (ng/g dry mass)

C1-fluorenes QA10TIS01

Assigned value = 71.4 ng/g dry mass s = 29.3 ng/g dry mass 95% CI = 14.9 ng/g dry mass 

Median value = 72.4 ng/g dry mass

Reported Results: 24 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

10

20

30

40

50

60

70

laboratory number

mass fraction (ng/g dry mass)

C1-fluorenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 14.0 ng/g dry mass

Reported Results: 17 Quantitative Results: 12 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
139

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

50

100

150

200

250

300

350

400

laboratory number

 mass fraction (ng/g dry mass)

C2-fluorenes QA10TIS01

Assigned value = 177 ng/g dry mass s = 77 ng/g dry mass 95% CI = 37 ng/g dry mass Median 

value = 186 ng/g dry mass

Reported Results: 24 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

20

40

60

80

100

120

140

160

laboratory number

mass fraction (ng/g dry mass)

C2-fluorenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 45.4 ng/g dry mass

Reported Results: 18 Quantitative Results: 13 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
140

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

100

200

300

400

500

600

700

800

900

laboratory number

 mass fraction (ng/g dry mass)

C3-fluorenes QA10TIS01

Assigned value = 328 ng/g dry mass s = 190 ng/g dry mass 95% CI = 93 ng/g dry mass Median 

value = 287 ng/g dry mass

Reported Results: 39 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

50

100

150

200

250

laboratory number

mass fraction (ng/g dry mass)

C3-fluorenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 96.3 ng/g dry mass

Reported Results: 18 Quantitative Results: 13 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
141

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

100

200

300

400

500

600

700

800

laboratory number

 mass fraction (ng/g dry mass)

C1-phenanthrenes/anthracenes QA10TIS01

Assigned value = 331 ng/g dry mass s = 138 ng/g dry mass 95% CI = 66 ng/g dry mass Median 

value = 296 ng/g dry mass

Reported Results: 24 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI

0

20

40

60

80

100

120

140

laboratory number

mass fraction (ng/g dry mass)

C1-phenanthrenes/anthracenes SRM 1974b

Target Value = 61.3 ng/g dry mass ; 95% CI 1.8 ng/g dry mass: Median value = 49.3 ng/g dry mass

Reported Results: 18 Quantitative Results: 13 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
142

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

100

200

300

400

500

600

700

800

900

1000

laboratory number

 mass fraction (ng/g dry mass)

C2-phenanthrenes/anthracenes QA10TIS01

Assigned value = 434 ng/g dry mass s = 219 ng/g dry mass 95% CI = 99 ng/g dry mass Median 

value = 502 ng/g dry mass

Reported Results: 24 Quantitative Results: 22 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

50

100

150

200

250

300

350

400

laboratory number

mass fraction (ng/g dry mass)

C2-phenanthrenes/anthracenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 123 ng/g dry mass

Reported Results: 18 Quantitative Results: 15 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
143

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

200

400

600

800

1000

1200

laboratory number

 mass fraction (ng/g dry mass)

C3-phenanthrenes/anthracenes QA10TIS01

Assigned value = 457 ng/g dry mass s = 224 ng/g dry mass 95% CI = 107 ng/g dry mass 

Median value = 361 ng/g dry mass

Reported Results: 24 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

100

200

300

400

500

600

laboratory number

mass fraction (ng/g dry mass)

C3-phenanthrenes/anthracenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 137 ng/g dry mass

Reported Results: 18 Quantitative Results: 15 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
144

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

100

200

300

400

500

600

700

laboratory number

 mass fraction (ng/g dry mass)

C4-phenanthrenes/anthracenes QA10TIS01

Assigned value = 246 ng/g dry mass s = 170 ng/g dry mass 95% CI = 89 ng/g dry mass Median 

value = 184 ng/g dry mass

Reported Results: 23 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

100

200

300

400

500

600

laboratory number

mass fraction (ng/g dry mass)

C4-phenanthrenes/anthracenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 107 ng/g dry mass

Reported Results: 17 Quantitative Results: 14 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
145

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

140

160

180

200

laboratory number

 mass fraction (ng/g dry mass)

C1-dibenzothiophenes QA10TIS01

Assigned value = 86.8 ng/g dry mass s = 35.0 ng/g dry mass 95% CI = 19.0 ng/g dry mass 

Median value = 83.9 ng/g dry mass

Reported Results: 21 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

laboratory number

mass fraction (ng/g dry mass)

C1-dibenzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 11.3 ng/g dry mass

Reported Results: 16 Quantitative Results: 9 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
146

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

100

200

300

400

500

600

700

laboratory number

 mass fraction (ng/g dry mass)

C2-dibenzothiophenes QA10TIS01

Assigned value = 211 ng/g dry mass s = 134 ng/g dry mass 95% CI = 73 ng/g dry mass Median 

value = 226 ng/g dry mass

Reported Results: 20 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

50

100

150

200

250

laboratory number

mass fraction (ng/g dry mass)

C2-dibenzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 59.6 ng/g dry mass

Reported Results: 17 Quantitative Results: 12 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
147

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

50

100

150

200

250

300

350

400

laboratory number

 mass fraction (ng/g dry mass)

C3-dibenzothiophenes QA10TIS01

Assigned value = 196 ng/g dry mass s = 73 ng/g dry mass 95% CI = 40 ng/g dry mass Median 

value = 206 ng/g dry mass

Reported Results: 20 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

20

40

60

80

100

120

140

160

laboratory number

mass fraction (ng/g dry mass)

C3-dibenzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 91.0 ng/g dry mass

Reported Results: 17 Quantitative Results: 13 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
148

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

50

100

150

200

250

300

laboratory number

 mass fraction (ng/g dry mass)

C4-dibenzothiophenes QA10TIS01

Assigned value = 113 ng/g dry mass s = 57 ng/g dry mass 95% CI = 35 ng/g dry mass Median 

value = 109 ng/g dry mass

Reported Results: 18 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

10

20

30

40

50

60

70

80

90

100

laboratory number

mass fraction (ng/g dry mass)

C4-dibenzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 63.0 ng/g dry mass

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
149

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

50

100

150

200

250

300

350

400

laboratory number

 mass fraction (ng/g dry mass)

C1-fluoranthenes/pyrenes QA10TIS01

Assigned value = 159 ng/g dry mass s = 107 ng/g dry mass 95% CI = 54 ng/g dry mass Median 

value = 119 ng/g dry mass

Reported Results: 21 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

50

100

150

200

250

300

350

400

450

500

laboratory number

mass fraction (ng/g dry mass)

C1-fluoranthenes/pyrenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 128 ng/g dry mass

Reported Results: 18 Quantitative Results: 16 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
150

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

50

100

150

200

250

300

laboratory number

 mass fraction (ng/g dry mass)

C2-fluoranthenes/pyrenes QA10TIS01

Assigned value = 74.1 ng/g dry mass s = 31.8 ng/g dry mass 95% CI = 17.3 ng/g dry mass 

Median value = 67.7 ng/g dry mass

Reported Results: 21 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

50

100

150

200

250

300

350

400

laboratory number

mass fraction (ng/g dry mass)

C2-fluoranthenes/pyrenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 75.5 ng/g dry mass

Reported Results: 18 Quantitative Results: 13 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
151

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

laboratory number

 mass fraction (ng/g dry mass)

C3-fluoranthenes/pyrenes QA10TIS01

Assigned value = 42.5 ng/g dry mass s = 20.3 ng/g dry mass 95% CI = 11.5 ng/g dry mass 

Median value = 36.7 ng/g dry mass

Reported Results: 20 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

20

40

60

80

100

120

140

160

laboratory number

mass fraction (ng/g dry mass)

C3-fluoranthenes/pyrenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 42.0 ng/g dry mass

Reported Results: 17 Quantitative Results: 11 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
152

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

laboratory number

 mass fraction (ng/g dry mass)

C4-fluoranthenes/pyrenes QA10TIS01

Assigned value = 16.3 ng/g dry mass s = 3.9 ng/g dry mass 95% CI = 3.1 ng/g dry mass Median 

value = 16.0 ng/g dry mass

Reported Results: 11 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

10

20

30

40

50

60

laboratory number

mass fraction (ng/g dry mass)

C4-fluoranthenes/pyrenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 20.1 ng/g dry mass

Reported Results: 10 Quantitative Results: 7 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
153

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

laboratory number

 mass fraction (ng/g dry mass)

C1-naphthobenzothiophenes QA10TIS01

Assigned value = 25.2 ng/g dry mass s = 17.3 ng/g dry mass 95% CI = 15.2 ng/g dry mass 

Median value = 19.1 ng/g dry mass

Reported Results: 10 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

laboratory number

mass fraction (ng/g dry mass)

C1-naphthobenzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 28.1 ng/g dry mass

Reported Results: 9 Quantitative Results: 5 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
154

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

laboratory number

 mass fraction (ng/g dry mass)

C2-naphthobenzothiophenes QA10TIS01

Assigned value = 13.6 ng/g dry mass s = 3.4 ng/g dry mass 95% CI = 3.3 ng/g dry mass Median 

value = 13.8 ng/g dry mass

Reported Results: 10 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

laboratory number

mass fraction (ng/g dry mass)

C2-naphthobenzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 27.6 ng/g dry mass

Reported Results: 9 Quantitative Results: 5 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
155

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

2

4

6

8

10

12

14

16

laboratory number

 mass fraction (ng/g dry mass)

C3-naphthobenzothiophenes QA10TIS01

Assigned value = 8.11 ng/g dry mass s = 1.46 ng/g dry mass 95% CI = 1.65 ng/g dry mass 

Median value = 7.28 ng/g dry mass

Reported Results: 10 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

laboratory number

mass fraction (ng/g dry mass)

C3-naphthobenzothiophenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 17.7 ng/g dry mass

Reported Results: 9 Quantitative Results: 5 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
156

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

80

laboratory number

 mass fraction (ng/g dry mass)

C1-chrysenes QA10TIS01

Assigned value = 42.3 ng/g dry mass s = 9.9 ng/g dry mass 95% CI = 5.6 ng/g dry mass Median 

value = 43.5 ng/g dry mass

Reported Results: 19 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

20

40

60

80

100

120

140

160

laboratory number

mass fraction (ng/g dry mass)

C1-chrysenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 53.8 ng/g dry mass

Reported Results: 17 Quantitative Results: 12 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
157

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

40

45

50

laboratory number

 mass fraction (ng/g dry mass)

C2-chrysenes QA10TIS01

Assigned value = 26.2 ng/g dry mass s = 7.6 ng/g dry mass 95% CI = 4.5 ng/g dry mass Median 

value = 24.8 ng/g dry mass

Reported Results: 19 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

20

40

60

80

100

120

laboratory number

mass fraction (ng/g dry mass)

C2-chrysenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 40.2 ng/g dry mass

Reported Results: 17 Quantitative Results: 11 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
158

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

2

4

6

8

10

12

14

16

18

laboratory number

 mass fraction (ng/g dry mass)

C3-chrysenes QA10TIS01

Assigned value = 9.25 ng/g dry mass s = 3.14 ng/g dry mass 95% CI = 2.51 ng/g dry mass 

Median value = 6.84 ng/g dry mass

Reported Results: 19 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

laboratory number

mass fraction (ng/g dry mass)

C3-chrysenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 11.7 ng/g dry mass

Reported Results: 17 Quantitative Results: 9 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
159

 z = +1 asg value 0.0 z = -3 z = -1 z = -2 z = +3 z = +2

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

laboratory number

 mass fraction (ng/g dry mass)

C4-chrysenes QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 0.54 ng/g dry mass

Reported Results: 18 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0.0

0.5

1.0

1.5

2.0

2.5

laboratory number

mass fraction (ng/g dry mass)

C4-chrysenes SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 0.80 ng/g dry mass

Reported Results: 16 Quantitative Results: 4 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
160

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

50

100

150

200

250

laboratory number

 mass fraction (ng/g dry mass)

Carbazole QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 115 ng/g dry mass

Reported Results: 6 Quantitative Results: 2 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

laboratory number

mass fraction (ng/g dry mass)

Carbazole SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 4.40 ng/g dry mass

Reported Results: 6 Quantitative Results: 1 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
161

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

20

40

60

80

100

120

140

laboratory number

 mass fraction (ng/g dry mass)

18a(H)-22,29,30-Trisnorhopane QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 19.8 ng/g dry mass

Reported Results: 12 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0.0

5.0

10.0

15.0

20.0

25.0

laboratory number

mass fraction (ng/g dry mass)

18a(H)-22,29,30-Trisnorhopane SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 19.8 ng/g dry mass

Reported Results: 7 Quantitative Results: 3 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
162

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

10

20

30

40

50

60

70

80

90

laboratory number

 mass fraction (ng/g dry mass)

17a(H)-22,29,30-Trisnorhopane QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 22.0 ng/g dry mass

Reported Results: 11 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

40

laboratory number

mass fraction (ng/g dry mass)

17a(H)-22,29,30-Trisnorhopane SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 21.5 ng/g dry mass

Reported Results: 9 Quantitative Results: 4 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
163

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

20

40

60

80

100

120

laboratory number

 mass fraction (ng/g dry mass)

17α(H),21β(H)-30-Norhopane QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 51.2 ng/g dry mass

Reported Results: 12 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

20

40

60

80

100

120

laboratory number

mass fraction (ng/g dry mass)

17α(H),21β(H)-30-Norhopane SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 30.4 ng/g dry mass

Reported Results: 10 Quantitative Results: 5 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
164

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

10

20

30

40

50

60

70

80

90

100

laboratory number

 mass fraction (ng/g dry mass)

18a(H)-30-Norneohopane QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 48.2 ng/g dry mass

Reported Results: 9 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

40

45

50

laboratory number

mass fraction (ng/g dry mass)

18a(H)-30-Norneohopane SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 32.1 ng/g dry mass

Reported Results: 7 Quantitative Results: 2 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
165

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

20

40

60

80

100

120

140

laboratory number

 mass fraction (ng/g dry mass)

17α(H),21β(H)-Hopane QA10TIS01

Assigned value = 69.9 ng/g dry mass s = 8.3 ng/g dry mass 95% CI = 6.7 ng/g dry mass Median 

value = 68.8 ng/g dry mass

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

20

40

60

80

100

120

140

160

laboratory number

mass fraction (ng/g dry mass)

17α(H),21β(H)-Hopane SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 72.8 ng/g dry mass

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
166

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

laboratory number

 mass fraction (ng/g dry mass)

17α(H),21β(H)-22R-Homohopane QA10TIS01

Assigned value = 18.8 ng/g dry mass s = 4.8 ng/g dry mass 95% CI = 4.7 ng/g dry mass Median 

value = 19.4 ng/g dry mass

Reported Results: 12 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

40

laboratory number

mass fraction (ng/g dry mass)

17α(H),21β(H)-22R-Homohopane SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 17.9 ng/g dry mass

Reported Results: 10 Quantitative Results: 4 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
167

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

40

45

50

laboratory number

 mass fraction (ng/g dry mass)

17α(H),21β(H)-22S-Homohopane QA10TIS01

Assigned value = 24.5 ng/g dry mass s = 3.2 ng/g dry mass 95% CI = 2.8 ng/g dry mass Median 

value = 24.4 ng/g dry mass

Reported Results: 12 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

40

45

50

laboratory number

mass fraction (ng/g dry mass)

17α(H),21β(H)-22S-Homohopane SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 25.4 ng/g dry mass

Reported Results: 10 Quantitative Results: 5 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
168

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

10

20

30

40

50

60

laboratory number

 mass fraction (ng/g dry mass)

13b(H)17a(H)-Diacholestane 20S QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 18.2 ng/g dry mass

Reported Results: 9 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

2

4

6

8

10

12

14

16

laboratory number

mass fraction (ng/g dry mass)

13b(H)17a(H)-Diacholestane 20S SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 13.1 ng/g dry mass

Reported Results: 7 Quantitative Results: 3 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
169

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

5

10

15

20

25

30

35

laboratory number

 mass fraction (ng/g dry mass)

5a(H),14a(H),17a(H)-Cholestane 20S QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 28.0 ng/g dry mass

Reported Results: 8 Quantitative Results: 2 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

laboratory number

mass fraction (ng/g dry mass)

5a(H),14a(H),17a(H)-Cholestane 20S SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 21.7 ng/g dry mass

Reported Results: 7 Quantitative Results: 3 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
170

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

80

laboratory number

 mass fraction (ng/g dry mass)

5a(H),14a(H),17a(H)-Cholestane 20R QA10TIS01

Assigned value = 42.2 ng/g dry mass s = 7.2 ng/g dry mass 95% CI = 6.3 ng/g dry mass Median 

value = 38.2 ng/g dry mass

Reported Results: 12 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

40

45

laboratory number

mass fraction (ng/g dry mass)

5a(H),14a(H),17a(H)-Cholestane 20R SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 28.7 ng/g dry mass

Reported Results: 10 Quantitative Results: 6 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
171

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

laboratory number

 mass fraction (ng/g dry mass)

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S QA10TIS01

Assigned value = 15.4 ng/g dry mass s = 4.4 ng/g dry mass 95% CI = 4.3 ng/g dry mass Median 

value = 14.6 ng/g dry mass

Reported Results: 10 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

laboratory number

mass fraction (ng/g dry mass)

5a(H),14a(H),17a(H)-24-Ethylcholestane 20S SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 10.0 ng/g dry mass

Reported Results: 8 Quantitative Results: 3 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
172

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

laboratory number

 mass fraction (ng/g dry mass)

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R QA10TIS01

Assigned value = 37.2 ng/g dry mass s = 16.3 ng/g dry mass 95% CI = 14.3 ng/g dry mass 

Median value = 30.0 ng/g dry mass

Reported Results: 11 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

10

20

30

40

50

60

70

laboratory number

mass fraction (ng/g dry mass)

5a(H),14a(H),17a(H)-24-Ethylcholestane 20R SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 34.3 ng/g dry mass

Reported Results: 9 Quantitative Results: 5 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
173

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

10

20

30

40

50

60

70

laboratory number

 mass fraction (ng/g dry mass)

5a(H),14b(H),17b(H)-Cholestane 20R QA10TIS01

Assigned value = 18.3 ng/g dry mass s = 1.5 ng/g dry mass 95% CI = 1.7 ng/g dry mass Median 

value = 18.8 ng/g dry mass

Reported Results: 12 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

30

35

laboratory number

mass fraction (ng/g dry mass)

5a(H),14b(H),17b(H)-Cholestane 20R SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 13.4 ng/g dry mass

Reported Results: 10 Quantitative Results: 4 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
174

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

10

20

30

40

50

60

70

laboratory number

 mass fraction (ng/g dry mass)

5a(H),14b(H),17b(H)-Cholestane 20S QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 18.8 ng/g dry mass

Reported Results: 9 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

2

4

6

8

10

12

14

16

laboratory number

mass fraction (ng/g dry mass)

5a(H),14b(H),17b(H)-Cholestane 20S SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 13.8 ng/g dry mass

Reported Results: 7 Quantitative Results: 3 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
175

 asg value

 z = +1

 z = -1

 z = +2

 z = -2

 z = +3

 z = -3

0

5

10

15

20

25

30

35

laboratory number

 mass fraction (ng/g dry mass)

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R QA10TIS01

Assigned value = 16.3 ng/g dry mass s = 6.7 ng/g dry mass 95% CI = 6.6 ng/g dry mass Median 

value = 16.4 ng/g dry mass

Reported Results: 12 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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

laboratory number

mass fraction (ng/g dry mass)

5a(H),14b(H),17b(H)-24-Ethylcholestane 20R SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 17.1 ng/g dry mass

Reported Results: 10 Quantitative Results: 4 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
176

 z = +1 asg value 0 z = -3 z = -1 z = -2 z = +3 z = +2

5

10

15

20

25

laboratory number

 mass fraction (ng/g dry mass)

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S QA10TIS01

Assigned value = No Target ng/g (dry mass) Median value = 19.1 ng/g dry mass

Reported Results: 9 Quantitative Results: 2 

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)

 } 95% CI

 -30%

 from CI

 +30%

 from CI 0

5

10

15

20

25

laboratory number

mass fraction (ng/g dry mass)

5a(H),14b(H),17b(H)-24-Ethylcholestane 20S SRM 1974b

Target Value = no target ng/g (dry mass): Median value = 18.9 ng/g dry mass

Reported Results: 7 Quantitative Results: 2 

Solid line: value from Certificate of Analysis ; dotted line: 95% confidence limits; dashed line: 30% 

from 95% confidence limits
177

Appendix E

Participants in the Sediment Interlaboratory Study QA10OIL01 in 

Alphabetical Order by Organization

Alpha Analytical, Inc.

320 Forbes Blvd

Mansfield, MA 02048

Elizabeth Porta

ALS Environmental Division

5424 97th St. NW

Edmonton, AB T6E 5C1 CANADA

Deib Birkholz / Sarah Stilson

Analytical Resources, Inc.

4611 S. 134th Place, Suite 100

Tukwila, WA 98168-03240

Susan D. Dunnihoo

Arizona Department of Health Services Laboratory

250 North 17th Avenue

Phoenix, AZ 85007

Aneddail Torres-Ayala/ Jason Mihalic

Axys Analytical Services

2045 Mills Road West

Sydney, B.C Canada

Dale Hoover

Battelle Analytical & Environmental Chemistry Laboratory

397 Washington Street

Duxbury, MA 02332

Jonathan Thorn

CA Animal Health & Food Safety Laboratory (CAHFS)

Toxicology / Thurman Bldg.

West Health Sciences Drive

Davis, CA 95616

Linda Aston

Columbia Analytical Services (CAS)

9143 Philips Highway, Suite 200

Jacksonville, FL 32256

Joe Wiegel / Karenya Fedele
178

Columbia Analytical Services (CAS)

1 Mustard Street, Ste. 250

Rochester, NY 14609

Mike Perry

Columbia Analytical Services (CAS)

1317 South 13th Avenue

Kelso, WA 98626

Greg Salata / Julie Gish

FDA / Arkansas Regional Laboratory

3900 NCTR Road

Jefferson, AR 72079

Russell Fairchild / Greg Satterfield 

FDA / Denver District Laboratory

Bldg 20 Denver Federal Center 

Denver, CO 80225

Patrick Ayres

FDA / Kansas City District Laboratory

11510 W.80th Street

Lenexa, KS 66214

Rachel Dietzel /

FDA / Southeast Regional Laboratory

60 8th Street NE

Atlanta, GA 30309

Jim Holcomb / Tiffany Harmon

Florida Department of Environmental Protection

2600 Blair Stone Road

Tallahassee, FL 32399-2400

Liang Lin / Timothy Fitzpatrick 

Michigan Department of Natural Resources and Environment

Bureau of Laboratories

927 Terminal Drive

Lansing, MI 48906

Bonita Taffe

Mississippi State Chemical Laboratory 

310 President’s Circle

Mississippi State, MS 39762

Christina Childers / Kang Xia / Gale Hagood
179

New York State Department of Health

Biggs Laboratory Room D-539

Wadsworth Center

Empire State Plaza

Albany, NY 12237

Kenneth Aldous / Anthony Bucciferro

NIST / Hollings Marine Laboratory

331 Fort Johnson Road

Charleston, SC 29412

John Kucklick

NIST

100 Bureau Drive, MS 8392

Gaithersburg, MD 20899-8392

Michele Schantz

NOAA/NCCOS/NOS

Chemical Contaminants Research Program

Center for Coastal Environmental Health and Biomolecular Research

331 Fort Johnson Road

Charleston, SC 29412

Ed Wirth / Dan Liebert

NOAA/NMFS/NW Fisheries Science Center

2725 Montlake Blvd. East

Seattle, WA 98112-2097

Jennie Bolton / Catherine Sloan / Gina Yitalo

TDI/B&B Laboratories, Inc

1902 Pinon

College Station, TX 77845

Juan Ramirez

TestAmerica Laboratories

900 Lakeside Drive

Mobile, AL 36693

Charles Newton / Eron Schellinger

TestAmerica Laboratories

880 Riverside Parkway 

West Sacramento, CA 95605

Karla Buechler / Robert Hrabak
180

TestAmerica Laboratories

2417 Bond Street

University Park, IL 60484

Michael Healy / Terese Preston 

TestAmerica Laboratories

301 Alpha Drive

RIDC Park

Pittsburgh, PA 15238

Larry Matko / Sharon Bacha

TestAmerica Laboratories

5815 Middlebrook Pike

Knoxville, TN 37921

Tom Yoder/ David Wiles

TestAmerica Laboratories

30 Community Drive

Suite 11

South Burlington, VT 05403

Bryce Stearns

TestAmerica Laboratories

5755 8th Street East

Tacoma, WA 98424

Kathy Kreps / Coleen McKean

Texas A&M University

Geochemical and Environmental Research Group

833 Graham Road

College Station, TX 77845

Terry Wade / Jóse Sericano 

University of Iowa

State Hygienic Laboratory

#H 101 OH, 102 Oakdale Campus

Iowa City, Iowa 52242-5002

Michael Wichman

US Army Engineer Research and Development Center

Environmental Chemistry Branch

3909 Halls Ferry Road 

Vicksburg, MS 39180

Anthony Bednar / Patricia Tuminello / Allyson Harrison
181

USGS Columbia Environmental Research Center

4200 New haven Road

Columbia, MO 65201

David Alvarez
182