NISTIR 7642

Description and Results of the 2007 NIST/NOAA Interlaboratory 

Comparison Exercise Program for Organic Contaminants in 

Marine Mammal Tissues 

John R. Kucklick 

Rebecca S. Pugh 

Paul R. Becker 

Michele M. Schantz 

Stephen A. Wise 

Teresa K. Rowles 

 
NISTIR 7642 

Description and Results of the 2007 NIST/NOAA Interlaboratory 

Comparison Exercise Program for Organic Contaminants in 

Marine Mammal Tissues 

John R. Kucklick 

Rebecca S. Pugh 

Paul R. Becker 

National Institute of Standards and Technology 

Chemical Science and Technology Laboratory 

Analytical Chemistry Division 

Charleston Laboratory 

Michele M. Schantz 

Stephen A. Wise 

National Institute of Standards and Technology 

Chemical Science and Technology Laboratory 

Analytical Chemistry Division 

Teresa K. Rowles 

National Oceanic and Atmospheric Administration 

National Marine Fisheries Service 

March 2009
ii

TABLE OF CONTENTS 

LIST OF APPENDICES ............................................................................................................ III

LIST OF TABLES ...................................................................................................................... IV

ABSTRACT .............................................................................................................................. VII

INTRODUCTION......................................................................................................................... 1

MATERIALS USED IN THE 2007 EXERCISE ....................................................................... 1

EVALUATION OF THE EXERCISE RESULTS ..................................................................... 2

RESULTS AND DISCUSSION ................................................................................................... 7

CONCLUSIONS AND FUTURE EXERCISES ........................................................................ 9

LITERATURE CITED ................................................................................................................ 9
iii

LIST OF APPENDICES 

A. Tabular results of PCB congener, pesticide, PBDE congener, and lipid data reported 

by all laboratories ...............................................................................................................A1-A36 

B. Graphical results of PCB congener and lipid data reported by all laboratories. The 

Z-scores for Homogenate VIII represent 25% of the as signed value so that z = +1 is 

the assigned value plus 25 % , z = -1 is th e assigned value minus 25 % and so f orth. 

Error bars are ± 1 standard deviation. ..............................................................................B1-B28 

C. Graphical results of pesticide and lipid data reported by all labo ratories. T he Zscores for Homogenate VIII represent 25% of the assigned value so that z = +1 is the 

assigned value plus 25 % , z = -1 is the assigned value minus 25 % and so forth. 

Error bars are ± 1 standard deviation ...............................................................................C1-C18 

D. Graphical results of PBDE congener data reported by all laboratories. The Z-scores 

for Homog enate VIII represent 2 5% of the assigned value so th at z = +1 is the 

assigned value plus 25 % , z = -1 is the assigned value minus 25 % and so forth. 

Error bars are ± 1 standard deviation ...............................................................................D1-D5 

E. Tabular summary of methods used for analysis by each laboratory ..............................E1-E7 

F. Additional analyte data and notes reported by individual laboratories .........................F1-F8 
iv

LIST OF TABLES 

Table 1: Laboratories Particip ating in th e NIST/NOAA Interlaboratory 

Comparison Exercise Program for Organic Contaminants .......................................................3 

Table 2a,b: Target and Optional Analytes for the NIST/NOAA 

Interlaboratory Comparison Exercise Program for Organic Contaminants in 

Marine Mammal Tissues .................................................................................................................4-5 

Table 3: Median organochlorine pesticid e and lipid concentrations in 

Homogenate VIII (Female pilot whale; ng/g w et mass) reported by each 

laboratory. The values in bold were no t used to derive the consens us value 

(see text for explanation).. ...............................................................................................................11 

Table 4: Median PCB congener co ncentrations in Homogenate VIII (Female 

pilot whale; ng/g wet mass) reported by each laboratory. The values in bold 

were not used to derive the consensus value (see text for explanation) ......................................12 

Table 5: Median PBDE conge ner co ncentrations in Homogen ate VIII 

(Female pilot whale; ng/g wet mass) reported by each laboratory. The values 

in bold were not used to derive the consensus value (see text for explanation). ........................13 

Table 6: Median organochlorine pestic ide and lipid co ncentrations in SRM 

1945 determined by each laboratory (ng/g w et mass and percent (mass 

fraction), respectively).. ...................................................................................................................14 

Table 7: Table 7: Median PCB congener concentrations in SRM 1945 

determined by each laboratory (ng/g wet mass). ........................................................................15 

Table 8: Median PBDE congener con centrations in SRM 1945 determined 

by each laboratory (ng/g wet mass). .............................................................................................16 

Table 9: Results from the analysis of Homogenate VIII (Female pilot whale ) 

for fatty a cids. Values are in percen t (mass fractio n). Fatty acids not 

requested for the exercise are given in Appendix F... ...................................................................17 

Table 10: Results from the analysis of SRM 1945 for fatty acids. Values are 

in percent (mass fraction). Fatty acid s not requested for the ex ercise a re 

given in Appendix F. 2003 and 2005 values also shown.... ..........................................................18 

Table 11: Median organochlorine pesticid e and lipid concentrations in 

MMCM-1 Serum (Female pilo t whale; pg /g w et mass) reported by each 

laboratory. The values in bold were no t used to derive the consens us value 

(see text for explanation)..... ............................................................................................................19 
v

Table 12: Median PCB congener concentrations in MMCM-1 Serum 

(Female pilot whale; pg/g wet mass) reported by each laboratory. The values 

in bold were not u sed to derive the consensus value (se e text fo r 

explanation)..... .................................................................................................................................20 

Table 13: Median PBDE congener concentrations in MMCM-1 Serum 

(Female pilot whale; pg/g wet mass) reported by each laboratory. The values 

in bold were not u sed to derive the consensus value (see text fo r 

explanation)..... .................................................................................................................................21 

Table 14: Median organochlorine pestic ide and lipid concentrations in SRM 

1958 determined by each laboratory (pg/g w et mass and percent (mass 

fraction), respectively). .... ..............................................................................................................22 

Table 15: Median PCB congener concentrations in SRM 1958 determined by 

each laboratory (pg/g wet mass)..... ................................................................................................23 

Table 16: Median PBDE congener con centrations in SRM 1958 determined 

by each laboratory (pg/g wet mass)..... ...........................................................................................24 
vi

DISCLAIMER 

Certain commercial equipment or instruments are identified in this report to specify adequately 

the experimental procedures. Such identification does not imply recommendations or 

endorsement by the National Institute of Standards and Technology nor does it imply that the 

equipment or instruments are the best available for the purpose. 
vii

ABSTRACT 

The National Institute of Standards and Technology (NIST), in support of the National Oceanic 

and Atmospheric Administration’s Marine Mammal Health and Stranding Response Program 

(NOAA/MMHSRP), conducts annual interlaboratory comparison exercises for the determination 

of chlorinated pesticides, polychlorinated biphenyl congeners (PCBs), and trace elements in 

marine mammal tissues. These exercises provide one mechanism for laboratories to evaluate 

their measurement quality and comparability for these constituents in marine mammal tissues. In 

the 2007 exercise, 21 data sets were submitted by 14 laboratories on requested organohalogen 

compounds in marine mammal blubber and serum or fatty acids in marine mammal blubber. The 

materials distributed for the 2007 exercise included SRM 1945 Organics in Whale Blubber, SRM 

1958 Human Serum (Fortified), a homogenized blubber control material “Marine Mammal 

Quality Assurance Exercise Homogenate VIII” (Homogenate VIII) from a Female pilot whale 

and “Marine Mammal Control Material 1-Serum” (MMCM1-serum) also derived from a Female 

pilot whale . This report includes the results reported by the participating laboratories, combined 

consensus data results, and summary statistics for each analyte in the samples. The numerical 

indices used to assess laboratory performance are also discussed. 
1

INTRODUCTION 

Laboratories measuring organic contaminants in the marine environment must assess the 

accuracy and precision of their measurements. Quality control of measurements made on marine 

environmental samples is vital to the accurate assessment of marine pollution and its effects on 

wildlife and human health. NIST aims to improve the quality of analytical measurements 

performed on the marine environment by developing improved analytical methods, producing 

NIST Standard Reference Materials (SRMs) and other control materials, and conducting annual 

interlaboratory comparison exercises. 

Through the NIST National Marine Analytical Quality Assurance Program and with support 

from the NOAA Marine Mammal Health and Stranding Response Program (MMHSRP), NIST 

conducts interlaboratory comparison activities to include analyses of marine mammal tissues. 

The 2007 NIST/NOAA Interlaboratory Comparison Exercise Program for Organic Contaminants 

in Marine Mammal Tissues was modeled after previous exercises (e.g., Schantz et al., 1996; 

Schantz et al., 2002; Kucklick et al., 2002, Kucklick et al., 2006, Kucklick et al., 2007). The 

current exercise was designed to help laboratories assess data comparability and quality relative 

to other groups providing measurements of organochlorine contaminants on marine mammal 

tissues and to link these important measurements to a national metrology laboratory. The results 

of the exercises presented in this report should be useful for both assessing current methodology 

and reducing the variability of contaminant data reported on marine mammals. Future exercises 

will allow for the assessment of analytical data quality over time. This report summarizes the 

2007 organic contaminant exercise including methods used for analysis, data reported by the 

laboratories on the intercomparison materials, and numerical indices used to assess laboratory 

performance. A report describing the 2007 trace element results of this exercise is also available 

(contact Steven Christopher, steven.christopher@nist.gov). 

MATERIALS USED IN THE 2007 EXERCISE 

The 2007 NIST/NOAA Interlaboratory Comparison Exercise for Organochlorines in Marine 

Mammal Tissues (2007 MMQA) used four materials distributed to 18 laboratories. Twenty-one 

data sets from 14 laboratories were submitted for this exercise (Table 1). Thirteen data sets were 

submitted for organohalogen compounds in blubber exercise, five for the organohalogens in 

serum, and three for fatty acid compounds in blubber. Participants were asked to make three 

measurements each on two materials: SRM 1945 “Organics in Whale Blubber” and MMQA-VIII 

(Homogenate VIII), the “unknown.” MMQA-VIII was originally designated MMQA-IV, but is 

relabeled here as MMQA-VIII to be consistent with past exercises. Participants were asked to 

make three measurements each on two materials: SRM 1945 “Organics in Whale Blubber” and 

MMQA-VIII the “unknown.” The unknown material was prepared from blubber taken from a 

350 cm female pilot whale. The animal stranded alive on the beach at Pea Island, NC (35° 

69.228’ N 75° 48.359’ W) and was euthanized on November 18, 1999. Other details on this 

material are given elsewhere (Kucklick et al., 2002). One bottle of this material containing 

approximately 10 g along with one bottle of SRM 1945 were sent either on dry ice or using a 

liquid nitrogen-cooled biological dry shipper via overnight express to each participating 

laboratory. In addition to the blubber materials, one bottle of SRM 1958 Human Serum 

(Fortified) and three vials of Marine Mammal Serum Unknown I (MMCM-1 Serum) were sent to 

laboratories participating in this portion of the exercise. Each serum vial contained 
2

approximately 5 mL of serum obtained from an adult male sea lion (Zalophus californianus). 

Samples were distributed in the spring of 2007. 

Exercise Requirements and Target Analytes 

A suite of analytes was chosen for the exercise based on those tested in prior exercises (Schantz 

et al., 1996; Schantz et al., 2002; Kucklick et al., 2002; Kucklick et al., 2006, Kucklick et al., 

2007) and several additional analytes were included to broaden this list (Table 2a). In addition to 

the compounds listed in Table 2a, participants were requested to provide, if possible, values for 

polybrominated diphenyl ether (PBDE) congeners, coplanar polychlorinated biphenyl (PCB) 

congeners, total toxaphene and toxaphene congeners, chlorinated dioxins and furans and fatty 

acids (Table 2b). Laboratories were requested to make triplicate measurements of these 

compounds in each of the materials and to report their data using a data template provided by 

NIST. 

EVALUATION OF THE EXERCISE RESULTS 

Determination of Laboratory Means and Consensus Values for Homogenate VIII 

Each laboratory reported the results of their analyses (Sample 1, Sample 2, and Sample 3) and 

the mean for each laboratory was calculated. The consensus value was calculated after 

comparing the results from an individual laboratory’s analysis of SRM 1945 and SRM 1958 to 

the certified or reference value for the target organohalogens compounds given on the Certificate 

of Analysis for SRMs 1945 and 1958. If the value of a compound from a given laboratory’s 

analysis for the SRM was within 30 % of the reference value, the laboratory’s result for the 

unknown sample was included in the calculation of the consensus value for the unknowns. The 

median value for each compound was then calculated (Tables x-y). 

For the fatty acid portion of the exercise, the consensus value was not derived after screening the 

data as above as NIST has not determined fatty acids in SRM 1945 and the existing data sets 

from other laboratories are limited. 

Reported Results 

Laboratories were assigned a random numerical identification code to shield the identity of the 

participants with the exception of NIST which is listed as laboratories 1, 2, and 1s. The results 

from the analysis of Homogenate VIII, SRM 1945, MMCM-1 Serum, and SRM 1958 are 

summarized in Tables 3 through 16. Appendix A shows the tabulated results from the individual 

laboratories for all materials and the results are shown graphically in Appendices B, C, and D for 

blubber only. Graphs were not constructed for the serum portion of the exercise due to the 

relatively small number of participants (n=5); tabular results are shown in Tables 11 through16. 

Appendix E gives the methods used for analysis by each laboratory and Appendix F shows data 

for additional analytes and notes. 
3

Table 1: Laboratories Participating in the 2005 NIST/NOAA Interlaboratory Comparison 

Exercise Program for Organic Contaminants. 

Mississippi State Chemical Lab 

Mississippi State, Mississippi, USA 

Southern California Coastal Water Research Project 

Costa Mesa, California, USA 

NOAA/National Ocean Service 

Hollings Marine Laboratory 

Charleston, South Carolina, USA 

Institute of Ocean Sciences 

Fisheries and Oceans 

Sydney, British Columbia, Canada 

NOAA/National Marine Fisheries Service 

Highlands, New Jersey, USA 

NOAA/National Marine Fisheries Service 

Northwest Fisheries Science Center 

Seattle, Washington, USA 

National Wildlife Research Center 

Science and Technology Branch 

Wildlife Toxicology and Disease Division 

Ottawa, Ontario, Canada 

NIST 

Hollings Marine Laboratory 

Charleston, South Carolina, USA 

NOAA/National Ocean Service 

Center for Coastal Environmental Health and 

Biomolecular Research 

Charleston, South Carolina, USA 

NIST 

Gaithersburg, Maryland, USA 

Toxicological Center 

University of Antwerp (UA) 

Wilrijk, Belgium

CRG Marine Laboratories, Inc 

Torrance, California, USA 

Veterinary Medical Center 

Michigan State University 

East Lansing, Michigan, USA 

Centre for Environment, Fisheries and Aquaculture 

Science 

CEFAS Burnham Laboratory 

Essex, UK
4

Table 2a: Target Analytes for the NIST/NOAA Interlaboratory Comparison Exercise Program 

for Organic Contaminants in Marine Mammal Tissues. 

Pesticides PCB Congeners Substitution 

2,4’-DDT 18 2,2’,5 

4,4’-DDT 28 2,4,4’ 

2,4’-DDE 31 2,4’,5 

4,4’-DDE 44 2,2’,3,5’ 

2,4’-DDD 49 2,2’,4,5’ 

4,4’-DDD 52 2,2’,5,5’ 

HCB 66 2,3’,4,4’ 

-HCH 87 2,2’,3,4,5’ 

-HCH 95 2,2’,3,5’,6l 

-HCH 99 2,2’,4,4’,5 

heptachlor epoxide 101 2,2’,4,5,5’ 

cis-chlordane 105 2,3,3’,4,4’ 

trans-chlordane 118 2,3’,4,4’,5 

oxychlordane 128 2,2’,3,3’,4,4’ 

cis-nonachlor 132 2,2’,3,3’,4,6’ 

trans-nonachlor 138 2,2’,3,4,4’,5’ 

dieldrin 149 2,2’,3,4’,5’,6 

Mirex 151 2,2’,3,5,5’,6 

 153 2,2’,4,4’,5,5’ 

 156 2,3,3’,4,4’,5 

 170 2,2’,3,3’,4,4’,5 

 180 2,2’,3,4,4’,5,5’ 

 183 2,2’,3,4,4’,5’,6 

 187 2,2’,3,4’,5,5’,6 

 194 2,2’,3,3’,4,4’,5,5’ 

 195 2,2’,3,3’,4,4’,5,6 

 201 2,2’,3,3’,4,5,5’,6’ 

 206 2,2’,3,3’,4,4’,5,5’,6 

 209 2,2’,3,3’,4,4’,5,5’,6,6’ 
5

Table 2b : Optional Analytes for the NIST/NOAA Interlaboratory Comparison Exercise 

Program for Organic Contaminants in Marine Mammal Tissues. 

Compound Subs titution Compound Subs titution 

Polybrominated 

Diphenyl Ethers 

 To xaphene 

PBDE 47 2,2’,4,4’ Total toxaphene 

PBDE 99 2,2’,4,4’,5 Toxaphene Congener 26 2-endo,3-exo,5-endo,6-

exo,8,8,10,10-

Octachlorobornane 

PBDE 100 2,2’,4,4,’6 Toxaphene Congener 50 2-endo,3-exo,5-endo,6-

exo,8,8,9,10,10-

Nonachlorobornane 

PBDE 153 2,2’,4,4’,5,5’ Toxaphene Congener 62 2,2,5,5,8,9,9,10,10-

Nonachlorobornane 

PBDE 154 2,2’,4,4’,5,6’ 

 Coplanar PCBs 

Fatty Acids PCB 77 3,3’,4,4’ 

Lauric acid C12:0 PCB 126 3,3’,4,4’,5 

Myristic acid C14:0 PCB 169 3,3’,4,4’,5,5’ 

Pentadecanoic acid C15:0 

Palmitic acid C16:0 

Chloro Dioxins and 

Furans 

Margaric acid C17:0 

Hexabromocyclodocecane 

Isomers (-, -, and 

Stearic acid C18:0 

Arachidic acid C20:0 

Palmitoleic acid C16:1(n-7) 

Vaccenic acid C18:1(n-7) 

Oleic acid C18:1(n-9) 

Elaidic acid C18:1(n-9) 

 C20:1(n-7) 

Gondoic C20:1(n-9) 

Gadoleic acid C:20:1(n-11) 

Erucic acid C22:1(n-9) 

Cetoleic C22:1(n-11) 

Nervonic acid C24:1(n-9) 

Linoleic acid C18:2(n-6) 

a-Linolenic acid C18:3(n-3) 

g-linolenic acid C18:3(n-6) 

Stearidonic acid C18:4(n-3) 

Homo-gamma-linoleic 

acid C20:2(n-6) 

 

Homo-alpha-linolenic acid C20:3(n-3) 

Arachidonic acid C20:4(n-6) 

EPA C20:5(n-3) 

 C22:2(n-6) 

DPA C22:5(n-3) 

DHA C22:6(n-3) 
6

Assignment of z-and p-scores 

Performance Scores: Different programs have different data quality needs. The acceptability of 

the results submitted by a laboratory will be decided by the individual program(s) for which the 

laboratory provides data. Typically, the program will use these exercise results in conjunction 

with the laboratory’s performance in the analysis of certified reference materials and/or control 

materials, and of other quality assurance samples. These exercise results are shown in a number 

of ways in this report to aid in the evaluation of data quality. 

IUPAC guidelines (IUPAC 1993) describe the use of “z-scores” and “p-scores” for assessment 

of accuracy and precision in interlaboratory comparison exercises, such as described in this 

report. These indices assess the difference between the result of the laboratory and the exercise 

assigned value, and can be used, with caution, to compare performance on different analytes and 

on different materials. 

Accuracy Assessment (z-score):

z = bias estimate / performance criterion 

 

or 

 

z = (x - X)/

    

where x is the individual laboratory result, X is the “Exercise Assigned Value,” and  is the 

target value for the standard deviation. As described in the IUPAC guidelines, the choice of  is 

dependent upon the data quality objective of a particular program. It can be fixed or determined 

by reference to validated methodology (e.g., the calculated  from the exercise data, see Tables x 

through y). 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 more 

problematic than usual. 

The z-scores calculated using both approaches and applied to each laboratory’s data are given in 

Appendix A. The same criterion was adopted for use in this exercise as was used in the former 

NIST/NOAA/NS&T program, where the target standard deviation was set to 25 % of the 

exercise assigned value. The z-scores for the Homogenate VIII represent 25 % of the assigned 

value so that z = +1 is the assigned value plus 25 %, z = -1 is the assigned value minus 25 % and 

so forth. z-scores are also calculated based on the standard deviation of an analyte in the 

unknown material such that z = +1 is one “exercise standard deviation” higher than the assigned 

value and z = -1 is one “exercise standard deviation” lower than the assigned value and so forth. 

From a scientific point of view, IUPAC does not recommend the classification of z-scores, but 

does allow for such classification, e.g.,

z Satisfactory 

z Questionable 
7

z Unsatisfactory 

The tables in Appendix A summarize the results and performance indices including the number 

of analytes that fall within each category for each laboratory for organohalogens in both the 

serum and blubber portions of the exercise. 

Precision Assessment (p-score):

 p = lab / target ≈ CVlab/ CVtarget

 

where lab and target are variance estimates for the individual laboratory and the target variance, 

respectively. The CVlab is the coefficient of variance (or ratio of standard deviation to the mean), 

while the CVtarget is a target value chosen by the participants. During the workshop that 

accompanied this exercise, a target CV of 15 % was agreed upon, which is the same value used 

by other NIST run exercise programs (Schantz et al., 1996; Schantz et al., 2002; Kucklick et al., 

2002; Kucklick et al., 2006, Kucklick et al., 2007). Note that the precision that p describes is 

that which occurs within a batch of analyses. Between-batch variance is likely larger and was 

not assessed in this exercise. 

RESULTS AND DISCUSSION 

Summarized results are shown in Tables 3 through 16 for the compounds listed in Tables 2a and 

2b. Tabular results for individual laboratories are given in Appendix A, graphical results are 

given in Appendices B, C and D, and methods used by individual laboratories along with 

additional data and notes are given in Appendices E and F, respectively. Thirteen data sets were 

submitted for the organohalogens in blubber portion, five sets of results were submitted for the 

serum samples and three data sets were submitted for the fatty acid portion of the exercise. 

Thirteen data sets were submitted for pesticides, 12 for PCB congeners, and 12 for the requested 

PBDE congeners. The number of submissions for the PBDEs in blubber was up from eight data 

sets in 2005 indicating that the analysis of the PBDEs is becoming more routine. Three 

laboratories had not participated in the exercise before. For the 2005 exercise, 17 data sets were 

submitted for the organohalogen portion (PCB congeners and organochlorine pesticides) of the 

exercise and four data sets were submitted for the fatty acid portion (Kucklick et al., 2007). 

The laboratories used a variety of methods to analyze the samples (Appendix E). For extraction, 

eight laboratories used pressurized fluid extraction, three used Soxhlet extraction, two used a 

column elution technique. For the serum, laboratories used a variety of extraction techniques 

including microwave extraction, liquid/liquid extraction, column elution, pressurized fluid 

extraction, and solid phase extraction (see Appendix E for greater detail). The fatty acid 

extraction used by laboratories was also variable and included pressurized fluid extraction, 

homogenization with solvent, and an unspecified method. Most data sets (from serum and 

blubber) used internal standards (15), three laboratories used external standards, and three 

laboratory used a combination of internal and external standards. For detection of 

organohalogen compounds, the most commonly used technique was gas chromatography-mass 
8

spectrometry (GC-MS; 16 data sets), followed by GC-electron capture detection (GC-ECD; two 

data sets). In the 2005 exercise, seven laboratories used GC-ECD relative to only two in the 

2007 exercise indicating more routine use of GC-MS. For fatty acid determination, GC-MS was 

used in two data sets for quantification and GC-flame ionization detection (GC-FID) was used by 

one lab. All laboratories employing GC used capillary columns ranging in length form 25 m to 

60 m. For organohalogen analysis, the most commonly used column was a 5 % phenyl methyl 

polysiloxane phase. 

Based on the consensus values, Homogenate VIII had considerably higher concentrations of total 

pesticides, PCBs, and PBDE congeners relative to SRM 1945 (Tables 3-8; Appendices B 

through D). The factor differences between Homogenate VIII and SRM 1945 (i.e., Homogenate 

VIII concentration/SRM 1945 concentration) were 19.8, 20.9, and 2.5 for the total 

organochlorine pesticides, total PCB congeners, and PBDE congeners, respectively, listed on 

Tables 3-8. The difference are most likely due to the reproductive status of the two animals 

used; SRM 1945 was collected from a mature female pilot whale while Homogenate VIII female 

pilot whale which may not have had offspring thereby maintain a relatively larger contaminant 

concentration. For the serum, the factor differences of total pesticides, PCBs, and PBDEs of 

MMCM-1 Serum relative to SRM 1958 were 3.23, 4.61, and 7.7, respectively, indicating much 

greater concentrations of the organohalogen compounds in the marine mammal serum than in the 

amended human serum SRM. 

The relative scatter of reported values seemed similar among compounds with some exceptions. 

The reported values for lipid (See Appendix C) were less than for the organohalogen 

compounds. PCB congener 201 showed somewhat of a bimodal distribution of values 

(Appendix A). For SRM 1945, the certified value for this compound is 16.8 ng/g ± 1.3 ng/g. 

However, most laboratories reported much greater values near to 80 ng/g for this compound. As 

in previous exercise, it is likely that the laboratories were using the Zell and Ballschmiter 

nomenclature (Guitart et al., 1993) and are actually reporting the value for IUPAC congener 199 

that has a reference value of 84.8 ng/g ± 2.2 ng/g in SRM 1945. For the 2007 exercise, 10 

laboratories submitted data for the PBDEs which is two more laboratories than in 2005 

(Kucklick et al., 2006). Relative to past exercises, the agreement among laboratories for the 

measurement of PBDE congeners appears to be improving. However, there is still a great deal of 

scatter in the reported values of PBDE 47 and 154 (Appendix D). The scatter for PBDE 47 

among laboratories is surprising as this is the most abundant PBDE present in the materials. 

With regard to PBDE 154, an overestimation of the PBDE 154 concentration can result if 

laboratories are not separating this congener from polybrominated biphenyl 153. 

This is the third exercise in which fatty acid analysis was requested. The values for individual 

fatty acids in SRM 1945 were on average within 3 % of the median of the 2003 and 2005 results. 

The largest deviations were for -linolenic and gadoleic acids which were reported to be 16 % 

lower and 15 % lower in this exercise relative to the 2003 and 2005 exercises. 
9

CONCLUSIONS AND FUTURE EXERCISES 

Fourteen-one laboratories submitted data for exercise materials reporting data on a wide variety 

of organic constituents including PCBs, pesticides, fatty acids, and PBDE congeners. The 

repeated participation of many laboratories in the exercise suggests that the exercise has been a 

useful tool for assessing their analytical performance. A new exercise will be conducted in 2009 

using SRM 1945 and a new unknown material. If possible, serum will also be distributed. 

However the collection of serum is more difficult than of blubber. The materials will be 

distributed in the spring of 2009 with the data due at the end of 2009. 

 

LITERATURE CITED 

Christopher, S.J., Pugh, R.S., Ellisor, M.B., Mackey, E.A., Spatz, R.O., Porter, B.J., Bealer, K.J., 

Kucklick, J.R., Becker, P.R., and Rowles, T.K. National Marine Analytical Quality 

Assurance Program: Results and Description of the 2005 NIST/NOAA Interlaboratory 

Comparison Exercise for Trace Elements in marine Mammals. National Institute of 

Standards and Technology, NISTIR 7361. 

Guitart, R., Puig, P., and Gomez-Catalan, J. Requirement for a Standardized Nomenclature 

Criterion for PCBs: Computer-Assisted Assignment of Correct Congener Denomination and 

Numbering. Chemosphere 27:1451-1459 (1993). 

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

Analytical Laboratories; Pure & Appl. Chem. 65:123-2144 (1993). 

Kucklick, J.R., Christopher, S.J., Becker, P.R., Pugh, R.S., Porter, B.J., Schantz, M.M., Mackey, 

E.A., Wise, S.A., Rowles, T.K. Description and Results of the 2000 NIST/NOAA 

Interlaboratory Comparison Exercise Program for Organic Contaminants and Trace Elements 

in Marine Mammal Tissues. National Institute of Standards and Technology, NISTIR 6849 

(2002). 

Kucklick J.R., Tuerk K.J.S., Vander Pol S.S, Schantz M.M., Wise SA. Polybrominated diphenyl 

ether congeners and toxaphene in selected marine standard reference materials. Anal. 

Bioanal. Chem. 378:1147-1151 (2004). 

Kucklick, J.R., Pugh, R.S., Becker, P.R., Schantz, M.M., Wise, S.A., and Rowles, T.K., 

Description and Results of the 2003 NIST/NOAA Interlaboratory Comparison Exercise 

Program for Organic Contaminants in Marine Mammal Tissues. National Institute of 

Standards and Technology, NISTIR 6849 (2002). 

Kucklick, J.R., Pugh, R.S., Becker, P.R., Schantz, M.M., Wise, S.A., and Rowles, T.K., 

Description and Results of the 2003 NIST/NOAA Interlaboratory Comparison Exercise 
10

Program for Organic Contaminants in Marine Mammal Tissues. National Institute of 

Standards and Technology, NISTIR 7269 (2006). 

Kucklick, J.R., Pugh, R.S., Becker, P.R., Poster, D.L., Schantz, M.M., Wise, S.A., and Rowles, 

T.K., Description and Results of the 2005 NIST/NOAA Interlaboratory Comparison 

Exercise Program for Organic Contaminants in Marine Mammal Tissues. National Institute 

of Standards and Technology, NISTIR 7410 (2007). 

Schantz, M.M., Wise, S.A., Segstro, M., Muir, D.C.G., and Becker, P.R. Interlaboratory 

Comparison Study for PCB Congeners and Chlorinated Pesticides in Beluga Whale Blubber. 

Chemosphere 33:1369-1390 (1996). 

Schantz, M.M., Kucklick, J.R., Parris, R.M., and Wise, S.A. NIST Intercomparison Exercise 

Program for Organic Contaminants in the Marine Environment. Description and Results of 

2000 Organic Intercomparison Exercise. National Institute of Standards and Technology 

NISTIR 6837 (2002). 

Zeisler, R., Langland, J.K., and Harrison, J.K. Cryogenic Homogenization Procedure for 

Biological Tissues. Anal. Chem. 60: 2760-2765 (1983). 
Compound 1 2 3 4 5 6 7 8 9 10 11 12 13 Median 1 SD 2,4’-DDT 1372 1355 1007 1293.3 968 no data 1193 2510 1206.7 1033 1115 1107 no data 1193 428 

4,4’-DDT 1991 2043 2017 1327 1915 2161 2753 5875 2177 1761 2432 2113 72.0 2043 1276 2,4’-DDE 410 439 379 305 560 no data 459 400 547 382 389 503 no data 410 78 

4,4’-DDE 23820 23356 19500 21567 25259 21140 29200 18639 24000 16700 23983 22633 841 22633 6783 

2,4’-DDD 444 433 342 443 250 no data 381 324 472 437 297 385 no data 385 71 

4,4’-DDD 1738 1804 1417 Interference 1271 1780 1783 1533 2230 1530 1630 1677 <10 1677 250 

HCB 285 270 249 197 380.6 250 343 262 354 156 256 no data no data 262 66 

alpha-HCH 9.42 8.56 5.72 Interference <2.06 21.9 6.75 no data 13.4 8.73 5.27 no data <10 8.65 5.5 

beta-HCH 38.4 38.8 39.3 43.8 <1.20 no data 37.8 47.6 48.0 44.2 33.9 no data <10 39.3 4.8 gamma-HCH 5.94 5.70 3.73 DL <1.91 21.4 4.03 57.3 <6.4 7.73 3.70 no data <10 5.82 19 Heptachlor Epoxide 12.9 14.1 69.4 12.2 118 no data no data 68.9 111 67.5 no data no data <10 68.2 43 Cis-Chlordane 90.5 90.7 109 49.3 88.3 no data 149 93.4 141 58.3 no data no data <10 90.7 33 Trans-Chlordane 22.5 20.6 8.73 32.8 12.5 no data 9.39 7.30 10.2 9.95 no data no data <10 10.2 8.6 Oxychlordane 77.9 79.7 61.9 54.4 76.1 no data no data 59.0 90.1 55.3 39.0 no data no data 61.9 16 Cis-Nonachlor 90.5 137 194 Interference 102 no data 174 167 233 143 no data no data no data 155 47 

Trans-Nonachlor 390 391 441 378 729 no data 409 436 624 500 294 no data no data 423 128 Dieldrin 389 411 395 Interference 1008 327 426 410 603 43.2 no data no data <10 410 256 Mirex 55.3 56.0 62.2 Interference 35.0 no data 44.7 43.8 67.7 28.9 no data no data no data 50.0 13 

Lipid 65.9 68.6 67.7 66.2 65.0 68.0 75.6 73.7 70.4 68.1 71.4 71.0 no data 68.3 3.2 

Table 3: Median organochlorine pesticide and lipid concentrations in Homogenate VIII (female pilot whale; ng/g wet mass) reported by each laboratory. The values in bold were not used to derive the consensus value (see text for explanation)
Table 4: Median PCB congener concentrations in Homogenate VIII (female pilot whale; ng/g wet mass) reported by each laboratory. The values in bold were not used to derive the consensus value (see text for explanation).

Compound 1 2 3 4 5 6 7 8 9 10 11 12 13 Median 1 SD 18 13.5 13.6 9.40 29.2 10.8 19 6.48 11.0 13.7 10.4 8.83 no data no data 11.0 6.2 

28 25.3 25.5 24.5 16.0 Interference 15.0 20.4 15.5 32.1 18.4 21.6 no data no data 21.0 5.5 31 <1 3.76 1.72 10.0 Interference 4.15 0.63 no data no data 8.04 no data no data no data 3.95 3.6 44 36.0 35.9 32.1 56.2 47.1 43.3 30.9 24.6 40.6 30.7 31.5 no data no data 35.9 9.0 49 103 103 91 108 107 111 no data 69.6 92.9 96.7 92.1 no data no data 99.7 12 52 343 341 285 327 340.9 272 271 220.0 317 292 302 no data no data 302 38 

66/95* see below below see below 658.7 Interference 130 see below see below see below see below see below no data no data 395 374 

87 263 232 218 Interference Interference no data 241 181 451 106 236 no data no data 234 98 

99 897 878 671 695 700 no data 861 482 1293 684 697 no data no data 699 217 101 (+90) 1482 1416 1043 Interference Interference 1163 no data 880 2197 1060 1220 no data no data 1192 410 105 378 376 377 282 346 366 314 245 760 494 389 no data no data 376 138 118 1135 1198 1240 1380 Interference 1246 1357 996 2567 1323 1283 no data no data 1264 435 128 474 475 473 301 Interference 563 436 395 950 527 512 no data no data 474 171 132 w/153 791 no data w/153 Interference no data 431 no data no data 251 481 no data no data 456 225 138 (+163+164) 4503 4505 4990 3177 8140 4414 6137 3983 6990 3493 4137 no data no data 4503 1526 149 3133 3124 2877 2413 2519 2218 2430 1880 4633 2443 2610 no data no data 2519 726 151 1003 1013 802 798 673 736 801 554 1380 697 806 no data no data 801 222 153 8625 7620 6967 4260 Interference 6709 5393 5650 13567 6540 7517 no data no data 6838 2534 156 208 213 220 118 211 236 230 151 371 397 237 no data no data 220 82 170 (+190) 1553 1070 1300 810 1105 1520 1303 1172 2460 1320 1219 no data no data 1300 423 180 3922 3781 3360 2350 Interference 3754 3613 2776 7120 3507 4116 no data no data 3684 1274 183 948 926 932 521 778 852 701 675 1583 783 856 no data no data 852 270 187 2955 2879 2527 1777 2718 2674 2370 1972 4997 2493 2843 no data no data 2674 833 194 356 353 312 242 309 320 334 253 504 323 311 no data no data 320 68 195 111 110 95.7 231 86.1 no data 94.0 65.3 no data 129 92.7 no data no data 95.7 48 

201 87.5 93.8 no data 282 421 no data 439 48.2 148 390 456 no data no data 282 169 

206 35.0 34.8 38.5 28.3 32.8 no data 25.5 22.1 51.7 36.2 34.4 no data no data 34.6 8.1 

209 13.8 14.4 13.3 12.8 13.8 no data 12.0 no data 10.8 7.99 12.8 no data no data 12.8 2.0 66 151 248 117 see above 162 no data 99.2 111 217.0 253 no data no data no data 157 62 

95 682 656 518 see above Interference no data 532 385 no data 382 534 no data no data 532 117 
Compound 1 2 3 4 5 6 7 8 9 10 11 12 13 Median 1 SD n 

PBDE 47 150 150 208 155 184 147 142 61.6 107 228 143 100 no data 149 45.5 12 

PBDE 99 20.6 21.1 26.8 no data 22.4 22.7 24.8 49.5 22.8 10.8 20.1 20.6 no data 22.4 9.4 11 PBDE 100 28.6 28.8 32.8 no data 27.6 24.7 28.9 26.7 30.9 33.4 25.3 21.5 no data 28.6 3.5 11 PBDE 153 7.16 7.19 6.04 no data 6.97 7.80 7.16 10.73 6.47 <0.5 7.27 6.20 no data 7.16 1.3 10 PBDE 154 21.5 no data 23.2 no data 30.4 23.0 21.8 25.4 18.0 43.2 20.7 11.3 no data 22.4 8.4 10 

Table 5: Median PBDE congener concentrations in Homogenate VIII (female pilot whale; ng/g wet mass) reported by each laboratory. The values in bold were not used to derive the consensus value (see text for ex
Table 6: Median organochlorine pesticide and lipid concentrations in SRM 1945 determined by each laboratory (ng/g wet mass and percent (mass fraction), respectively). 

Compound 1 2 3 4 5 6 7 8 9 10 11 12 13 Median 1 SD ± 95% CI 2,4’-DDT 101 92.6 85.1 67.7 118.4 no data 89 135 79.9 122 68.2 69.4 no data 88.7 23 14 4,4’-DDT 238 240 240 117 223 225 302 416.3 239 225 226 186 no data 232 70 40 2,4’-DDE 13.3 13.7 14.0 10.8 15.9 no data 15.2 14.5 15.3 13.0 12.6 13.5 no data 13.7 1.4 0.8 4,4’-DDE 513 507 508 413 583 481 693 509 551 466 460 399 21.7 507 154 84 2,4’-DDD 20.0 20.0 20.0 19.1 19.9 no data 20.9 22.9 22.3 11.7 15.9 17.9 no data 20.0 3.1 1.8 4,4’-DDD 120 122 150 Interference 162 116 125 104 133 121 103 115 no data 121 18 11 HCB 30.6 30.4 26.7 24.9 35.9 26.7 37.2 27.8 39.1 30.6 23.6 no data no data 30.4 5.1 3.0 alpha-HCH 16.3 16.2 15.0 Interference 13.0 30.4 18.4 no data 19.1 16.1 13.5 14.6 no data 16.2 5.0 3.1 beta-HCH <5 <4 Interference 8.61 8.75 no data 2.04 no data <10 9.36 1.63 no data no data 8.61 3.9 3.4 

gamma-HCH 3.14 2.99 2.48 DL <1.91 28.7 3.05 no data <2.9 5.17 3.27 3.10 no data 3.12 9.0 6.2 

Heptachlor Epoxide 10.7 10.2 10.2 4.37 14.5 no data no data 11.8 15.8 14.3 no data 7.33 no data 10.7 3.6 2.4 Cis-Chlordane 48.5 48.9 56.5 32.4 26.5 no data 78.8 49.0 59.3 36.8 no data 11.3 no data 48.7 18.9 11.7 Trans-Chlordane 12.1 11.8 12.0 13.8 3.1 no data 12.4 10.4 10.7 13.7 no data 34.5 no data 12.0 8.0 5.0 Oxychlordane 22.2 21.9 20.0 15.7 17.9 no data no data 19.7 23.1 20.7 13.7 17.6 no data 19.9 3.0 1.9 Cis-Nonachlor 48.5 46.8 58.3 Interference 41.1 no data 54.3 49.3 51.0 51.2 no data 37.9 no data 49.3 6.3 4.1 Trans-Nonachlor 199 203 181 125.7 213.4 no data 222 166 189 171 123 205 no data 189 33 20 Dieldrin 50.7 50.5 52.0 Interference 44.3 44.3 60.1 48.2 57.5 32.3 no data 50.4 no data 50.5 7.7 5 Mirex 34.5 33.6 40.1 Interference 22.7 no data 32.8 31.2 <50 22.3 no data 36.5 no data 33.2 6.3 4.4 Lipid 70.7 71.2 72.9 70.9 72.7 72.2 82.2 74.8 69.4 72.2 68.9 78.2 no data 72.2 3.7 1.9 
Table 7: Median PCB congener concentrations in SRM 1945 determined by each laboratory (ng/g wet mass). 

Congener 1 2 3 4 5 6 7 8 9 10 11 12 13 Median 1 SD ± 95% CI 18 3.88 3.98 2.64 4.37 6.44 2.77 1.88 2.37 <8.5 2.96 3.10 8.63 no data 3.10 2.0 1.2 28 12.3 12.5 11.5 6.72 Interference 5.35 10.1 4.30 14.9 11.3 9.67 11.2 no data 11.2 3.2 1.9 31 3.39 3.41 3.45 2.34 Interference 4.25 3.04 3.53 no data 7.57 no data 3.63 no data 3.45 1.5 1.0 44 11.7 11.9 12.1 13.7 20.7 9.2 10.7 8.3 15.6 11.8 11.1 15.3 no data 11.8 3.3 1.9 49 18.2 18.2 17.5 15.5 23.0 18.5 no data 12.1 18.1 19.7 16.8 15.5 no data 18.1 2.7 1.6 52 41.4 42.3 40.8 31.7 42.4 40.4 33.8 26.9 39.5 35.8 37.3 38.4 no data 38.9 4.8 2.7 66/95* see below below see below 48.5 Interference 21.1 see below see below see below see below see below see below no data 34.8 19 

87 22.8 20.6 23.6 Interference Interference no data 22.2 18.8 17.6 15.6 20.6 18.7 no data 20.6 2.6 1.7 

99 63.5 61.5 56.3 47.7 56.8 no data 64.5 43.5 46.1 57.8 49.5 43.1 no data 56.3 8.0 5 101 (+90) 86.7 84.6 87.5 Interference Interference 79.7 no data 62.9 66.9 74.4 77.5 67.1 no data 77.5 9.2 6 105 28.6 28.6 28.7 12.8 26.8 29.7 22.0 18.9 27.2 48.2 27.1 26.8 no data 27.1 8.3 4.7 118 75.1 76.3 86.2 70.0 Interference 84.1 82.8 65.9 74.3 88.5 77.5 71.5 no data 76.3 7.1 4 128 22.1 22.5 25.2 18.2 Interference 29.9 18.3 20.3 21.1 29.3 21.8 21.5 no data 21.8 3.9 2.3 132 w/153 21.4 no data w/153 Interference no data 15.9 no data no data 21.3 17.5 10.6 no data 17.5 4.5 4 138 (+163+164) 146 150 192 92.7 269 160 192 136 108 130 124 133 no data 141 47 27 149 92.1 93.2 89.9 71.4 83.4 78.8 70.8 60.9 68.6 88.9 79.2 70.9 no data 79.0 11 6 151 29.4 29.1 27.2 23.2 31.2 21 23 20.9 20.3 27.6 23.8 22.9 no data 23.5 3.8 2.1 153 268 223 260 119.7 Interference 208 195 201 186 207 201 210 no data 207 39 23 156 11.1 11.2 13.2 5.22 20.1 10.9 10.2 6.83 8.93 25.7 11.2 8.03 no data 11.0 5.7 3 170 (+190) 43.4 43.0 45.5 20.8 35.6 50.2 42.1 37.2 39.1 45.7 34.4 35.2 no data 40.6 7.6 4 180 140 138 166 91.6 Interference 161 149 112 137 156 148 123 no data 140 22.2 13 183 38.7 39.1 42.1 20.0 24.7 41.4 31.0 29.5 32.0 41.4 34.2 31.6 no data 33.1 7.0 4.0 187 132 127 145 75 123 118 107 91 109 128 121 112 no data 120 18.8 11 194 58.2 53.0 66.9 33.8 52.1 61.2 56.6 43.4 43.7 66.3 53.3 43.4 no data 53.2 10.1 6 195 13.5 13.9 11.1 19.3 11.3 no data 8.60 6.37 no data 15.5 8.77 13.1 no data 12.2 3.8 2.3 201 16.8 16.7 no data 36.5 73.4 no data 75.6 8.87 14.7 89.97 80.0 12.0 no data 26.6 33 21 206 48.9 47.1 62.2 29.0 50.4 no data 71.2 30.9 41.5 52.6 50.0 43.4 no data 48.9 12 7.2 209 18.4 18.1 20.1 13.6 17.5 no data 17.7 no data 12.0 10.5 18.0 13.6 no data 17.6 3.2 2.0 66 21.9 22.1 22.6 see above 24.7 no data 17.5 21.4 24.6 25.6 no data 22.1 no data 22.1 2.4 1.6 95 33.1 33.8 37.1 see above Interference no data 36.2 26.8 no data 30.6 34.6 29.9 no data 33.4 3.5 2.4 
Table 8: Median PBDE congener concentrations in SRM 1945 determined by each laboratory (ng/g wet mass). 

Ref

Congener 1 2 3 4 5 6 7 8 9 10 11 12 13 Median 1 SD ± 95% CI n VPBDE 47 39.5 38.9 42.1 44.1 53.2 39.0 41.3 26.1 42.9 64.9 39.7 33.1 no data 40.5 9.6 5.4 12 3PBDE 99 17.9 18.1 21.2 19.5 17.8 18.7 22.4 16.2 18.5 6.92 18.0 15.9 no data 18.0 3.8 2.2 12 1PBDE 100 9.75 9.89 12.3 10.4 10.4 9.23 11.4 5.08 12.7 23.0 9.80 10.7 no data 10.4 4.2 2.4 12 1PBDE 153 8.68 8.51 7.36 non detect 8.9 9.7 9.6 7.29 9.82 21.4 9.53 7.90 no data 8.94 3.9 2.3 11 8PBDE 154 13.0 w/PBB 153 14.5 non detect 22.4 15.7 13.8 16.5 13.7 22.3 12.8 12.7 no data 14.2 3.7 2.3 10 1
Table 9: Results from the analysis of Homogenate VIII (female pilot whale) for fatty acids. Values are in percent (mass fraction). 

Fatty Acid Lab 1fa Lab 2a Lab 3fa Lauric acid Dodecanoic acid C12:0 0.130 0.107 0.255 Myristic acid Tetradecanoic acid C14:0 2.65 2.31 2.50 Pentadecanoic acid Pentadecanoic acid C15:0 0.330 0.287 0.318 Palmitic acid Hexadecanoic acid C16:0 8.27 7.46 7.97 Margaric acid Heptadecanoic acid C17:0 0.272 0.267 0.605 Stearic acid Octadecanoic acid C18:0 1.60 1.51 1.60 Arachidic acid Eicosanoic acid C20:0 0.102 0.091 0.117 Palmitoleic acid (Z)-9-Hexadecanoic acid C16:1(n-7) 7.23 6.27 7.41 Vaccenic acid (Z)-11-Octadecenoic acid C18:1(n-7) 1.71 1.56 no data Oleic acid (Z)-9-Octadecanoic acid C18:1(n-9) 17.0 15.7 17.8 Elaidic acid (E)-9-Octadecenoic acid C18:1(n-9) no data no data 0.12 

(Z)-13-eicosenoic acid C20:1(n-7) 0.18 0.19 no data 

Gondoic (Z)-11-eicosenoic acid C20:1(n-9) 3.24 3.07 3.39 Gadoleic acid (Z)-9-Eicosenoic acid C:20:1(n-11) 1.04 1.06 no data Erucic acid (Z)-13-Docosenoic acid C22:1(n-9) 0.430 0.370 0.472 Cetoleic (Z)-11-docosenoic acid C22:1(n-11) 2.15 2.09 no data Nervonic acid (Z)-15-Tetracosenoic acid C24:1(n-9) 0.179 0.139 0.229 Linoleic acid (Z,Z)-9,12-Octadecadienoic acid C18:2(n-6) 0.679 0.584 0.784 a-Linolenic acid (Z,Z,Z)-9,12,15-Octadecatrienoic acid C18:3(n-3) 0.277 0.236 0.288 g-linolenic acid (Z,Z,Z)-6,9,12-Octadecatetraenoic acid C18:3(n-6) 0.019 no data 0.02 Stearidonic acid (Z,Z,Z,Z,)-6,9,12,15-Octadecatetraenoic acid C18:4(n-3) 0.144 0.225 no data Homo-gamma-linoleic acid (Z,Z)-11,14-Eicosadienoic acid C20:2(n-6) 0.214 0.170 0.203 Homo-alpha-linolenic acid (Z,Z,Z)-11,14,17-Eicosatrienoic acid C20:3(n-3) 0.150 0.121 0.162 Arachidonic acid (Z,Z,Z,Z)-5,8,11,14-Eicosatetraenoic acid C20:4(n-6) 0.347 0.314 0.516 EPA (Z,Z,Z,Z,Z)-5,8,11,14,17-Eicosapentaenoic acid C20:5(n-3) 1.70 1.60 2.02 

(Z,Z)-13,16-Docosadienoic acid C22:2(n-6) 0.021 no data no data 

DPA (Z,Z,Z,Z,Z)-7,10,13,16,19-Docosapentaenoic acid C22:5(n-3) 0.59 0.55 0.78 DHA (Z,Z,Z,Z,Z,Z)-4,7,10,13,16,19-Docosahexaenoic Acid C22:6(n-3) 4.44 3.91 6.27 
Table 10: Results from the analysis of SRM 1945 for fatty acids. Values are in percent (mass fraction). Fatty acids not requested for the exercise are given in Appendix F. 2003 and 2005 values also s

Fatty Acid Lab 1fa Lab 2fa Lab 3fa Median 1 SD Median Lauric acid Dodecanoic acid C12:0 0.181 0.155 0.226 0.181 0.04 0.198 Myristic acid Tetradecanoic acid C14:0 3.49 3.12 3.32 3.32 0.18 3.44 Pentadecanoic acid Pentadecanoic acid C15:0 0.331 0.301 0.316 0.316 0.02 0.365 Palmitic acid Hexadecanoic acid C16:0 7.69 7.43 7.47 7.47 0.14 7.13 Margaric acid Heptadecanoic acid C17:0 0.214 0.241 0.539 0.241 0.18 0.252 Stearic acid Octadecanoic acid C18:0 1.26 1.25 1.32 1.26 0.03 1.36 Arachidic acid Eicosanoic acid C20:0 0.093 0.092 0.111 0.093 0.01 0.108 Palmitoleic acid (Z)-9-Hexadecanoic acid C16:1(n-7) 6.36 5.73 6.52 6.36 0.42 6.47 Vaccenic acid (Z)-11-Octadecenoic acid C18:1(n-7) 1.89 1.81 no data 1.85 2.04 Oleic acid (Z)-9-Octadecanoic acid C18:1(n-9) 14.3 14.2 14.8 14.3 0.31 16.7 Elaidic acid (E)-9-Octadecenoic acid C18:1(n-9) no data no data 0.08 0.08 0.207 

(Z)-13-eicosenoic acid C20:1(n-7) 0.22 0.24 no data 0.23 

Gondoic (Z)-11-eicosenoic acid C20:1(n-9) 4.74 4.73 5.15 4.74 0.24 5.04 Gadoleic acid (Z)-9-Eicosenoic acid C:20:1(n-11) 2.90 3.01 no data 2.96 1.41 Erucic acid (Z)-13-Docosenoic acid C22:1(n-9) 0.584 0.535 0.675 0.584 0.07 0.702 Cetoleic (Z)-11-docosenoic acid C22:1(n-11) 4.36 4.59 no data 4.47 4.12 Nervonic acid (Z)-15-Tetracosenoic acid C24:1(n-9) 0.213 0.185 0.265 0.213 0.04 0.305 Linoleic acid (Z,Z)-9,12-Octadecadienoic acid C18:2(n-6) 0.824 0.754 0.930 0.824 0.09 0.912 a-Linolenic acid (Z,Z,Z)-9,12,15-Octadecatrienoic acid C18:3(n-3) 0.352 0.317 0.393 0.352 0.04 0.618 g-linolenic acid (Z,Z,Z)-6,9,12-Octadecatetraenoic acid C18:3(n-6) 0.016 no data no data 0.02 0.018 Stearidonic acid (Z,Z,Z,Z,)-6,9,12,15-Octadecatetraenoic acid C18:4(n-3) 0.149 0.230 no data 0.189 0.184 Homo-gamma-linoleic acid (Z,Z)-11,14-Eicosadienoic acid C20:2(n-6) 0.226 0.183 0.213 0.213 0.02 0.244 Homo-alpha-linolenic acid (Z,Z,Z)-11,14,17-Eicosatrienoic acid C20:3(n-3) 0.148 0.126 0.183 0.148 0.03 0.181 Arachidonic acid (Z,Z,Z,Z)-5,8,11,14-Eicosatetraenoic acid C20:4(n-6) 0.231 0.221 0.356 0.231 0.08 0.303 EPA (Z,Z,Z,Z,Z)-5,8,11,14,17-Eicosapentaenoic acid C20:5(n-3) 1.16 1.12 1.38 1.16 0.14 1.44 

(Z,Z)-13,16-Docosadienoic acid C22:2(n-6) 0.019 no data no data 0.019 0.02 

DPA (Z,Z,Z,Z,Z)-7,10,13,16,19-Docosapentaenoic acid C22:5(n-3) 0.86 0.89 1.16 0.89 0.16 1.05 DHA (Z,Z,Z,Z,Z,Z)-4,7,10,13,16,19-Docosahexaenoic Acid C22:6(n-3) 3.87 3.50 5.47 3.87 1.05 4.42 

2003 Values 
Compounon detect 1s 2s 3s 4s 5s Median 1 SD n Consen

2,4’-DDT 144 no data <531 30.4 180 144 78 3 144 4,4’-DDT 1189 24131 894 234 1423 1189 10383 5 130

2,4’-DDE 490 no data <536 100 410 410 206 3 450 4,4’-DDE 177313 non detect 201667 47767 209500 189490 75452 4 2016

2,4’-DDD 77.2 no data <535 19.4 <100 48.3 41 2 77 4,4’-DDD 3501 17822 2493 585 2950 2950 6992 5 322

HCB <25 non detect <533 21.0 <50 21.0 1

alpha-HCH <25 non detect <561 23.7 46.7 35.2 16 2 47 

beta-HCH <25 non detect 1623 1400 1940 1623 271 3 194

gamma-HCH <25 non detect <380 30.9 53.3 42.1 16 2 53 

Heptachlor Epoxide no data 510 <380 no data no data 510 1 510 

Cis-Chlordane 656 519 <380 197 no data 519 235 3 656 

Trans-Chlordane 123 45.5 5423 11.7 no data 84.0 2682 4 277

Oxychlordane 454 511 <1280 no data 447 454 35 3 454 Cis-Nono datachlor 1725 1804 1453 321 no data 1589 686 4 172Trans-Nono datachlor 6746 6195 5423 1056 5103 5423 2246 5 580

Dieldrin no data non detect 998 271 no data 635 514 2 998 

Mirex 245 non detect <540 22.9 no data 134 157 2 245 Table 11: Median organochlorine pesticide and lipid concentrations in MMCM-1 Serum (female pilot whale; pg/g wet mass) reported by eabold were not used to derive the consensus value (see text for explanation).
Consensus

Congener 1s 2s 3s 4s 5s Median 1 SD n Value 18 30.5 non detect <539 9.9 <50 20 15 2 30.5 28 <25 405 <540 21.0 <50 213 271 231 w/28 non detect <407 8.6 <50 9 144 104 non detect <539 23.7 <50 64 56 2 104 

49 317 210 <537 no data 397 317 93 3 264 52 599 690 561 110 660 599 237 5 629 66/95* see below see below see below see below see below87 657 non detect 640 133 720.0 649 272 4 657 99 2497 1885 2320 578 2647 2320 837 5 2408 101 (+90) 2045 1527 2087 no data 2500 2066 399 4 2066 

105 1178 non detect 1357 235 1193 1185 510 4 1193 

118 4059 non detect 3633 782 3873 3753 1546 4 3873 128 1203 non detect 1207 199 1453 1205 557 4 1207 132 w/153 no data no data 75.0 533 304 324 2 533 138 (+163+164) 7261 non detect 9747 1750 7743 7502 3424 4 7743 149 1434 271 1460 204 1643 1434 703 5 1447 151 331 non detect <420 44.0 517 331 238 3 424 153 13136 1395 1423 1920 13532 1920 6443 5 13136 

156 68.4 non detect <136 10.9 <40 40 41 2 68.4 

170 (+190) 1575 1726 1603 240 1822 1603 652 5 1603 

180 5754 6025 6003 821 6285 6003 2331 5 6003 

183 1328 113 1317 181 1500 1317 681 5 1322 187 2158 480 1937 269 2445 1937 1008 5 2047 

194 1060 1075 907 129 1033 1033 403 5 1046 195 222 316 <543 29.8 247 235 123 4 247 201 203 non detect no data 155 1450 203 734 3206 453 387 <541 47.2 433 410 191 4 433 209 216 no data <541 25.4 no data 121 135 2 216 66 343 319 <537 74.3 no data 319 149 3 331 95 451 431 410 92.3 523 431 167 5 441 Table 12: Median PCB congener concentrations in MMCM-1 Serum (female pilot whale; pg/g wet mass) reported by each laboratory. The not used to derive the consensus value (see text for explanation).
Consensus

Congener 1s 2s 3s 4s 5s Median 1 SD n Value 1 SD PBDE 47 9256 10056 7217 1960 9960 9256 3401 5 9608 1319 PBDE 99 1868 2837 2097 397 2093 2093 895 5 2095 423 PBDE 100 3499 4153 3593 636 3617 3593 1401 5 3605 296 PBDE 153 739 1272 <1010 110 642 690 476 4 739 339 

PBDE 154 652 1298 <1010 100 w/PBB153 652 599 3 1298 -- Table 13: Median PBDE congener concentrations in MMCM-1 Serum (female pilot whale; pg/g wet mass) reported by each laboratory. Thwere not used to derive the consensus value (see text for explanation). 
Reference

Compound 1s 2s 3s 4s 5s Median 1 SD ± 95% CI n Value 2,4’-DDT 357 no data <409 no data 430 393 52 72 2 321 4,4’-DDT 238 non detect <411 no data 270 254 22 31 2 296 2,4’-DDE 540 NA 426.0 no data 513 513 60 67 3 464 4,4’-DDE 1056 non detect 1117 no data 1387 1117 176 199 3 1280 2,4’-DDD 421 NA 451.7 no data 430 430 16 18 3 344 4,4’-DDD 411 non detect <416 no data 363 387 34 47 2 417 HCB 462 263 <411 no data 393 393 101 114 3 450 alpha-HCH <25 non detect <432 no data 242 242 -- -- 1 266 beta-HCH <25 non detect <429 no data 235 235 -- -- 1 284 gamma-HCH <25 non detect <412 no data 313 313 -- -- 1 322 Heptachlor Epoxide no data non detect <413 no data NA -- -- -- 0 -- Cis-Chlordane 439 280 <412 no data NA 360 113 156 2 420 Trans-Chlordane 422 293 <415 no data NA 358 91 126 2 422 Oxychlordane 249 non detect <1100 no data 193 221 39 55 2 230 Cis-Nonachlor 422 355 <422 no data NA 389 47 66 2 431 Trans-Nonachlor 473 358 <415 no data 370 370 63 71 3 479 Dieldrin NA non detect 430.0 no data NA 430 -- -- 1 -- Mirex 374 468.0 <415 no data NA 421 67 93 2 389 Table 14: Median organochlorine pesticide and lipid concentrations in SRM 1958 determined by each laboratory (pg/g wet mass and percent (mass f
Table 15: Median PCB congener concentrations in SRM 1958 determined by each laboratory (pg/g wet mass). 

Reference

Congener 1s 2s 3s 4s 5s Median 1 SD ± 95% CI n Value 18 394 non detect 483.7 no data no data 439 63.6 88.1 2 387 28 518 587 501.3 no data no data 518 45.5 51.5 3 415 31 w/28 non detect <313 no data no data -- -- -- 0 -- 44 383 575 422.0 no data 397 409 88.9 87.2 4 417 49 416 428 408.0 no data 603 422 93.4 91.5 4 426 52 406 377 439.0 no data 500 422 52.9 51.9 4 407 66/95* see below see below see below no data see below -- -- -- 087 336 non detect 373.0 no data 427 373 45.7 51.7 3 406 99 359 380 <413 no data 383 380 13.3 15 3 391 101 (+90) 338 372 416.5 no data 393 383 33.3 33 4 415 105 376 non detect 362.7 no data 373 373 7.1 8.0 3 425 118 468 non detect 494.3 no data 410 468 43.1 49 3 418 128 345 391 383.0 no data 400 387 23.9 23.5 4 427 132 w/153 non detect no data no data <20 -- -- -- 0 -- 138 (+163+164) 481 545 544.0 no data 448 513 48.1 47 4 474 149 363 321 428.0 no data 457 395 61.7 60 4 379 151 356 non detect <420 no data 380 368 17.2 23.8 2 388 153 474 648 <623 no data 413 474 122 138 3 468 156 337 288 <105 no data 483 337 101 115 3 424 170 (+190) 359 267 <413 no data 348 348 50.5 57 3 429 180 399 322 413 no data 398 399 41.4 41 4 470 183 310 292 <413 no data 315 310 12.0 13.6 3 412 187 365 335 <414 no data 357 357 15.6 18 3 417 194 337 320 <418 no data 333 333 8.6 10 3 393 195 304 340 <419 no data no data 322 25.4 35.1 2 392 201 <25 non detect no data no data 356.7 357 -- -- 1 397 206 325 277 <420 no data <50 301 33.7 46.7 2 373 209 295 no data <413 no data no data 295 -- -- 1 344 66 355 396.0 <414 no data no data 375 29.1 40.4 2 424 95 <25 non detect <209 no data <20 -- -- -- 0 -- 
Table 16: Median PBDE congener concentrations in SRM 1958 determined by each laboratory (pg/g wet mass). 

Reference

Congener 1s 2s 3s 4s 5s Median 1 SD ± 95% CI n Value PBDE 47 580 857 <818 no data 580 580 160 181 3 661 PBDE 99 451 657 <817 no data 413 451 131 148 3 499 PBDE 100 470 540 <817 no data 397 470 71.8 81.3 3 482 PBDE 153 432 613 <814 no data 358 432 131 149 3 460 PBDE 154 312 938 <821 no data no data 625 no data no data 2 450 
Appendix A

Tabular results of PCB congeners, pesticides, PBDE congeners, lipid, and 

fatty acids reported by all laboratories
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Uncert 

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT 1374 1367 1374 106 108 90 1372 0.3 101 9.9 1200 89 90.9 13 4,4’-DDT 2066 1983 1925 238 237 241 1991 3.6 238 0.9 2078 173 233 8.0 2,4’-DDE 421 422 386 13.5 12.9 13.6 410 5.0 13 2.7 410 46 14.2 1.4 4,4’-DDE 23589 23844 24028 515 517 507 23820 0.9 513 1.0 22633 1569 497 19 2,4’-DDD 443 438 452 19.2 21.0 19.8 444 1.5 20 4.7 383 45 19.5 1.2 4,4’-DDD 1874 1725 1616 120 110 131 1738 7.4 120 8.5 1708 138 120 4.9 HCB 286 283 288 30.9 30.9 29.9 285 0.9 31 1.9 262 39 30.6 1.5 CH 8.77 9.68 9.82 16.2 16.6 16.0 9.42 6.1 16 2.0 8.56 2.1 16.9 1.4 CH 38.1 40.6 36.6 <LOD <LOD <LOD 38.4 5.2 39.1 3.8 CH 6.03 5.94 5.85 3.18 3.06 3.19 5.94 1.5 3 2.4 4.87 16 3.18 0.01 Heptachlor Epoxide 13.6 11.9 13.1 10.7 10.7 10.8 12.9 6.6 11 0.5 41.5 31 10.7 0.09 Cis-Chlordane 91.3 86.0 94.3 48.3 49.8 47.5 90.5 4.6 49 2.4 92.0 22 48.1 1.6 Trans-Chlordane 21.0 24.4 22.1 12.5 11.5 12.4 22.5 7.8 12 4.5 10.1 6.3 11.8 0.54 Oxychlordane 71.6 82.0 80.0 22.6 22.2 21.8 77.9 7.1 22 1.8 69.0 9.2 21.2 1.1 Cis-Nonachlor 91.3 86.0 94.3 48.3 49.8 47.5 90.5 4.6 49 2.4 155 33 45.8 3.3 Trans-Nonachlor 400 395 376 208 198 192 390 3.3 199 3.9 439 86 198 16 Dieldrin 411 405 352 49.1 49.3 53.7 389 8.3 51 5.1 411 153 50.1 4.1 Mirex 54.7 56.0 55.3 34.1 36.3 33.2 55.3 1.1 35 4.6 50.0 9.3 31.0 3.3 

PBDE 47 149 152 151 39.6 39.4 39.5 150 0.9 40 0.3 147 20 39.6 0.18 PBDE 99 19.8 20.8 21.0 18.6 17.1 18.1 20.6 3.1 18 4.2 22.5 5.5 18.9 2.3 PBDE 100 27.0 30.4 28.5 9.90 9.76 9.57 28.6 6.1 10 1.7 28.6 2.2 10.3 1.1 PBDE 153 7.31 6.79 7.37 8.69 8.67 8.67 7.16 4.5 9 0.1 7.16 0.8 8.34 0.55 PBDE 154 21.7 21.4 21.3 13.2 12.8 12.9 21.5 1.0 13 1.5 21.6 3.0 13.3 1.7 Lipid (mass fraction (%)) 65.7 66.4 65.5 70.4 70.8 70.9 65.9 0.7 71 0.4 68.1 1.8 71.9 1.3 

Category 

 

2 to 3 

 

Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Uncert 

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 13.2 14.1 13.2 3.73 3.75 4.17 13.5 3.8 3.88 6.3 13.6 6.8 4.35 0.56 28 25.3 25.4 25.0 12.8 11.7 12.3 25.3 0.8 12.3 4.4 24.5 3.3 13.1 1.1 31 <1 <1 <1 3.42 3.29 3.46 3.39 2.5 2.7 1.6 3.56 0.3644 36.0 36.2 35.8 11.5 11.8 11.6 36.0 0.6 11.7 1.2 35.9 5.4 12.1 0.51 49 101 104 103 18.2 18.3 18.2 103 1.4 18.2 0.4 99.7 7.4 18.3 0.04 52 341 348 341 41.8 41.1 41.2 343 1.2 41.4 0.9 309 18 40.7 1.3 66/95* see below see below see below see below see below see below 13087 259 265 264 23.3 22.8 22.2 263 1.3 22.8 2.5 234 68 20.6 2.6 99 883 913 895 62.6 65.0 63.0 897 1.7 63.5 2.0 699 134 58.5 5.2 101 (+90) 1478 1480 1487 86.9 84.1 89.0 1482 0.3 86.7 2.9 1192 284 78.2 12 105 371 382 382 29.5 28.4 27.9 378 1.7 28.6 2.9 376 94 28.6 1.2 118 1121 1145 1139 78.2 74.8 72.2 1135 1.1 75.1 4.0 1264 269 76.5 2.9 128 467 478 477 22.0 22.3 21.9 474 1.2 22.1 0.9 474 101 23.0 1.1 132 w/153 w/153 w/153 w/153 w/153 w/153 456 220 21.1 4.8138 (+163+164) 4449 4517 4542 147 147 143 4503 1.1 146 1.7 4414 833 146 13 149 3145 3106 3150 93.1 94.8 88.5 3133 0.8 92.1 3.5 2610 475 89.0 6.9 151 1001 1014 992 29.8 30.3 28.3 1003 1.1 29.4 3.6 802 145 28.6 1.3 153 8520 8670 8686 274 279 252 8625 1.1 268 5.5 6967 1594 228 9.8 156 204 210 211 11.4 11.3 10.5 208 1.9 11.1 4.4 230 42 11.4 0.95 170 (+190) 1534 1559 1565 43.3 44.3 42.6 1553 1.1 43.4 2.0 1302 250 42.6 2.2 180 3889 3943 3934 143 145 132 3922 0.7 140 5.1 3754 806 138 9.7 183 937 951 956 37.0 40.5 38.6 948 1.0 38.7 4.5 856 175 38.0 1.8 187 2919 2974 2973 133 132 131 2955 1.1 132 0.5 2696 502 121 11 194 356 355 358 57.4 61.0 56.2 356 0.5 58.2 4.3 321 40 53.5 5.2 195 111 110 111 14.0 13.5 13.1 111 0.5 13.5 3.1 110 21 14.3 2.2 201 86.2 87.9 88.3 16.5 17.6 16.1 87.5 1.3 16.8 4.8 93.8 38 16.8 1.3 206 34.5 35.4 35.2 48.9 48.9 48.8 35.0 1.4 48.9 0.1 34.9 5.6 44.9 4.2 209 13.3 13.9 14.3 18.3 19.0 18.1 13.8 3.7 18.4 2.5 13.6 1.7 17.2 1.9 66 151 152 151 22.6 21.4 21.8 151 0.2 21.9 2.9 157 50 22.4 0.51 95 677 685 683 32.8 33.7 32.7 682 0.6 33.1 1.7 532 94 33.9 0.51 

Category 

 

2 to 3 

 

Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT 1377 1333 1354 92 93 94 1355 1.6 93 1.2 1200 89 90.9 14,4’-DDT 2099 1985 2045 235 241 244 2043 2.8 240 1.9 2078 173 233 82,4’-DDE 422 451 444 13.9 13.5 13.8 439 3.4 14 1.5 410 46 14.2 14,4’-DDE 23567 23044 23457 507 500 515 23356 1.2 507 1.5 22633 1569 497 12,4’-DDD 425 444 431 19.6 20.5 19.9 433 2.2 20 2.3 383 45 19.5 14,4’-DDD 1807 1818 1788 125 122 119 1804 0.8 122 2.5 1708 138 120 4HCB 265 266 279 29.8 30.4 31.1 270 2.9 30 2.1 262 39 30.6 1CH 8.35 8.88 8.45 16.4 15.9 16.2 8.56 3.3 16 1.6 8.56 2.1 16.9 1CH 38.7 39.1 38.7 <4 <4 <4 38.8 0.6 39.1 3.8 CH 5.88 5.55 5.67 3.09 3.01 2.87 5.70 2.9 3 3.7 4.87 16 3.18 0.0Heptachlor Epoxide 13.3 15.4 13.7 10.0 10.5 10.1 14.1 7.9 10 2.6 41.5 31 10.7 0.0Cis-Chlordane 91.8 90.5 89.7 49.7 48.7 48.4 90.7 1.2 49 1.4 92.0 22 48.1 1Trans-Chlordane 19.9 20.5 21.4 12.1 11.5 11.9 20.6 3.7 12 2.6 10.1 6.3 11.8 0.5Oxychlordane 79.8 81.7 77.5 21.5 22.2 22.1 79.7 2.6 22 1.7 69.0 9.2 21.2 1Cis-Nonachlor 144 135 133 45.5 47.7 47.1 137 4.3 47 2.4 155 33 45.8 3Trans-Nonachlor 401 388 385 201 210 199 391 2.2 203 2.9 439 86 198 1Dieldrin 405 411 418 49.9 50.4 51.1 411 1.6 50 1.2 411 153 50.1 4Mirex 55.5 56.7 55.7 33.3 34.5 33.1 56.0 1.1 34 2.3 50.0 9.3 31.0 3

PBDE 47 149 152 151 39.6 39.4 39.5 150 0.9 40 0.3 147 20 39.6 0.PBDE 99 19.8 20.8 21.0 18.6 17.1 18.1 20.6 3.1 18 4.2 22.5 5.5 18.9 2PBDE 100 27.0 30.4 28.5 9.90 9.76 9.57 28.6 6.1 10 1.7 28.6 2.2 10.3 1PBDE 153 7.31 6.79 7.37 8.69 8.67 8.67 7.16 4.5 9 0.1 7.16 0.8 8.34 0.5PBDE 154 21.7 21.4 21.3 13.2 12.8 12.9 21.5 1.0 13 1.5 21.6 3.0 13.3 1Lipid (mass fraction (%)) 68.1 68.5 69.1 71.5 70.9 71.1 68.6 0.7 71 0.4 68.1 1.8 71.9 1

Cate



2 t



Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 13.3 13.5 14.1 4.01 3.99 3.94 13.6 3.1 3.98 0.9 13.6 6.8 4.35 0.528 25.5 26.1 24.8 12.8 12.5 12.2 25.5 2.6 13 2.4 24.5 3.3 13.1 131 3.44 3.98 3.85 3.22 3.55 3.45 3.8 7.5 3.41 5.0 2.7 1.6 3.56 0.344 36.5 35.8 35.5 12.1 11.8 11.8 35.9 1.4 11.9 1.5 35.9 5.4 12.1 0.549 105 101 103 18.1 18.3 18.3 103 1.9 18.2 0.6 99.7 7.4 18.3 0.052 338 341 345 41.6 42.1 43.1 341 1.0 42.3 1.8 309 18 40.7 166/95* see below see below see below see below see below see below 13087 234 233 229 20.2 20.6 21.1 232 1.1 20.6 2.2 234 68 20.6 299 868 878 888 61.5 62.4 60.7 878 1.1 61.5 1.4 699 134 58.5 5101 (+90) 1444 1398 1405 84.1 83.9 85.7 1416 1.8 84.6 1.2 1192 284 78.2 1105 381 378 369 29.1 28.5 28.1 376 1.7 28.6 1.8 376 94 28.6 1118 1112 1254 1227 77.7 75.5 75.7 1198 6.3 76.3 1.6 1264 269 76.5 2128 488 475 461 22.3 22.7 22.5 475 2.8 22.5 0.9 474 101 23.0 1132 801 798 775 20.5 21.5 22.2 791 1.8 21.4 4.0 456 220 21.1 4138 (+163+164) 4544 4449 4521 149 151 149 4505 1.1 150 0.8 4414 833 146 1149 3154 3111 3107 91.5 94.4 93.7 3124 0.8 93.2 1.6 2610 475 89.0 6151 1005 1014 1021 30.5 28.8 27.9 1013 0.8 29.1 4.5 802 145 28.6 1153 7545 7705 7611 221 228 219 7620 1.1 223 2.1 6967 1594 228 9156 212 222 205 11.9 10.5 11.1 213 4.0 11.2 6.3 230 42 11.4 0.9170 (+190) 155 1534 1521 44.5 42.1 42.5 1070 74.1 43.0 3.0 1302 250 42.6 2180 3788 3801 3754 144 138 133 3781 0.6 138 4.0 3754 806 138 9183 901 933 945 40.5 38.8 38.1 926 2.5 39.1 3.2 856 175 38.0 1187 2887 2904 2845 131 128 122 2879 1.1 127 3.6 2696 502 121 1194 345 361 354 50.4 55.5 53.2 353 2.3 53 4.8 321 40 53.5 5195 113 115 102 13.5 13.9 14.4 110 6.4 13.9 3.2 110 21 14.3 2201 99.8 89.4 92.1 17.2 16.5 16.4 93.8 5.8 16.7 2.6 93.8 38 16.8 1206 33.9 35.1 35.5 46.5 48.1 46.7 34.8 2.4 47.1 1.9 34.9 5.6 44.9 4209 14.5 13.9 14.7 18.1 17.9 18.2 14.4 2.9 18.1 0.8 13.6 1.7 17.2 166 149 444 151 22.5 21.8 22.1 248 68.4 22.1 1.6 157 50 22.4 0.595 655 648 666 33.9 34.1 33.4 656 1.4 33.8 1.1 532 94 33.9 0.5

Cate



2 t



Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT 992 1010 1020 84 85 86 1007 1.4 85.1 1.1 1200 89 90.9 14,4’-DDT 1990 2020 2040 244 236 239 2017 1.2 240 1.7 2078 173 233 82,4’-DDE 375 379 383 13.9 14.0 14.1 379 1.1 14.0 0.7 410 46 14.2 14,4’-DDE 19200 19600 19700 509 505 509 19500 1.4 508 0.5 22633 1569 497 12,4’-DDD 338 340 349 19.7 19.9 20.4 342 1.7 20.0 1.8 383 45 19.5 14,4’-DDD 1400 1420 1430 148 150 151 1417 1.1 150 1.0 1708 138 120 4HCB 245 251 251 26.7 26.6 26.7 249 1.4 26.7 0.2 262 39 30.6 1-HCH 5.84 5.57 5.76 14.7 15.1 15.2 5.72 2.4 15.0 1.8 8.56 2.1 16.9 1-HCH 38.6 39.8 39.5 interference interference interference 39.3 1.6 39.1 3.8 -HCH 3.75 3.69 3.76 2.54 2.47 2.42 3.73 1.0 2.48 2.4 4.87 16 3.18 0.0Heptachlor Epoxide 70.1 68.4 69.8 10.1 10.1 10.3 69.4 1.3 10.2 1.1 41.5 31 10.7 0.0Cis-Chlordane 108.0 109.0 110.0 55.4 57.0 57.0 109.0 0.9 56.5 1.6 92.0 22 48.1 1Trans-Chlordane 8.53 8.70 8.96 11.8 12.0 12.2 8.73 2.5 12.0 1.7 10.1 6.3 11.8 0.5Oxychlordane 60.2 62.5 63.0 19.3 20.2 20.6 61.9 2.4 20.0 3.3 69.0 9.2 21.2 1Cis-Nonachlor 192 194 195 56.9 58.8 59.3 194 0.8 58.3 2.2 155 33 45.8 3Trans-Nonachlor 437 440 446 182 180 182 441 1.0 181 0.6 439 86 198 1Dieldrin 395 406 384 51.5 52.0 52.6 395 2.8 52.0 1.1 411 153 50.1 4Mirex 62.1 62.2 62.3 37.4 41.4 41.6 62.2 0.2 40.1 5.9 50.0 9.3 31.0 3

PBDE 47 208 208 208 41.3 42.2 42.8 208 0.0 42.1 1.8 147 20 39.6 0.PBDE 99 26.3 27.0 27.1 21.6 20.7 21.4 26.8 1.6 21.2 2.2 22.5 5.5 18.9 2PBDE 100 32.5 32.8 33.1 12.4 12.0 12.5 32.8 0.9 12.3 2.2 28.6 2.2 10.3 1PBDE 153 6..06 6.02 6.05 7.23 7.44 7.40 6.04 0.4 7.36 1.5 7.16 0.8 8.34 0.5PBDE 154 22.7 23.5 23.4 14.5 14.5 14.5 23.2 1.9 14.5 0.0 21.6 3.0 13.3 1Lipid (mass fraction (%)) 68.0 68.3 66.7 72.9 72.4 73.3 67.7 1.3 72.9 0.6 68.1 1.8 71.9 1

Cate

 

2 t

 

Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 9.3 9.4 9.5 2.70 2.65 2.58 9.4 0.8 2.64 2.3 13.6 6.8 4.35 0.528 24.5 24.6 24.3 11.4 11.7 11.4 24.5 0.6 11.5 1.5 24.5 3.3 13.1 131 1.80 1.65 1.72 3.55 3.18 3.62 1.7 4.4 3.45 6.9 2.7 1.6 3.56 0.344 31.7 32.3 32.3 12.1 12.0 12.2 32.1 1.1 12.1 0.8 35.9 5.4 12.1 0.549 90 91 92 17.4 17.5 17.5 91 1.3 17.5 0.3 99.7 7.4 18.3 0.052 281 287 286 40.8 40.6 40.9 285 1.1 40.8 0.4 309 18 40.7 166/95* see below see below see below see below see below see below 13087 217 219 219 23.6 23.6 23.6 218 0.5 23.6 0.0 234 68 20.6 299 665 675 672 56.1 56.4 56.4 671 0.8 56.3 0.3 699 134 58.5 5101 (+90) 1040 1050 1040 87.9 87.2 87.5 1043 0.6 87.5 0.4 1192 284 78.2 1105 373 377 380 28.6 28.7 28.8 377 0.9 28.7 0.3 376 94 28.6 1118 1230 1250 1240 86.5 85.8 86.2 1240 0.8 86.2 0.4 1264 269 76.5 2128 471 475 474 25.0 25.2 25.3 473 0.4 25.2 0.6 474 101 23.0 1132 no data no data no data no data no data no data 456 220 21.1 4138 (+163+164) 4950 5020 5000 195 190 192 4990 0.7 192 1.3 4414 833 146 1149 2860 2890 2880 89.7 89.6 90.4 2877 0.5 89.9 0.5 2610 475 89.0 6151 795 804 806 26.9 27.2 27.4 802 0.7 27.2 0.9 802 145 28.6 1153 6900 7010 6990 262 258 260 6967 0.8 260 0.8 6967 1594 228 9156 220 221 219 13.0 13.2 13.3 220 0.5 13.2 1.2 230 42 11.4 0.9170 (+190) 1280 1310 1310 45.1 45.6 45.9 1300 1.3 45.5 0.9 1302 250 42.6 2180 3340 3370 3370 166 165 167 3360 0.5 166 0.6 3754 806 138 9183 929 933 934 41.8 42.2 42.4 932 0.3 42.1 0.7 856 175 38.0 1187 2510 2530 2540 145 144 145 2527 0.6 145 0.4 2696 502 121 1194 312 314 311 63.9 68.3 68.4 312 0.5 66.9 3.8 321 40 53.5 5195 95 95 96 11.0 11.3 10.9 96 0.5 11.1 1.9 110 21 14.3 2201 no data no data no data no data no data no data 93.8 38 16.8 1206 37.6 39.7 38.1 60.0 63.4 63.3 38.5 2.9 62.2 3.1 34.9 5.6 44.9 4209 13.2 13.4 13.4 19.8 20.1 20.4 13.3 0.9 20.1 1.5 13.6 1.7 17.2 166 114 119 117 22.6 22.6 22.7 117 2.2 22.6 0.3 157 50 22.4 0.595 515 522 518 36.9 37.0 37.5 518 0.7 37.1 0.9 532 94 33.9 0.5

Cate

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2 t

 

Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT 1280 1310 1290 66 69 68 1293 1.2 67.7 2.3 1200 89 90.9 14,4’-DDT 1340 1340 1300 113 122 117 1327 1.7 117 3.8 2078 173 233 82,4’-DDE 299 309 307 8.6 11.5 12.2 305 1.7 10.8 18 410 46 14.2 14,4’-DDE 21200 22000 21500 378 433 428 21567 1.9 413 7.4 22633 1569 497 12,4’-DDD 443 447 439 19.0 19.3 19.1 443 0.9 19.1 0.8 383 45 19.5 14,4’-DDD Interference Interference Interference Interference Interference Interference 1708 138 120 4HCB 190 205 195 22.6 26.4 25.8 197 3.9 24.9 8.2 262 39 30.6 1-HCH Interference Interference Interference Interference Interference Interference 8.56 2.1 16.9 1-HCH 37.2 42.4 51.8 8.10 7.95 9.79 43.8 16.9 9 12 39.1 3.8 -HCH <LOD <LOD <LOD <LOD <LOD <LOD 4.87 16 3.18 0.0Heptachlor Epoxide 12.7 8.4 15.6 3.4 5.5 4.2 12.2 29.9 4.4 24.0 41.5 31 10.7 0.0Cis-Chlordane 49.0 50.8 48.0 30.7 33.6 32.8 49.3 2.9 32.4 4.6 92.0 22 48.1 1Trans-Chlordane 38.00 28.70 31.60 13.2 14.6 13.7 32.77 14.5 13.8 5.1 10.1 6.3 11.8 0.5Oxychlordane 48.7 56.7 57.7 15.4 15.9 15.9 54.4 9.1 15.7 1.8 69.0 9.2 21.2 1Cis-Nonachlor Interference Interference Interference Interference Interference Interference 155 33 45.8 3Trans-Nonachlor 376 383 374 117 130 130 378 1.3 126 6.0 439 86 198 1Dieldrin Interference Interference Interference Interference Interference Interference 411 153 50.1 4Mirex Interference Interference Interference Interference Interference Interference 50.0 9.3 31.0 3

PBDE 47 160 143 162 42.1 43.2 47.1 155 6.7 44.1 6.0 147 20 39.6 0.PBDE 99 no data no data no data 19.9 16.0 22.7 19.5 17 22.5 5.5 18.9 2PBDE 100 no data no data no data 9.50 10.5 11.3 10.4 8.4 28.6 2.2 10.3 1PBDE 153 no data no data no data <LOD <LOD <LOD 7.16 0.8 8.34 0.5PBDE 154 no data no data no data <LOD <LOD <LOD 21.6 3.0 13.3 1Lipid (mass fraction (%)) 69.0 66.2 63.3 71.4 65.5 75.7 66.2 4.3 70.9 7.2 68.1 1.8 71.9 1

Cate

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2 t



Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 36.4 28.1 23.1 4.26 2.51 6.33 29.2 23.0 4.37 43.8 13.6 6.8 4.35 0.528 16.0 <LOD <LOD 5.73 7.58 6.84 16.0 6.72 13.8 24.5 3.3 13.1 131 10.0 <LOD <LOD 2.65 2.08 2.30 10.0 2.34 12.1 2.7 1.6 3.56 0.344 39.9 56.9 71.7 16.9 12.3 12.0 56.2 28.3 13.7 20.0 35.9 5.4 12.1 0.549 103 118 102 13.9 16.2 16.5 108 8.3 15.5 9.2 99.7 7.4 18.3 0.052 321 338 322 29.0 33.1 32.9 327 2.9 31.7 7.3 309 18 40.7 166/95* 654 671 651 47.6 49.2 48.8 659 1.6 48.5 1.7 130 87 Interference Interference Interference Interference Interference Interference 234 68 20.6 299 685 718 682 46.4 48.3 48.3 695 2.9 47.7 2.3 699 134 58.5 5101 (+90) Interference Interference Interference Interference Interference Interference 1192 284 78.2 1105 299 269 279 14.2 13.2 11.1 282 5.4 12.8 12.3 376 94 28.6 1118 1410 1390 1340 67.6 71.2 71.3 1380 2.6 70.0 3.0 1264 269 76.5 2128 306 305 293 17.7 19.0 17.9 301 2.4 18.2 3.8 474 101 23.0 1132 w/153 w/153 w/153 w/153 w/153 w/153 456 220 21.1 4138 (+163+164) 3260 3190 3080 92.0 94.1 92.1 3177 2.9 92.7 1.3 4414 833 146 1149 2420 2440 2380 70.2 71.8 72.3 2413 1.3 71.4 1.5 2610 475 89.0 6151 799 809 787 22.7 23.5 23.3 798 1.4 23.2 1.8 802 145 28.6 1153 4390 4290 4100 122 119 118 4260 3.5 120 1.7 6967 1594 228 9156 121 117 116 4.8 5.5 5.3 118 2.2 5.2 6.7 230 42 11.4 0.9170 (+190) 850 770 809 19.7 21.8 21.0 810 4.9 20.8 5.1 1302 250 42.6 2180 2420 2340 2290 90 93 91 2350 2.8 91.6 1.6 3754 806 138 9183 536 520 506 19.8 20.4 19.8 521 2.9 20.0 1.7 856 175 38.0 1187 1840 1770 1720 75.5 75.7 73.5 1777 3.4 75 1.6 2696 502 121 1194 258 238 231 33.6 34.3 33.4 242 5.8 33.8 1.4 321 40 53.5 5195 232 213 249 20.0 20.2 17.8 231 7.8 19.3 6.9 110 21 14.3 2201 293.0 278.0 275.0 36.7 36.8 35.9 282.0 3.4 36.5 1.4 93.8 38 16.8 1206 29.7 27.7 27.6 28.4 29.7 29.0 28.3 4.2 29.0 2.2 34.9 5.6 44.9 4209 16.2 11.0 11.1 12.8 14.2 13.7 12.8 23.3 13.6 5.2 13.6 1.7 17.2 166 see above see above see above see above see above see above 157 50 22.4 0.595 see above see above see above see above see above see above 532 94 33.9 0.5

Cate

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2 t



Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

4,4’-DDT 1975 1939 1831 266 207 197 1915 3.9 223 16.7 2078 173 233 82,4’-DDE 551 584 547 16.7 15.5 15.5 560 3.6 16 4.5 410 46 14.2 14,4’-DDE 24006 26986 24784 565 595 590 25259 6.1 583 2.8 22633 1569 497 12,4’-DDD 231 255 263 17.8 18.6 23.4 250 6.8 20 15.3 383 45 19.5 14,4’-DDD 1166 1430 1218 161 163 163 1271 11.0 162 0.8 1708 138 120 4HCB 382 391 368 36.6 35.8 35.4 381 3.1 36 1.7 262 39 30.6 1-HCH <2.06 <2.06 <2.06 15.6 12.8 10.7 13 18.8 8.56 2.1 16.9 1-HCH <1.20 <1.20 <1.20 8.55 8.69 9.00 9 2.6 39.1 3.8-HCH <1.91 <1.91 <1.91 <1.91 <1.91 <1.91 4.87 16 3.18 0.0Heptachlor Epoxide 116.7 121.6 116.3 14.0 15.1 14.5 118.2 2.5 15 3.9 41.5 31 10.7 0.0Cis-Chlordane 90.7 93.1 81.1 34.5 23.6 21.5 88.3 7.2 27 26.3 92.0 22 48.1 1Trans-Chlordane 15.3 12.9 9.2 1.3 5.2 2.8 12.5 24.7 3 62.7 10.1 6.3 11.8 0.5Oxychlordane 75.6 76.2 76.5 17.6 17.1 19.0 76.1 0.6 18 5.5 69.0 9.2 21.2 1Cis-Nonachlor 101 103 102 40.2 41.4 41.6 102 1.0 41 1.9 155 33 45.8 3Trans-Nonachlor 726 753 709 214 213 213 729 3.1 213 0.2 439 86 198 1Dieldrin 1004 1068 953 40.6 45.2 47.1 1008 5.7 44 7.5 411 153 50.1 4Mirex 34.2 35.0 35.9 25.0 22.1 21.0 35.0 2.4 23 9.0 50.0 9.3 31.0 3

PBDE 47 178 190 184 52.5 53.7 53.5 184 3.2 53 1.3 147 20 39.6 0.PBDE 99 22.2 23.4 21.6 18.1 17.6 17.7 22.4 4.0 18 1.3 22.5 5.5 18.9 2PBDE 100 27.0 28.9 26.9 10.46 10.46 10.35 27.6 4.2 10 0.6 28.6 2.2 10.3 1PBDE 153 7.04 7.11 6.76 9.47 8.63 8.72 6.97 2.7 9 5.2 7.16 0.8 8.34 0.5PBDE 154 29.6 31.5 30.1 22.8 22.1 22.4 30.4 3.1 22 1.6 21.6 3.0 13.3 1Lipid (mass fraction (%)) 67.0 67.0 61.0 73.0 72.0 73.0 65.0 5.3 73 0.8 68.1 1.8 71.9 1

Cate

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2 t

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Data as Submitted by Laboratory (ng/g wet mass)

SRM 1945

Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 10.3 12.0 10.3 6.42 6.29 6.62 10.8 8.8 6.44 2.6 13.6 6.8 4.35 0.528 Interference Interference Interference Interference Interference Interference 24.5 3.3 13.1 131 Interference Interference Interference Interference Interference Interference 2.74 1.6 3.56 0.344 45.7 48.7 46.8 20.5 20.3 21.1 47.1 3.2 20.7 2.0 35.9 5.4 12.1 0.549 106 114 101 23.4 22.2 23.3 107 6.3 23.0 3.0 99.7 7.4 18.3 0.052 341 359 323 43.0 41.3 42.8 341 5.4 42.4 2.2 309 18 40.7 166/95* Interference Interference Interference Interference Interference Interference 130 0.00 0.087 Interference Interference Interference Interference Interference Interference 234 68 20.6 299 694 755 651 55.6 59.3 55.4 700 7.5 56.8 3.9 699 134 58.5 5101 (+90) Interference Interference Interference Interference Interference Interference 1192 284 78.2 1105 341 378 317 25.8 28.1 26.5 346 8.9 26.8 4.3 376 94 28.6 1118 Interference Interference Interference Interference Interference Interference 1264 269 76.5 2128 Interference Interference Interference Interference Interference Interference 474 101 23.0 1132 Interference Interference Interference Interference Interference Interference 456 220 21.1 4138 (+163+164) 8075 8249 8094 267 279 262 8140 1.2 269 3.2 4414 833 146 1149 2497 2675 2385 85.2 83.7 81.2 2519 5.8 83.4 2.5 2610 475 89.0 6151 665 712 642 31.7 31.1 30.7 673 5.3 31.2 1.6 802 145 28.6 1153 Interference Interference Interference Interference Interference Interference 6967 1594 228 9156 205 223 205 20.1 19.8 20.4 211 4.9 20.1 1.5 230 42 11.4 0.9170 (+190) 1066 1169 1081 38.4 34.3 34.0 1105 5.0 35.6 6.9 1302 250 42.6 2180 Interference Interference Interference Interference Interference Interference 3754 806 138 9183 786 746 800 27.2 24.2 22.6 778 3.6 24.7 9.5 856 175 38.0 1187 2643 2799 2711 127 120 121 2718 2.9 123 3.2 2696 502 121 1194 313 316 298 49.8 51.3 55.2 309 3.1 52 5.4 321 40 53.5 5195 87 85 87 13.6 12.0 8.4 86 1.6 11.3 23.7 110 21 14.3 2201 431.6 413.8 418.3 78.9 71.3 70.1 421.2 2.2 73.4 6.5 93.8 38 16.8 1206 32.5 33.8 32.1 50.8 49.6 50.8 32.8 2.8 50.4 1.4 34.9 5.6 44.9 4209 13.9 14.2 13.4 17.5 16.3 18.6 13.8 2.7 17.5 6.5 13.6 1.7 17.2 166 161 171 152 26.5 19.9 27.5 162 5.9 24.7 16.8 157 50 22.4 0.595 Interference Interference Interference Interference Interference Interference 532 94 33.9 0.5

Cate

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2 t

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT no data no data no data no data no data no data 1200 89 90.9 14,4’-DDT 2051 2437 1996 224 224 228 2161 11 225 1.1 2078 173 233 82,4’-DDE no data no data no data no data no data no data 410 46 14.2 14,4’-DDE 21172 21580 20667 509 488 446 21140 2.2 481 6.6 22633 1569 497 12,4’-DDD no data no data no data no data no data no data 383 45 19.5 14,4’-DDD 1536 1805 1998 109 128 109 1780 13 116 9.6 1708 138 120 4HCB 244 245 262 23.4 29.5 27.1 250 4.1 27 11.5 262 39 30.6 1-HCH 16.0 26.4 23.4 24.6 39.9 26.7 21.9 24 30 27.3 8.56 2.1 16.9 1-HCH no data no data no data no data no data no data 39.1 3.8-HCH 20.4 22.8 21.1 29.7 30.9 25.4 21.4 5.7 29 10.1 4.87 16 3.18 0.0Heptachlor Epoxide no data no data no data no data no data no data 41.5 31 10.7 0.0Cis-Chlordane no data no data no data no data no data no data 92.0 22 48.1 1Trans-Chlordane no data no data no data no data no data no data 10.1 6.3 11.8 0.5Oxychlordane no data no data no data no data no data no data 69.0 9.2 21.2 1Cis-Nonachlor no data no data no data no data no data no data 155 33 45.8 3Trans-Nonachlor no data no data no data no data no data no data 439 86 198 1Dieldrin 41.5 448 492 8.7 67.8 56.4 327 76 44 70.8 411 153 50.1 4Mirex no data no data no data no data no data no data 50.0 9.3 31.0 3

PBDE 47 160 150 130 43.0 39.0 35.0 147 10 39 10.3 147 20 39.6 0.PBDE 99 26.0 21.0 21.0 22.0 18.0 16.0 22.7 13 19 16.4 22.5 5.5 18.9 2PBDE 100 28.0 22.0 24.0 10.00 8.80 8.90 24.7 12 9 7.2 28.6 2.2 10.3 1PBDE 153 7.70 8.60 7.10 9.90 10.00 9.10 7.80 9.7 10 5.1 7.16 0.8 8.34 0.5PBDE 154 23.0 23.0 23.0 16.0 16.0 15.0 23.0 0.0 16 3.7 21.6 3.0 13.3 1Lipid (mass fraction (%)) 67.9 68.0 68.0 71.7 72.5 72.5 68.0 0.1 72 0.6 68.1 1.8 71.9 1

Cate



2 t



Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 16.5 16.3 23.5 3.00 2.40 2.90 18.8 22 2.77 12 13.6 6.8 4.35 0.528 11.2 17.1 16.7 <1 4.3 6.4 15.0 22 5.4 28 24.5 3.3 13.1 131 2.80 <1 5.49 4.10 <1 4.40 4.1 46 4.25 5.0 2.7 1.6 3.56 0.344 30.6 45.0 54.4 <1 3.2 15.2 43.3 28 9.2 92 35.9 5.4 12.1 0.549 109 102 122 28.1 4.3 23.1 111 9.2 18.5 68 99.7 7.4 18.3 0.052 258 284 274 43.1 38.9 39.3 272 4.9 40.4 5.7 309 18 40.7 166/95* 133.63 132 125.7 23.4 18.6 21.2 130 3.2 21 11 130 87 no data no data no data no data no data no data 234 68 20.6 299 no data no data no data no data no data no data 699 134 58.5 5101 (+90) 1192 1199 1098 78.5 83.0 77.5 1163 4.8 79.7 3.7 1192 284 78.2 1105 352 390 357 26.8 32.8 29.4 366 5.7 29.7 10 376 94 28.6 1118 1240 1248 1249 90.1 75.9 86.3 1246 0.4 84.1 8.7 1264 269 76.5 2128 517 591 580 27.2 28.6 33.8 563 7.0 29.9 12 474 101 23.0 1132 no data no data no data no data no data no data 456 220 21.1 4138 (+163+164) 4393 4529 4319 175 149 157 4414 2.4 160 8.4 4414 833 146 1149 2169 2289 2196 90.6 68.6 77.3 2218 2.8 78.8 14 2610 475 89.0 6151 739 762 707 17.0 23.2 21.9 736 3.8 20.7 16 802 145 28.6 1153 6357 6886 6885 223 188 215 6709 4.6 208 8.8 6967 1594 228 9156 240 249 218 13.7 7.8 11.3 236 6.8 10.9 27 230 42 11.4 0.9170 (+190) 1547 1565 1449 60.6 41.7 48.3 1520 4.1 50.2 19 1302 250 42.6 2180 3806 3790 3668 177 156 150 3754 2.0 161 8.6 3754 806 138 9183 889 821 845 44.0 38.9 41.3 852 4.0 41.4 6.2 856 175 38.0 1187 2559 2805 2657 113 115 127 2674 4.6 118 6.5 2696 502 121 1194 326 336 297 67.9 59.7 56.0 320 6.4 61.2 10 321 40 53.5 5195 no data no data no data no data no data no data 110 21 14.3 2201 no data no data no data no data no data no data 93.8 38 16.8 1206 no data no data no data no data no data no data 34.9 5.6 44.9 4209 no data no data no data no data no data no data 13.6 1.7 17.2 166 no data no data no data no data no data no data 157 50 22.4 0.595 no data no data no data no data no data no data 532 94 33.9 0.5

Cate

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2 t



Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT 1190 1200 1190 91.1 84.4 90.6 1193 0.5 89 4.2 1200 89 90.9 14,4’-DDT 2690 2790 2780 297 307 301 2753 2.0 302 1.7 2078 173 233 82,4’-DDE 445 465 467 14.4 15.9 15.3 459 2.7 15.2 5.0 410 46 14.2 14,4’-DDE 32500 26900 28200 683 696 699 29200 10.0 693 1.2 22633 1569 497 12,4’-DDD 355 408 380 20.0 19.8 22.8 381 7.0 20.9 8.0 383 45 19.5 14,4’-DDD 1650 1800 1900 130 112 132 1783 7.1 125 8.8 1708 138 120 4HCB 338 341 350 36.3 38.8 36.6 343 1.8 37.2 3.7 262 39 30.6 1-HCH 6.70 6.71 6.83 18.9 18.2 18.0 6.75 1.1 18.4 2.6 8.56 2.1 16.9 1-HCH 37.8 38.1 37.6 1.93 2.10 2.09 37.8 0.7 2.04 4.7 39.1 3.8 -HCH 3.94 4.01 4.15 3.10 3.08 2.98 4.03 2.7 3.05 2.1 4.87 16 3.18 0.0Heptachlor Epoxide no data no data no data no data no data no data 41.5 31 10.7 0.0Cis-Chlordane 145.0 152.0 150.0 80.8 75.6 80.0 149.0 2.4 78.8 3.6 92.0 22 48.1 1Trans-Chlordane 9.72 9.50 8.95 11.80 12.00 13.30 9.4 4.2 12.4 6.6 10.1 6.3 11.8 0.5Oxychlordane no data no data no data no data no data no data 69.0 9.2 21.2 1Cis-Nonachlor 172 169 180 56.5 53.1 53.3 173.7 3.3 54.3 3.5 155 33 45.8 3Trans-Nonachlor 195 523 508 220 218 229 409 45 222 2.6 439 86 198 1Dieldrin 421 416 440 59.4 59.4 61.5 426 3.0 60.1 2.0 411 153 50.1 4Mirex 45.0 44.0 45.2 33.1 32.7 32.6 44.7 1.4 32.8 0.8 50.0 9.3 31.0 3

PBDE 47 139 145 142 39.8 41.0 43.1 142 2.1 41.3 4.0 147 20 39.6 0.PBDE 99 23.7 24.6 26.0 21.8 22.5 22.8 24.8 4.7 22.4 2.3 22.5 5.5 18.9 2PBDE 100 28.6 28.9 29.2 11.20 11.30 11.60 28.9 1.0 11.4 1.8 28.6 2.2 10.3 1PBDE 153 6.99 7.05 7.45 9.39 9.80 9.67 7.16 3.5 9.6 2.2 7.16 0.8 8.34 0.5PBDE 154 22.2 21.4 21.7 13.8 13.7 14.0 21.8 1.9 13.8 1.1 21.6 3.0 13.3 1Lipid (mass fraction (%)) 74.5 77.2 75.0 80.7 81.8 84.1 75.6 1.9 82.2 2.1 68.1 1.8 71.9 1

Cate

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2 t

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 6.15 6.68 6.61 1.87 1.84 1.92 6.48 4.4 1.88 2.2 13.6 6.8 4.35 0.528 20.1 20.3 20.7 10.1 9.94 10.3 20.4 1.5 10.1 1.8 24.5 3.3 13.1 131 0.61 0.68 0.61 2.74 3.11 3.27 0.63 6.3 3.04 8.9 2.7 1.6 3.56 0.344 30.1 32.2 30.5 10.3 10.8 11.1 30.9 3.6 10.7 3.8 35.9 5.4 12.1 0.549 no data no data no data no data no data no data 99.7 7.4 18.3 0.052 273 279 262 33.4 33.3 34.6 271 3.2 33.8 2.1 309 18 166/95* see below see below see below see below see below see below 130 0.0087 237 238 248 21.3 22.5 22.7 241 2.5 22.2 3.4 234 68 20.6 299 845 848 889 63.1 64.3 66.0 861 2.9 64.5 2.3 699 134 58.5 5101 (+90) no data no data no data no data no data no data 1192 284 78.2 1105 303 307 332 21.6 21.8 22.7 314 5.0 22.0 2.7 376 94 28.6 1118 1310 1330 1430 81.4 82.1 84.9 1357 4.7 82.8 2.2 1264 269 76.5 2128 425 429 455 17.7 18.1 19.0 436 3.7 18.3 3.6 474 101 23.0 1132 423 429 440 15.4 15.9 16.5 431 2.0 15.9 3.5 456 220 21.1 4138 (+163+164) 6160 6220 6030 184 191 200 6137 1.6 192 4.2 4414 833 146 1149 2400 2500 2390 70.3 69.2 73.0 2430 2.5 70.8 2.8 2610 475 89.0 6151 782 826 796 23.2 22.4 23.9 801 2.8 23.2 3.2 802 145 28.6 1153 5090 5390 5700 189 194 203 5393 5.7 195 3.6 6967 1594 228 9156 232 232 227 9.79 10.2 10.7 230 1.3 10.2 4.5 230 42 11.4 0.9170 (+190) 1350 1310 1250 41.2 41.7 43.5 1303 3.9 42.1 2.9 1302 250 42.6 2180 3650 3670 3520 146 147 154 3613 2.3 149 3.0 3754 806 138 9183 738 680 685 30.1 30.7 32.3 701 4.6 31.0 3.7 856 175 38.0 1187 2400 2360 2350 105 105 111 2370 1.1 107 3.1 2696 502 121 1194 330 338 334 55.8 56.4 57.7 334 1.2 56.6 1.7 321 40 53.5 5195 91.5 95.7 94.8 8.58 8.31 8.92 94.0 2.4 8.6 3.6 110 21 14.3 2201 424 452 442 75.3 73.7 77.9 439.3 3.2 75.6 2.8 93.8 38 16.8 1206 26.4 25.9 24.1 60.3 99.8 53.4 25.5 4.8 71.2 35.2 34.9 5.6 44.9 4209 11.8 12.1 12.1 17.3 17.5 18.2 12.0 1.4 17.7 2.7 13.6 1.7 17.2 166 97.1 100 101 17.2 16.9 18.4 99.2 2.0 17.5 4.5 157 50 22.4 0.595 523 523 550 35.1 36.0 37.6 532 2.9 36.2 3.5 532 94 33.9 0.5

Cate

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2 t

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT 2508 2445 2578 133.0 137.0 136.0 2510 2.7 135 1.5 1200 89 90.9 14,4’-DDT 5724 5594 6306 411 433 405 5875 6.5 416 3.5 2078 173 233 82,4’-DDE 399 396 406 13.9 15.4 14.3 400 1.3 14.5 5.3 410 46 14.2 14,4’-DDE 18497 18588 18832 475 537 514 18639 1 509 6.2 22633 1569 497 12,4’-DDD 319 324 329 21.0 24.4 23.4 324 1.5 22.9 7.6 383 45 19.5 14,4’-DDD 1535 1486 1579 98 110 105 1533 3.0 104 5.8 1708 138 120 4HCB 269 256 261 25.5 31.9 26.1 262 2.5 27.8 12.7 262 39 30.6 1-HCH no data no data no data no data no data no data 8.56 2.1 16.9 1-HCH 46.9 49.8 46.0 no data no data no data 47.6 4.2 39.1 3.8 -HCH 58.50 59.10 54.40 no data no data no data 57.33 4.5 4.87 16 3.18 0.0Heptachlor Epoxide 69.3 67.3 70.0 10.8 12.1 12.6 68.9 2.0 12 7.9 41.5 31 10.7 0.0Cis-Chlordane 95.2 91.2 93.7 46.5 52.5 48.1 93.4 2.2 49.0 6.3 92.0 22 48.1 1Trans-Chlordane 7.30 7.30 7.30 9.91 10.90 10.30 7.30 0.0 10.4 4.8 10.1 6.3 11.8 0.5Oxychlordane 58.8 58.1 60.0 17.9 21.6 19.5 59.0 1.6 20 9.4 69.0 9.2 21.2 1Cis-Nonachlor 168 165 167 46.2 52.9 48.7 167 0.9 49.3 6.9 155 33 45.8 3Trans-Nonachlor 440 427 442 157 178 164 436 2 166 6.4 439 86 198 1Dieldrin 414 399 416 48.1 47.7 48.7 410 2.3 48.2 1.0 411 153 50.1 4Mirex 44.6 42.4 44.5 29.4 31.9 32.2 43.8 2.8 31.2 4.9 50.0 9.3 31.0 3

PBDE 47 60.6 62.1 62.2 24.2 23.2 30.8 61.6 1.5 26.1 15.8 147 20 39.6 0.PBDE 99 47.7 53.4 47.3 16.7 15.6 16.4 49.5 6.9 16.2 3.5 22.5 5.5 18.9 2PBDE 100 24.6 26.9 28.7 4.99 5.21 5.03 26.7 7.7 5.08 2.3 28.6 2.2 10.3 1PBDE 153 10.5 10.6 11.1 9.46. 7.65 6.93 10.7 3.0 7.29 7.0 7.16 0.8 8.34 0.5PBDE 154 25.7 23.8 26.7 16.8 15.7 16.9 25.4 5.8 16.5 4.0 21.6 3.0 13.3 1Lipid (mass fraction (%)) 73.3 74.2 73.6 76.8 73.3 74.2 73.7 0.6 74.8 2.4 68.1 1.8 71.9 1

Cate

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2 t

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 10.7 11.3 11.0 2.40 2.00 2.70 11.00 2.7 2.37 14.8 13.6 6.8 4.35 0.528 16.0 15.1 15.4 4.40 4.00 4.50 15.5 3.0 4.30 6.2 24.5 3.3 13.1 131 no data no data no data 3.50 3.60 3.50 3.53 1.6 2.74 1.6 3.56 0.344 25.8 23.5 24.5 8.40 7.90 8.60 24.6 4.7 8.30 4.3 35.9 5.4 12.1 0.549 72.9 66.9 68.9 12.5 12.0 11.8 69.6 4.4 12.1 3.0 99.7 7.4 18.3 0.052 229 211 220 27.1 27.4 26.1 220 4.1 26.9 2.5 309 18 40.7 166/95* see below see below see below see below see below see below 130 56.3087 186 175 181 18.7 19.5 18.1 181 3.0 18.8 3.7 234 68 20.6 299 485 469 492 43.1 48.1 39.2 482 2.4 43.5 10.3 699 134 58.5 5101 (+90) 891 863 885 61.1 68.3 59.2 880 1.7 62.9 7.6 1192 284 78.2 1105 252 233 249 18.7 19.8 18.2 245 4.2 18.9 4.3 376 94 28.6 1118 1003 971 1014 64.5 70.7 62.6 996 2.2 65.9 6.4 1264 269 76.5 2128 404 382 400 20.1 21.7 19.1 395 3.0 20.3 6.5 474 101 23.0 1132 no data no data no data no data no data no data 456 220 21.1 4138 (+163+164) 4102 3841 4006 133 139 136 3983 3.3 136 2.2 4414 833 146 1149 1923 1816 1902 59.3 63.3 60.1 1880 3.0 60.9 3.5 2610 475 89.0 6151 570 535 558 18.6 25.4 18.7 554 3.2 20.9 18.6 802 145 28.6 1153 5712 5473 5765 196 208 198 5650 2.8 201 3.2 6967 1594 228 9156 156 145 151 6.30 7.8 6.4 151 3.7 6.83 12.3 230 42 11.4 0.9170 (+190) 1201 1131 1184 36.0 37.7 38.0 1172 3.1 37.2 2.9 1302 250 42.6 2180 2804 2686 2837 109 114 113 2776 2.9 112 2.4 3754 806 138 9183 692 649 684 28.0 31.6 29.0 675 3.4 29.5 6.3 856 175 38.0 1187 2014 1907 1996 88.9 92.0 91.1 1972 2.9 90.7 1.8 2696 502 121 1194 260 242 257 42.5 43.7 44.0 253 3.8 43.4 1.8 321 40 53.5 5195 66.5 62.7 66.6 6.20 6.70 6.20 65.3 3.4 6.37 4.5 110 21 14.3 2201 49.0 48.8 46.8 8.80 8.80 9.00 48.2 2.5 8.87 1.3 93.8 38 16.8 1206 23.1 20.7 22.6 31.7 28.9 32.0 22.1 5.7 30.9 5.5 34.9 5.6 44.9 4209 no data no data no data no data no data no data 13.6 1.7 17.2 166 115.0 108 111 22.2 21.0 21.0 111 3.2 21.4 3.2 157 50 22.4 0.595 394 366 394 26.0 29.4 25.1 385 4.2 26.8 8.5 532 94 33.9 0.5

Cate

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2 t



Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT 1190 1180 1250 78 90 71 1207 3.1 80 12.0 1200 89 90.9 14,4’-DDT 2110 2230 2190 253 237 228 2177 2.8 239 5.5 2078 173 233 82,4’-DDE 538 544 560 16.9 14.8 14.2 547 2.1 15 9.2 410 46 14.2 14,4’-DDE 23100 25100 23800 523 603 526 24000 4.2 551 8.2 22633 1569 497 12,4’-DDD 457 480 479 22.4 23.6 21.1 472 2.7 22 5.4 383 45 19.5 14,4’-DDD 2110 2250 2330 136 125 140 2230 5.0 133 5.8 1708 138 120 4HCB 356 349 356 41.8 40.8 34.8 354 1.2 39 9.6 262 39 30.6 1-HCH 11.8 <9.6 15.1 15.7 22.7 18.9 13.4 17.6 19 18.6 8.56 2.1 16.9 1-HCH 52.9 45.4 45.6 <10.0 <10.0 <10.0 48.0 8.9 39.1 3.8 -HCH <5.4 <10 <3.8 <3.1 <3.1 <2.6 4.87 16 3.18 0.0Heptachlor Epoxide 111.6 117.3 105.1 14.1 17.3 16.0 111 5.5 16 10.4 41.5 31 10.7 0.0Cis-Chlordane 142.6 143.7 136.2 60.4 62.4 55.0 141 2.9 59 6.5 92.0 22 48.1 1Trans-Chlordane <6.7 <8.1 10.2 10.7 <8.6 10.6 10.2 11 0.4 10.1 6.3 11.8 0.5Oxychlordane 86.7 93.8 89.7 22.0 25.5 21.9 90.1 3.9 23 8.7 69.0 9.2 21.2 1Cis-Nonachlor 218 243 236 50.9 52.9 49.2 233 5.5 51 3.6 155 33 45.8 3Trans-Nonachlor 634 630 608 187 206 175 624 2.3 189 8.3 439 86 198 1Dieldrin 637 584 587 50.3 64.6 57.6 603 4.9 57 12.4 411 153 50.1 4Mirex 68.6 60.9 73.7 <50.0 <50.0 <50.0 67.7 9.6 50.0 9.3 31.0 3

PBDE 47 114 107 101 44.5 40.5 43.7 107 6.0 43 4.9 147 20 39.6 0.PBDE 99 24.6 23.2 20.6 20.5 17.9 17.1 22.8 8.9 19 9.6 22.5 5.5 18.9 2PBDE 100 27.5 33.3 31.8 14.1 12.0 12.00 30.9 9.7 13 9.3 28.6 2.2 10.3 1PBDE 153 6.59 6.90 5.91 12.1 10.2 7.11 6.47 7.8 10 25.8 7.16 0.8 8.34 0.5PBDE 154 15.1 20.2 18.6 14.6 14.4 11.9 18.0 14.7 14 11.3 21.6 3.0 13.3 1Lipid (mass fraction (%)) 69.4 69.8 71.9 67.8 68.8 71.6 70.4 1.9 69 2.9 68.1 1.8 71.9 1

Cate

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2 t

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 11.8 15.2 14.2 <6.7 <9.2 <=9.67 13.7 13 13.6 6.8 4.35 0.528 31.4 30.7 34.2 13.2 14.4 16.9 32.1 5.8 14.9 13 24.5 3.3 13.1 131 no data no data no data no data no data no data 2.7 1.6 3.56 0.344 42.7 41.1 37.9 14.7 15.4 16.8 40.6 6.1 15.6 7.0 35.9 5.4 12.1 0.549 94.0 96.1 88.8 18.7 18.6 17.0 92.9 4.1 18.1 5.3 99.7 7.4 18.3 0.052 321 328 302 39.5 40.9 38.2 317 4.3 39.5 3.5 309 18 40.7 166/95* see below see below see below see below see below see below 130 56.3087 432 465 457 17.1 17.6 18.1 451 3.8 17.6 2.7 234 68 20.6 299 1180 1380 1320 47.7 46.3 44.2 1293 7.9 46.1 3.9 699 134 58.5 5101 (+90) 2030 2300 2260 64.5 68.3 67.9 2197 6.6 66.9 3.1 1192 284 78.2 1105 711 822 746 27.1 27.6 26.8 760 7.5 27.2 1.4 376 94 28.6 1118 2440 2640 2620 72.5 74.4 76.2 2567 4.3 74.3 2.5 1264 269 76.5 2128 882 1050 918 22.2 20.8 20.4 950 9.3 21.1 4.7 474 101 23.0 1132 no data no data no data no data no data no data 456 220 21.1 4138 (+163+164) 6650 7660 6660 113 107 105 6990 8.3 108 3.9 4414 833 146 1149 4320 4910 4670 72.6 68.6 64.7 4633 6.4 68.6 5.8 2610 475 89.0 6151 1280 1460 1400 19.9 20.2 20.7 1380 6.6 20.3 2.0 802 145 28.6 1153 12800 14300 13600 188 184 187 13567 5.5 186 1.1 6967 1594 228 9156 345 422 347 9.13 8.86 8.80 371 12 8.9 2.0 230 42 11.4 0.9170 (+190) 2260 2790 2330 42.6 37.5 37.1 2460 12 39.1 7.9 1302 250 42.6 2180 6660 7860 6840 141 135 135 7120 9.1 137 2.5 3754 806 138 9183 1480 1710 1560 33.3 31.1 31.7 1583 7.4 32.0 3.5 856 175 38.0 1187 4660 5400 4930 109 109 109 4997 7.5 109 0.5 2696 502 121 1194 453 577 481 42.2 44.6 44.4 504 13 43.7 3.1 321 40 53.5 5195 no data no data no data no data no data no data 110 21 14.3 2201 138 161 146 14.8 14.5 14.8 148.4 7.9 14.7 1.1 93.8 38 16.8 1206 46.8 60.7 47.6 39.9 42.8 41.7 51.7 15 41.5 3.6 34.9 5.6 44.9 4209 10.3 10.5 11.7 10.8 13.7 11.5 10.8 7.0 12.0 13 13.6 1.7 17.2 166 223 231 198 18.5 26.5 28.8 217 7.9 24.6 22 157 50 22.4 0.595 no data no data no data no data no data no data #DIV/0! 532 94 33.9 0.5

Cate

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2 t



Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT 960 1100 1040 126 116 123 1033 6.8 122 4.2 1200 89 90.9 14,4’-DDT 1643 1870 1769 234 213 228 1761 6.5 225 4.8 2078 173 233 82,4’-DDE 356 414 377 13.6 11.8 13.6 382 7.7 13 8.0 410 46 14.2 14,4’-DDE 16400 18400 15300 465 447 486 16700 9.4 466 4.2 22633 1569 497 12,4’-DDD 423 457 431 12.3 10.5 12.3 437 4.1 12 8.9 383 45 19.5 14,4’-DDD 1430 1640 1520 127 121 114 1530 6.9 121 5.4 1708 138 120 4HCB 167 154 147 33.7 29.0 29.2 156 6.5 31 8.7 262 39 30.6 1-HCH 7.65 9.60 8.95 15.5 15.5 17.4 8.73 11.4 16 6.8 8.56 2.1 16.9 1-HCH 40.7 49.7 42.2 12.10 7.59 8.38 44.2 10.9 9 25.7 39.1 3.8 -HCH 7.68 8.06 7.46 5.51 5.28 4.72 7.73 3.9 5 7.9 4.87 16 3.18 0.0Heptachlor Epoxide 63.1 73.2 66.1 14.4 14.6 13.9 67.5 7.7 14 2.5 41.5 31 10.7 0.0Cis-Chlordane 53.8 62.0 59.1 37.5 34.1 38.7 58.3 7.1 37 6.5 92.0 22 48.1 1Trans-Chlordane 11.3 9.2 9.3 13.4 14.2 13.4 10.0 11.8 14 3.4 10.1 6.3 11.8 0.5Oxychlordane 51.2 59.0 55.6 19.8 20.0 22.2 55.3 7.1 21 6.4 69.0 9.2 21.2 1Cis-Nonachlor 135.0 151.0 143.0 52.2 49.3 52.0 143.0 5.6 51 3.2 155 33 45.8 3Trans-Nonachlor 465 541 495 181 172 160 500 7.7 171 6.2 439 86 198 1Dieldrin 44.3 40.1 45.1 26.3 33.6 36.9 43 6.2 32 16.8 411 153 50.1 4Mirex 27.0 29.8 29.9 24.2 21.3 21.3 28.9 5.7 22 7.5 50.0 9.3 31.0 3

PBDE 47 215 244 224 70.3 62.7 61.8 228 6.5 65 7.2 147 20 39.6 0.PBDE 99 11.7 10.3 10.3 5.7 7.5 7.6 10.8 7.5 7 15.3 22.5 5.5 18.9 2PBDE 100 33.2 36.2 30.9 24.8 20.6 23.6 33.4 7.9 23 9.4 28.6 2.2 10.3 1PBDE 153 <0.500 <0.500 <0.500 21.8 18.6 23.9 21 12.5 7.16 0.8 8.34 0.5PBDE 154 41.8 47.1 40.7 23.6 21.1 22.1 43.2 7.9 22 5.7 21.6 3.0 13.3 1Lipid (mass fraction (%)) 68.0 68.9 67.4 71.9 72.5 72.2 68.1 1.1 72 0.4 68.1 1.8 71.9 1

Cate



2 t



Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 11.2 10.8 9.2 3.14 2.78 2.96 10.4 10 2.96 6.1 13.6 6.8 4.35 0.528 17.7 15.5 21.9 11.8 11.2 10.9 18.4 18 11.3 4.1 24.5 3.3 13.1 131 8.62 7.74 7.77 8.06 6.74 7.92 8.04 6.2 7.57 9.6 2.7 1.6 3.56 0.344 33.2 30.1 28.9 12.0 11.3 12.0 30.7 7.2 11.8 3.4 35.9 5.4 12.1 0.549 110 93 88 20.1 18.9 20.2 97 12 19.7 3.7 99.7 7.4 18.3 0.052 335 276 265 36.2 34.2 36.9 292 13 35.8 3.9 309 18 40.7 166/95* see below see below see below see below see below see below 13087 89.3 107 123 15.1 17.5 14.3 106 16 15.6 11 234 68 20.6 299 641 663 747 53.6 56.1 63.6 684 8.2 57.8 9.0 699 134 58.5 5101 (+90) 1090 1030 1060 69.8 72.3 81.1 1060 2.8 74.4 8.0 1192 284 78.2 1105 469 483 530 48.0 45.8 50.8 494 6.5 48.2 5.2 376 94 28.6 1118 1320 1310 1340 82.4 85.0 98.1 1323 1.2 88.5 9.5 1264 269 76.5 2128 497 512 572 28.3 28.6 31.1 527 7.5 29.3 5.2 474 101 23.0 1132 243 235 276 20.4 20.4 23 251 8.6 21.3 7.1 456 220 21.1 4138 (+163+164) 3500 3430 3550 124 126 140 3493 1.7 130 6.7 4414 833 146 1149 2400 2440 2490 83.1 86.5 97.0 2443 1.8 88.9 8.2 2610 475 89.0 6151 653 677 762 25.9 26.6 30.4 697 8.2 27.6 8.8 802 145 28.6 1153 6500 6460 6660 196 200 224 6540 1.6 207 7.3 6967 1594 228 9156 378 388 425 23.7 24.8 28.7 397 6.2 25.7 10.2 230 42 11.4 0.9170 (+190) 1320 1300 1340 43.9 44.0 49.1 1320 1.5 45.7 6.5 1302 250 42.6 2180 3520 3450 3550 147 150 170 3507 1.5 156 8.0 3754 806 138 9183 740 761 848 39.0 40.6 44.5 783 7.3 41.4 6.8 856 175 38.0 1187 2480 2460 2540 121 124 139 2493 1.7 128 7.5 2696 502 121 1194 309 315 345 61.3 66.1 71.5 323 6.0 66.3 7.7 321 40 53.5 5195 124 127 137 14.5 14.6 17.3 129 5.3 15.5 10.3 110 21 14.3 2201 375.0 377.0 417.0 83.8 87.3 98.8 389.7 6.1 90.0 8.7 93.8 38 16.8 1206 35.7 35.6 37.3 49.4 51.0 57.5 36.2 2.6 52.6 8.2 34.9 5.6 44.9 4209 8.99 7.88 7.10 9.4 10.2 11.8 8.0 12 10.5 11.6 13.6 1.7 17.2 166 241 247 271 23.7 24.9 28.3 253 6.3 25.6 9.3 157 50 22.4 0.595 351 371 423 28.6 29.5 33.6 382 9.7 30.6 8.7 532 94 33.9 0.5

Cate

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT 1115 1110 1120 68 67 69 1115 0.4 68 1.5 1200 89 90.9 14,4’-DDT 2426 2417 2453 226 226 226 2432 0.8 226 0.0 2078 173 233 82,4’-DDE 393 380 393 12.9 12.4 12.6 389 1.9 12.6 2.0 410 46 14.2 14,4’-DDE 23750 24530 23670 455 467 458 23983 2.0 460 1.4 22633 1569 497 12,4’-DDD 296 295 299 15.6 16.5 15.6 297 0.7 15.9 3.3 383 45 19.5 14,4’-DDD 1620 1626 1643 102 104 102 1630 0.7 103 1.1 1708 138 120 4HCB 254 260 253 23.3 23.5 24.0 256 1.5 23.6 1.5 262 39 30.6 1-HCH 5.20 5.50 5.10 12.7 14.3 13.4 5.27 4.0 13.5 6.0 8.56 2.1 16.9 1-HCH 34.3 33.9 33.4 1.60 1.70 1.60 33.9 1.3 1.63 3.5 39.1 3.8 -HCH 4.00 3.60 3.50 3.80 3.40 2.60 3.70 7.2 3.27 18.7 4.87 16 3.18 0.0Heptachlor Epoxide no data no data no data no data no data no data 41.5 31 10.7 0.0Cis-Chlordane no data no data no data no data no data no data 92.0 22 48.1 1Trans-Chlordane no data no data no data no data no data no data 10.1 6.3 11.8 0.5Oxychlordane 40.1 38.9 37.9 14.0 14.0 13.0 39.0 2.8 13.7 4.2 69.0 9.2 21.2 1Cis-Nonachlor no data no data no data no data no data no data 155 33 45.8 3Trans-Nonachlor 300 296 287 123 126 120 294 2.3 123 2.4 439 86 198 1Dieldrin no data no data no data no data no data no data 411 153 50.1 4Mirex no data no data no data no data no data no data 50.0 9.3 31.0 3

PBDE 47 141 146 142 39.7 40.2 39.1 143 1.9 39.7 1.4 147 20 39.6 0.PBDE 99 20.0 21.0 19.3 18.1 18.0 17.8 20.1 4.3 18.0 0.9 22.5 5.5 18.9 2PBDE 100 24.9 25.6 25.4 9.90 10.10 9.40 25.3 1.4 9.8 3.7 28.6 2.2 10.3 1PBDE 153 7.20 7.40 7.20 9.20 9.90 9.50 7.27 1.6 9.5 3.7 7.16 0.8 8.34 0.5PBDE 154 20.4 21.1 20.7 13.1 12.9 12.3 20.7 1.7 12.8 3.3 21.6 3.0 13.3 1Lipid (mass fraction (%)) 72.1 69.3 72.8 67.3 69.3 70.1 71.4 2.6 68.9 2.1 68.1 1.8 71.9 1

Cate

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 9.0 8.9 8.6 3.30 3.00 3.00 8.83 2.4 3.10 5.6 13.6 6.8 4.35 0.528 21.6 22.2 20.9 9.7 9.7 9.6 21.6 3.0 9.67 0.6 24.5 3.3 13.1 131 no data no data no data no data no data no data 2.7 1.6 3.56 0.344 31.1 31.9 31.5 10.2 11.4 11.6 31.5 1.3 11.1 6.8 35.9 5.4 12.1 0.549 92.3 92.3 91.7 16.2 17.6 16.6 92.1 0.4 16.8 4.3 99.7 7.4 18.3 0.052 304 303 299 37.6 37.3 37.0 302 0.9 37.3 0.8 309 18 40.7 166/95* see below see below see below see below see below see below 130 0.00 0.087 233 237 237 20.6 21.1 20.2 236 1.0 20.6 2.2 234 68 20.6 299 693 703 695 49.1 50.4 49.0 697 0.8 49.5 1.6 699 134 58.5 5101 (+90) 1217 1225 1218 77.1 77.9 77.6 1220 0.4 77.5 0.5 1192 284 78.2 1105 387 388 391 26.8 27.3 27.2 389 0.5 27.1 1.0 376 94 28.6 1118 1273 1296 1279 76.7 78.9 76.9 1283 0.9 77.5 1.6 1264 269 76.5 2128 506 516 515 21.8 22.1 21.5 512 1.1 21.8 1.4 474 101 23.0 1132 462 484 496 17.3 17.6 17.6 481 3.6 17.5 1.0 456 220 21.1 4138 (+163+164) 4070 4241 4100 123 126 123 4137 2.2 124 1.4 4414 833 146 1149 2569 2660 2600 78.5 80.6 78.5 2610 1.8 79.2 1.5 2610 475 89.0 6151 797 818 803 23.5 24.0 23.8 806 1.3 23.8 1.1 802 145 28.6 1153 7369 7680 7502 200 202 200 7517 2.1 201 0.6 6967 1594 228 9156 233 240 237 11.4 11.2 10.9 237 1.5 11.2 2.3 230 42 11.4 0.9170 (+190) 1193 1239 1225 34.2 35.2 33.7 1219 1.9 34.4 2.2 1302 250 42.6 2180 4033 4195 4120 150 146 149 4116 2.0 148 1.4 3754 806 138 9183 838 871 858 33.7 34.9 34.0 856 1.9 34.2 1.8 856 175 38.0 1187 2783 2908 2837 119 124 121 2843 2.2 121 1.8 2696 502 121 1194 304 315 313 52.5 54.6 52.8 311 1.9 53.3 2.1 321 40 53.5 5195 90.6 94.5 93.0 9.30 8.60 8.40 92.7 2.1 8.77 5.4 110 21 14.3 2201 445.0 467.0 456.0 79.1 81.1 79.7 456.0 2.4 80.0 1.3 93.8 38 16.8 1206 34.4 34.1 34.6 50.1 49.4 50.6 34.4 0.7 50.0 1.2 34.9 5.6 44.9 4209 12.8 12.8 12.9 17.9 18.0 18.2 12.8 0.4 18.0 0.8 13.6 1.7 17.2 166 no data no data no data no data no data no data 157 50 22.4 0.595 531 537 533 34.4 35.2 34.2 534 0.6 34.6 1.5 532 94 33.9 0.5

Cate

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT 1040 1100 1180 64.9 74.3 68.9 1107 6.3 69.4 6.8 1200 89 90.9 14,4’-DDT 1980 2210 2150 198 179 181 2113 5.6 186 5.6 2078 173 233 82,4’-DDE 499 524 487 17.8 12.2 10.6 503 3.8 13.5 28 410 46 14.2 14,4’-DDE 22400 21900 23600 383 402 411 22633 3.9 399 3.6 22633 1569 497 12,4’-DDD 387 366 401 16.7 19.5 17.5 385 4.6 17.9 8.1 383 45 19.5 14,4’-DDD 1760 1590 1680 122 114 109 1677 5.1 115 5.7 1708 138 120 4HCB no data no data no data no data no data no data 262 39 30.6 1-HCH no data no data no data 14.0 15.1 14.7 14.6 3.8 8.56 2.1 16.9 1-HCH no data no data no data no data no data no data 39.1 3.8-HCH no data no data no data 2.70 3.50 3.10 3.10 12.9 4.87 16 3.18 0.0Heptachlor Epoxide no data no data no data 5.20 6.70 10.1 7.33 34 41.5 31 10.7 0.0Cis-Chlordane no data no data no data 12.2 10.6 11.1 11.3 7.2 92.0 22 48.1 1Trans-Chlordane no data no data no data 29.3 33.4 40.9 34.5 17.0 10.1 6.3 11.8 0.5Oxychlordane no data no data no data 16.8 18.3 17.6 17.6 4.3 69.0 9.2 21.2 1Cis-Nonachlor no data no data no data 34.7 37.7 41.2 37.9 8.6 155 33 45.8 3Trans-Nonachlor no data no data no data 189 203 222 205 8.1 439 86 198 1Dieldrin no data no data no data 53.6 49.9 47.8 50.4 5.8 411 153 50.1 4Mirex no data no data no data 36.4 37.4 35.8 36.5 2.2 50.0 9.3 31.0 3

PBDE 47 94.2 101 105 34.1 29.3 36.0 100 5.5 33.1 10 147 20 39.6 0.PBDE 99 18.8 20.7 22.4 14.6 17.1 15.9 20.6 8.7 15.9 7.9 22.5 5.5 18.9 2PBDE 100 23.6 19.4 21.4 12.1 9.10 11.0 21.5 9.8 10.7 14.1 28.6 2.2 10.3 1PBDE 153 7.10 5.60 5.90 8.60 7.20 7.90 6.20 12.8 7.90 8.9 7.16 0.8 8.34 0.5PBDE 154 14.9 9.3 9.8 12.6 13.7 11.9 11.3 27 12.7 7.1 21.6 3.0 13.3 1Lipid (mass fraction (%)) 72.1 69.3 72.8 67.3 69.3 70.1 71.4 2.6 68.9 2.1 68.1 1.8 71.9 1

Cate

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 9.00 8.90 8.60 3.30 3.00 3.00 8.83 2.4 3.10 5.6 13.6 6.8 4.35 0.528 21.6 22.2 20.9 9.70 9.70 9.60 21.6 3.0 9.67 0.6 24.5 3.3 13.1 131 no data no data no data no data no data no data 2.74 1.6 3.56 0.344 31.1 31.9 31.5 10.2 11.4 11.6 31.5 1.3 11.1 6.8 35.9 5.4 12.1 0.549 92.3 92.3 91.7 16.2 17.6 16.6 92.1 0.4 16.8 4.3 99.7 7.4 18.3 0.052 304 303 299 37.6 37.3 37.0 302 0.9 37.3 0.8 309 18 40.7 166/95* see below see below see below see below see below see below 13087 233 237 237 20.6 21.1 20.2 236 1.0 20.6 2.2 234 68 20.6 299 693 703 695 49.1 50.4 49.0 697 0.8 49.5 1.6 699 134 58.5 5101 (+90) 1217 1225 1218 77.1 77.9 77.6 1220 0.4 77.5 0.5 1192 284 78.2 1105 387 388 391 26.8 27.3 27.2 389 0.5 27.1 1.0 376 94 28.6 1118 1273 1296 1279 76.7 78.9 76.9 1283 0.9 77.5 1.6 1264 269 76.5 2128 506 516 515 21.8 22.1 21.5 512 1.1 21.8 1.4 474 101 23.0 1132 462 484 496 17.3 17.6 17.6 481 3.6 17.5 1.0 456 220 21.1 4138 (+163+164) 4070 4241 4100 123 126 123 4137 2.2 124 1.4 4414 833 146 1149 2569 2660 2600 78.5 80.6 78.5 2610 1.8 79.2 1.5 2610 475 89.0 6151 797 818 803 23.5 24.0 23.8 806 1.3 23.8 1.1 802 145 28.6 1153 7369 7680 7502 200 202 200 7517 2.1 201 0.6 6967 1594 228 9156 233 240 237 11.4 11.2 10.9 237 1.5 11.2 2.3 230 42 11.4 0.9170 (+190) 1193 1239 1225 34.2 35.2 33.7 1219 1.9 34.4 2.2 1302 250 42.6 2180 4033 4195 4120 150 146 149 4116 2.0 148 1.4 3754 806 138 9183 838 871 858 33.7 34.9 34.0 856 1.9 34.2 1.8 856 175 38.0 1187 2783 2908 2837 119 124 121 2843 2.2 121 1.8 2696 502 121 1194 304 315 313 52.5 54.6 52.8 311 1.9 53.3 2.1 321 40 53.5 5195 90.6 94.5 93.0 9.30 8.60 8.40 92.7 2.1 8.77 5.4 110 21 14.3 2201 445.0 467.0 456.0 79.1 81.1 79.7 456.0 2.4 80.0 1.3 93.8 38 16.8 1206 34.4 34.1 34.6 50.1 49.4 50.6 34.4 0.7 50.0 1.2 34.9 5.6 44.9 4209 12.8 12.8 12.9 17.9 18.0 18.2 12.8 0.4 18.0 0.8 13.6 1.7 17.2 166 no data no data no data no data no data no data 157 50 22.4 0.595 531 537 533 34.4 35.2 34.2 534 0.6 34.6 1.5 532 94 33.9 0.5

Cate

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945

Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PESTICIDE, PBDE, AND 

LIPID RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

2,4’-DDT no data no data no data no data no data no data 1200 89 90.9 14,4’-DDT 121 49 46 <10 <10 <10 72 59.0 2078 173 233 82,4’-DDE no data no data no data no data no data no data 410 46 14.2 14,4’-DDE 850 947 725 24 20 21 841 13.2 22 9.6 22633 1569 497 12,4’-DDD no data no data no data no data no data no data 383 45 19.5 14,4’-DDD <10 <10 <10 <10 <10 <10 1708 138 120 4HCB no data no data no data no data no data no data 262 39 30.6 1-HCH <10 <10 <10 <10 <10 <10 8.56 2.1 16.9 1-HCH <10 <10 <10 <10 <10 <10 39.1 3.8-HCH <10 <10 <10 <10 <10 <10 4.87 16 3.18 0.0Heptachlor Epoxide <10 <10 <10 <10 <10 <10 41.5 31 10.7 0.0Cis-Chlordane <10 <10 <10 <10 <10 <10 92.0 22 48.1 1Trans-Chlordane <10 <10 <10 <10 <10 <10 10.1 6.3 11.8 0.5Oxychlordane no data no data no data no data no data no data 69.0 9.2 21.2 1Cis-Nonachlor no data no data no data no data no data no data 155 33 45.8 3Trans-Nonachlor no data no data no data no data no data no data 439 86 198 1Dieldrin <10 <10 <10 <10 <10 <10 411 153 50.1 4Mirex no data no data no data no data no data no data 50.0 9.3 31.0 3

PBDE 47 no data no data no data no data no data no data 147 20 39.6 0.PBDE 99 no data no data no data no data no data no data 22.5 5.5 18.9 2PBDE 100 no data no data no data no data no data no data 28.6 2.2 10.3 1PBDE 153 no data no data no data no data no data no data 7.16 0.8 8.34 0.5PBDE 154 no data no data no data no data no data no data 21.6 3.0 13.3 1Lipid (mass fraction (%)) NA NA NA NA NA NA 68.1 1.8 71.9 1

Cate

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIII SRM 1945 Homog VIII SRM 1945 Homog VIII SRM 1945
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: Homogenate VIII AND SRM 1945

PCB CONGENER 

RESULTS Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 1/2 95% CI Target Unc

Date(s) of measurements ng/g wet %RSD ng/g wet %RSD Value Value 

18 no data no data no data no data no data no data 13.6 6.8 4.35 0.528 no data no data no data no data no data no data 24.5 3.3 13.1 131 no data no data no data no data no data no data 2.7 1.6 3.56 0.344 no data no data no data no data no data no data 35.9 5.4 12.1 0.549 no data no data no data no data no data no data 99.7 7.4 18.3 0.052 no data no data no data no data no data no data 309 18 40.7 166/95* no data no data no data no data no data no data 13087 no data no data no data no data no data no data 234 68 20.6 299 no data no data no data no data no data no data 699 134 58.5 5101 (+90) no data no data no data no data no data no data 1192 284 78.2 1105 no data no data no data no data no data no data 376 94 28.6 1118 no data no data no data no data no data no data 1264 269 76.5 2128 no data no data no data no data no data no data 474 101 23.0 1132 no data no data no data no data no data no data 456 220 21.1 4138 (+163+164) no data no data no data no data no data no data 4414 833 146 1149 no data no data no data no data no data no data 2610 475 89.0 6151 no data no data no data no data no data no data 802 145 28.6 1153 no data no data no data no data no data no data 6967 1594 228 9156 no data no data no data no data no data no data 230 42 11.4 0.9170 (+190) no data no data no data no data no data no data 1302 250 42.6 2180 no data no data no data no data no data no data 3754 806 138 9183 no data no data no data no data no data no data 856 175 38.0 1187 no data no data no data no data no data no data 2696 502 121 1194 no data no data no data no data no data no data 321 40 53.5 5195 no data no data no data no data no data no data 110 21 14.3 2201 no data no data no data no data no data no data 93.8 38 16.8 1206 no data no data no data no data no data no data 34.9 5.6 44.9 4209 no data no data no data no data no data no data 13.6 1.7 17.2 166 no data no data no data no data no data no data 157 50 22.4 0.595 no data no data no data no data no data no data 532 94 33.9 0.5

Cate

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Data as Submitted by Laboratory (ng/g wet mass) Material Reference Values (ng/g wet mass) 

Homog VIIII SRM 1945

Homog VIIII SRM 1945 Homog VIII SRM 1945
Marine Mammal Interlaboratory Comparison Exericise 2007-- Fatty Acids 

Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Fatty Acid Analysis A Analysis B Analysis C Analysis A Analysis B Analysis C Homog V

(mass percent) (mass percent) (mass percent) (mass percent) (mass percent) (mass percent) Mean 

Lauric acid Dodecanoic acid C12:0 0.133 0.129 0.127 0.181 0.183 0.180 0.130 Myristic acid Tetradecanoic acid C14:0 2.72 2.64 2.60 3.49 3.55 3.43 2.65 Pentadecanoic acid Pentadecanoic acid C15:0 0.338 0.328 0.325 0.331 0.339 0.322 0.33 Palmitic acid Hexadecanoic acid C16:0 8.40 8.18 8.24 7.73 7.88 7.47 8.27 Margaric acid Heptadecanoic acid C17:0 0.277 0.269 0.271 0.216 0.221 0.205 0.27 Stearic acid Octadecanoic acid C18:0 1.63 1.57 1.60 1.27 1.32 1.20 1.60 Arachidic acid Eicosanoic acid C20:0 0.103 0.0993 0.104 0.0940 0.0981 0.0871 0.102 Palmitoleic acid (Z)-9-Hexadecanoic acid C16:1(n-7) 7.38 7.20 7.12 6.36 6.49 6.23 7.23 Vaccenic acid (Z)-11-Octadecenoic acid C18:1(n-7) 1.74 1.70 1.69 1.91 1.94 1.83 1.71 Oleic acid (Z)-9-Octadecanoic acid C18:1(n-9) 17.3 16.8 17.0 14.4 14.8 13.8 17.0 Elaidic acid (E)-9-Octadecenoic acid C18:1(n-9) not measured not measured not measured not measured not measured not measured

(Z)-13-eicosenoic acid C20:1(n-7) 0.185 0.178 0.182 0.226 0.233 0.210 0.182 

Gondoic (Z)-11-eicosenoic acid C20:1(n-9) 3.28 3.17 3.26 4.80 4.94 4.49 3.24 

Gadoleic acid (Z)-9-Eicosenoic acid C:20:1(n-11) 1.04 1.03 1.04 2.94 3.02 2.75 1.04 

Erucic acid (Z)-13-Docosenoic acid C22:1(n-9) 0.429 0.426 0.435 0.605 0.607 0.541 0.430 

Cetoleic (Z)-11-docosenoic acid C22:1(n-11) 2.18 2.09 2.18 4.41 4.63 4.03 2.15 

Nervonic acid (Z)-15-Tetracosenoic acid C24:1(n-9) 0.181 0.172 0.185 0.216 0.228 0.195 0.179 

Linoleic acid (Z,Z)-9,12-Octadecadienoic acid C18:2(n-6) 0.693 0.670 0.673 0.834 0.839 0.798 0.679 

a-Linolenic acid (Z,Z,Z)-9,12,15-Octadecatrienoic acid C18:3(n-3) 0.281 0.274 0.275 0.355 0.360 0.341 0.277 

g-linolenic acid (Z,Z,Z)-6,9,12-Octadecatetraenoic acid C18:3(n-6) 0.0184 0.0193 0.0190 0.0168 0.0156 0.0157 0.019 Stearidonic acid (Z,Z,Z,Z,)-6,9,12,15-Octadecatetraenoic acid C18:4(n-3) 0.146 0.144 0.143 0.147 0.154 0.145 0.144 

Homo-gamma-linoleic acid (Z,Z)-11,14-Eicosadienoic acid C20:2(n-6) 0.218 0.210 0.215 0.232 0.233 0.212 0.214 

Homo-alpha-linolenic acid (Z,Z,Z)-11,14,17-Eicosatrienoic acid C20:3(n-3) 0.154 0.149 0.148 0.152 0.150 0.141 0.150 

Arachidonic acid (Z,Z,Z,Z)-5,8,11,14-Eicosatetraenoic acid C20:4(n-6) 0.351 0.342 0.349 0.236 0.235 0.223 0.347 EPA (Z,Z,Z,Z,Z)-5,8,11,14,17-Eicosapentaenoic acid C20:5(n-3) 1.72 1.67 1.70 1.19 1.17 1.11 1.70 

(Z,Z)-13,16-Docosadienoic acid C22:2(n-6) 0.0206 0.0204 0.0220 0.0196 0.0207 0.0171 0.021 

DPA (Z,Z,Z,Z,Z)-7,10,13,16,19-Docosapentaenoic acid C22:5(n-3) 0.601 0.583 0.600 0.888 0.884 0.820 0.59 

DHA (Z,Z,Z,Z,Z,Z)-4,7,10,13,16,19-Docosahexaenoic Acid C22:6(n-3) 4.48 4.34 4.50 3.98 3.94 3.69 4.44 
Marine Mammal Interlaboratory Comparison Exericise 2007-- Fatty Acids 

Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Fatty Acid Analysis A Analysis B Analysis C Analysis A Analysis B Analysis C Homog VIII 

(mg/g wet wt) (mg/g wet wt) (mg/g wet wt) (mg/g wet wt) (mg/g wet wt) (mg/g wet wt) Mean 

Lauric acid Dodecanoic acid C12:0 0.106 0.109 0.107 0.155 0.160 0.149 0.107 

Myristic acid Tetradecanoic acid C14:0 2.32 2.34 2.26 3.09 3.25 3.03 2.31 

Pentadecanoic acid Pentadecanoic acid C15:0 0.288 0.292 0.281 0.297 0.311 0.294 0.287 

Palmitic acid Hexadecanoic acid C16:0 7.53 7.55 7.29 7.37 7.71 7.21 7.46 

Margaric acid Heptadecanoic acid C17:0 0.271 0.267 0.263 0.240 0.252 0.230 0.267 

Stearic acid Octadecanoic acid C18:0 1.54 1.53 1.47 1.25 1.30 1.21 1.51 

Arachidic acid Eicosanoic acid C20:0 0.09 0.09 0.09 0.09 0.10 0.09 0.09 

Palmitoleic acid (Z)-9-Hexadecanoic acid C16:1(n-7) 6.30 6.34 6.18 5.67 5.94 5.58 6.27 

Vaccenic acid (Z)-11-Octadecenoic acid C18:1(n-7) 1.58 1.58 1.52 1.79 1.88 1.75 1.56 

Oleic acid (Z)-9-Octadecanoic acid C18:1(n-9) 15.8 15.9 15.5 14.0 14.7 13.8 15.7 

Elaidic acid (E)-9-Octadecenoic acid C18:1(n-9) not measured not measured not measured not measured not measured not measured not measured n

(Z)-13-eicosenoic acid C20:1(n-7) 0.198 0.193 0.191 0.239 0.248 0.230 0.194 

Gondoic (Z)-11-eicosenoic acid C20:1(n-9) 3.15 3.09 2.96 4.70 4.94 4.56 3.07 

Gadoleic acid (Z)-9-Eicosenoic acid C:20:1(n-11) 1.09 1.07 1.03 2.99 3.14 2.91 1.06 

Erucic acid (Z)-13-Docosenoic acid C22:1(n-9) 0.38 0.37 0.36 0.56 0.55 0.50 0.37 

Cetoleic (Z)-11-docosenoic acid C22:1(n-11) 2.12 2.12 2.03 4.56 4.81 4.40 2.09 

Nervonic acid (Z)-15-Tetracosenoic acid C24:1(n-9) 0.151 0.139 0.128 0.183 0.194 0.179 0.139 Linoleic acid (Z,Z)-9,12-Octadecadienoic acid C18:2(n-6) 0.592 0.589 0.570 0.746 0.785 0.732 0.584 a-Linolenic acid (Z,Z,Z)-9,12,15-Octadecatrienoic acid C18:3(n-3) 0.237 0.240 0.230 0.313 0.330 0.308 0.236 

g-linolenic acid (Z,Z,Z)-6,9,12-Octadecatetraenoic acid C18:3(n-6) not measured not measured not measured not measured not measured not measured not measured nStearidonic acid (Z,Z,Z,Z,)-6,9,12,15-Octadecatetraenoic acid C18:4(n-3) 0.227 0.228 0.220 0.226 0.241 0.223 0.225 Homo-gamma-linoleic acid(Z,Z)-11,14-Eicosadienoic acid C20:2(n-6) 0.175 0.173 0.162 0.195 0.187 0.168 0.170 

Homo-alpha-linolenic acid(Z,Z,Z)-11,14,17-Eicosatrienoic acid C20:3(n-3) 0.126 0.122 0.115 0.123 0.134 0.120 0.121 

Arachidonic acid (Z,Z,Z,Z)-5,8,11,14-Eicosatetraenoic acid C20:4(n-6) 0.319 0.316 0.306 0.218 0.230 0.216 0.314 EPA (Z,Z,Z,Z,Z)-5,8,11,14,17-Eicosapentaenoic acid C20:5(n-3) 1.63 1.61 1.55 1.10 1.17 1.08 1.60 

(Z,Z)-13,16-Docosadienoic acid C22:2(n-6) not measured not measured not measured not measured not measured not measured not measured n

DPA (Z,Z,Z,Z,Z)-7,10,13,16,19-Docosapentaenoic acid C22:5(n-3) 0.569 0.552 0.535 0.853 0.901 0.926 0.552 DHA (Z,Z,Z,Z,Z,Z)-4,7,10,13,16,19-Docosahexaenoic AciC22:6(n-3) 4.03 3.92 3.79 3.44 3.69 3.36 3.91 
Marine Mammal Interlaboratory Comparison Exericise 2007-- Fatty Acids Lab 

Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Fatty Acid Analysis A Analysis B Analysis C Analysis A Analysis B Analysis C Homog VIII SRM 

(mg/g wet wt) (mg/g wet wt) (mg/g wet wt) (mg/g wet wt) (mg/g wet wt) (mg/g wet wt) Mean 1sd M

Lauric acid Dodecanoic acid C12:0 0.252 0.259 0.253 0.223 0.230 0.225 0.255 0.004 0

Myristic acid Tetradecanoic acid C14:0 2.46 2.55 2.49 3.28 3.38 3.30 2.50 0.05 3

Pentadecanoic acid Pentadecanoic acid C15:0 0.312 0.323 0.318 0.311 0.321 0.316 0.318 0.01 0

Palmitic acid Hexadecanoic acid C16:0 7.83 8.11 7.97 7.41 7.56 7.44 7.97 0.14 7

Margaric acid Heptadecanoic acid C17:0 0.593 0.617 0.603 0.534 0.545 0.538 0.605 0.01 0

Stearic acid Octadecanoic acid C18:0 1.58 1.63 1.60 1.31 1.32 1.31 1.60 0.02 1

Arachidic acid Eicosanoic acid C20:0 0.116 0.118 0.116 0.111 0.111 0.110 0.117 0.00 0

Palmitoleic acid (Z)-9-Hexadecanoic acid C16:1(n-7) 7.23 7.57 7.42 6.46 6.59 6.51 7.41 0.17 6

Vaccenic acid (Z)-11-Octadecenoic acid C18:1(n-7) not measured not measured not measured not measured not measured not measured not measured not measured not m

Oleic acid (Z)-9-Octadecanoic acid C18:1(n-9) 17.4 18.1 17.9 14.6 14.8 14.8 17.8 0.35 1

Elaidic acid (E)-9-Octadecenoic acid C18:1(n-9) 0.132 0.110 0.110 0.080 0.078 0.078 0.117 0.01 0

(Z)-13-eicosenoic acid C20:1(n-7) not measured not measured not measured not measured not measured not measured not measured not measured not m

Gondoic (Z)-11-eicosenoic acid C20:1(n-9) 3.33 3.44 3.40 5.14 5.16 5.15 3.39 0.05 5

Gadoleic acid (Z)-9-Eicosenoic acid C:20:1(n-11) not measured not measured not measured not measured not measured not measured not measured not measured not m

Erucic acid (Z)-13-Docosenoic acid C22:1(n-9) 0.46 0.48 0.47 0.68 0.67 0.67 0.47 0.01 0

Cetoleic (Z)-11-docosenoic acid C22:1(n-11) not measured not measured not measured not measured not measured not measured not measured not measured not m

Nervonic acid (Z)-15-Tetracosenoic acid C24:1(n-9) 0.221 0.236 0.230 0.263 0.266 0.267 0.229 0.01 0

Linoleic acid (Z,Z)-9,12-Octadecadienoic acid C18:2(n-6) 0.769 0.795 0.787 0.922 0.936 0.931 0.784 0.01 0

a-Linolenic acid (Z,Z,Z)-9,12,15-Octadecatrienoic acid C18:3(n-3) 0.273 0.298 0.294 0.390 0.395 0.394 0.288 0.01 0

g-linolenic acid (Z,Z,Z)-6,9,12-Octadecatetraenoic acid C18:3(n-6) 0.019 0.019 0.020 0.019 0.019 0.019 0.020 0.001 0

Stearidonic acid (Z,Z,Z,Z,)-6,9,12,15-Octadecatetraenoic acid C18:4(n-3) not measured not measured not measured not measured not measured not measured not measured not measured not mHomo-gamma-linoleic acid (Z,Z)-11,14-Eicosadienoic acid C20:2(n-6) 0.200 0.205 0.204 0.212 0.214 0.213 0.203 0.003 0

Homo-alpha-linolenic acid (Z,Z,Z)-11,14,17-Eicosatrienoic acid C20:3(n-3) 0.159 0.164 0.164 0.183 0.183 0.183 0.162 0.003 0

Arachidonic acid (Z,Z,Z,Z)-5,8,11,14-Eicosatetraenoic acid C20:4(n-6) 0.504 0.525 0.520 0.353 0.357 0.358 0.516 0.01 0EPA (Z,Z,Z,Z,Z)-5,8,11,14,17-Eicosapentaenoic acid C20:5(n-3) 1.96 2.08 2.03 1.38 1.38 1.38 2.02 0.06 1

(Z,Z)-13,16-Docosadienoic acid C22:2(n-6) not measured not measured not measured not measured not measured not measured not measured not measured not m

DPA (Z,Z,Z,Z,Z)-7,10,13,16,19-Docosapentaenoic acid C22:5(n-3) 0.756 0.802 0.783 1.16 1.16 1.17 0.78 0.02 1

DHA (Z,Z,Z,Z,Z,Z)-4,7,10,13,16,19-Docosahexaenoic AcidC22:6(n-3) 6.02 6.45 6.34 5.47 5.45 5.48 6.27 0.22 5
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: MMCM-1 and SRM 1958

PESTICIDE, PBDE, AND 

LIPID ANALYSES Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements pg/g wet %RSD pg/g wet %RSD Value Value 2,4’-DDT 128 159 147 349 373 349 144 10.8 357 3.8 144 -- 321 54,4’-DDT 1203 1177 1187 239 237 239 1189 1.1 238 0.6 1306 11253 296 22,4’-DDE 486 489 496 539 544 538 490 1.0 540 0.6 450 -- 464 24,4’-DDE 175192 176438 180308 1052 1066 1051 177313 1.5 1056 0.8 201667 18994 1280 112,4’-DDD 71.4 76.1 84.2 411 438 414 77 8.3 421 3.6 77 -- 344 34,4’-DDD 3473 3440 3591 410 414 409 3501 2.3 411 0.5 3226 7283 417 1HCB <25 <25 <25 470 447 469 462 2.8 450 4HCH <25 <25 <25 <25 <25 <25 47 -- 266 4CH <25 <25 <25 <25 <25 <25 1940 -- 284 4

HCH <25 <25 <25 <25 <25 <25 53 -- 322 4

Heptachlor Epoxide NA NA NA NA NA NA 510 -- -- -Cis-Chlordane 652 638 677 444 426 448 656 3.0 439 2.7 656 -- 420 2Trans-Chlordane 120 122 125 424 420 422 123 1.8 422 0.5 2773 -- 422 2Oxychlordane 445 473 443 238 249 260 454 3.7 249 4.4 454 40 230 4Cis-Nonachlor 1734 1770 1670 407 412 448 1725 3.0 422 5.3 1725 208 431 3Trans-Nonachlor 6719 6659 6860 473 473 473 6746 1.5 473 0.0 5809 729 479 1Dieldrin NA NA NA NA NA NA 998 -- -- -Mirex 255 243 236 379 364 378 245 4.0 374 2.2 245 -- 389 5PBDE 47 9221 9210 9337 579 584 578 9256 0.8 580 0.6 9608 1293 661 3PBDE 99 1901 1856 1847 482 439 433 1868 1.6 451 5.9 2095 414 499 1PBDE 100 3478 3499 3520 510 447 454 3499 0.6 470 7.4 3605 290 482 2PBDE 153 754 697 766 455 421 419 739 5.0 432 4.7 739 384 460 5PBDE 154 654 648 655 340 296 299 652 0.6 312 8.0 1298 -- 450 3

Cate



2 t



SRM 1958 MMCM-1

Data as Submitted by Laboratory (pg/g wet mass) Material Reference Values (pg/g wet mass) 

MMCM-1 SRM 1958 MMCM-1 SRM 1958
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: MMCM-1 and SRM 1958

PCB CONGENER 

ANALYSES Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements pg/g wet %RSD pg/g wet %RSD Value Value 18 29.6 30.0 31.9 400 382 399 30 4.0 394 2.6 30 -- 387 728 <25 <25 <25 549 455 548 518 10.5 415 131 w/28 w/28 w/28 w/28 w/28 w/28 -- -

44 114 98 98 382 386 381 104 8.9 383 0.7 104 -- 417 149 343 304 304 416 417 415 317 7.2 416 0.2 264 -- 426 152 613 593 590 404 411 403 599 2.1 406 1.1 629 57 407 266/95* see below see below see below see below see below see below87 659 663 649 335 337 335 657 1.1 336 0.4 657 48 406 499 2515 2504 2471 359 360 358 2497 0.9 359 0.3 2408 323 391 2101 (+90) 2056 2060 2020 339 336 339 2045 1.1 338 0.5 2066 391 415 2105 1198 1174 1161 381 366 381 1178 1.6 376 2.3 1193 112 425 2118 4392 4178 3608 473 457 472 4059 10.0 468 2.0 3873 242 418 3128 1227 1182 1200 350 337 349 1203 1.9 345 2.0 1207 162 427 6 132 w/153 w/153 w/153 w/153 w/153 w/153 533 -- -- -138 (+163+164) 7162 7362 7259 480 485 479 7261 1.4 481 0.7 7743 1492 474 5149 1452 1495 1355 367 356 366 1434 5.0 363 1.7 1447 615 379 1151 299 360 332 359 349 359 331 9.3 356 1.6 424 -- 388 1153 13033 13168 13208 471 481 470 13136 0.7 474 1.3 13136 7785 468 1156 70.2 67.6 67.3 340 333 339 68 2.3 337 1.2 68 -- 424 2170 (+190) 1649 1556 1520 364 351 363 1575 4.2 359 2.1 1603 153 429 2180 5760 5657 5846 399 399 398 5754 1.6 399 0.1 6003 300 470 2183 1340 1298 1346 312 307 312 1328 2.0 310 1.0 1322 627 412 3187 2185 2109 2181 367 362 366 2158 2.0 365 0.8 2047 858 417 3194 1058 1058 1063 337 336 336 1060 0.3 337 0.1 1046 80 393 1195 226 224 218 307 300 307 222 1.9 304 1.4 247 55 392 2201 201 202 206 <25 <25 <25 203 1.3 397 6 206 450 454 457 327 322 326 453 0.8 325 0.9 433 39 373 1209 211 216 222 296 293 295 216 2.6 295 0.6 216 -- 344 266 356 343 331 357 351 356 343 3.6 355 0.9 331 -- 424 295 456 452 446 <25 <25 <25 451 1.1 441 48 -- -

Cate



2 t



SRM 1958 MMCM-1 SRM 1958

Data as Submitted by Laboratory (pg/g wet mass) Material Reference Values (pg/g wet mass) 

MMCM-1 SRM 1958 MMCM-1
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: MMCM-1 and SRM 1958

PESTICIDE, PBDE, AND 

LIPID ANALYSES Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements pg/g wet %RSD pg/g wet %RSD Value Value 2,4’-DDT n/a n/a n/a n/a n/a n/a 144 -- 321 5

4,4’-DDT 22614 23600 26179 ND ND ND 24131 7.6 1306 11253 296 2

2,4’-DDE n/a n/a n/a n/a n/a n/a 450 -- 464 2

4,4’-DDE ND ND ND ND ND ND 201667 18994 1280 11

2,4’-DDD n/a n/a n/a n/a n/a n/a 77 -- 344 34,4’-DDD 17165 17700 18602 ND ND ND 17822 4.1 3226 7283 417 1

HCB ND ND ND 282 288 218 263 14.8 450 4HCH ND ND ND ND ND ND 47 -- 266 4

CH ND ND ND ND ND ND 1940 -- 284 4

HCH ND ND ND ND ND ND 53 -- 322 4

Heptachlor Epoxide 402.8 540.4 585.7 ND ND ND 510 18.7 510 -- -- -Cis-Chlordane 474 530 551 247 274 319 519 7.7 280 13.0 656 -- 420 2Trans-Chlordane 40.3 51.5 44.6 270 263 347 45 12.4 293 15.9 2773 -- 422 2Oxychlordane 431 575 528 ND ND ND 511 14.4 454 40 230 4Cis-Nonachlor 1527 1923 1962 271 319 476 1804 13.4 355 30.2 1725 208 431 3Trans-Nonachlor 5452 6555 6579 279 323 471 6195 10.4 358 28.1 5809 729 479 1Dieldrin ND ND ND ND ND ND 998 -- -- -Mirex ND ND ND 319 374 711 468 45.3 245 -- 389 5PBDE 47 9616 10597 9954 948 934 688 10056 5.0 857 17.1 9608 1293 661 3PBDE 99 2805 2991 2717 716 672 583 2837 4.9 657 10.3 2095 414 499 1PBDE 100 4081 4357 4022 612 536 473 4153 4.3 540 12.9 3605 290 482 2PBDE 153 1299 1330 1185 661 636 543 1272 6.0 613 10.1 739 384 460 5PBDE 154 1312 1366 1215 971 938 905 1298 5.9 938 3.5 1298 -- 450 3

Cate



2 t



SRM 1958 MMCM-1

Data as Submitted by Laboratory (pg/g wet mass) Material Reference Values (pg/g wet mass) 

MMCM-1 SRM 1958 MMCM-1 SRM 1958
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: MMCM-1 and SRM 1958

PCB CONGENER 

ANALYSES Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements pg/g wet %RSD pg/g wet %RSD Value Value 18 ND ND ND ND ND ND 30 -- 387 7

28 481 394 339 547 492 722 405 17.7 587 20.5 415 1

31 ND ND ND ND ND ND -- -44 ND ND ND 571 540 615 575 6.6 104 -- 417 1

49 284 199 148 447 456 382 210 32.7 428 9.5 264 -- 426 152 833 612 626 333 415 382 690 17.9 377 11.0 629 57 407 266/95* see below see below see below see below see below see below87 ND ND ND ND ND ND 657 48 406 499 2444 1459 1753 380 345 416 1885 26.8 380 9.3 2408 323 391 2101 (+90) 1997 1436 1148 217 321 578 1527 28.3 372 50.0 2066 391 415 2105 ND ND ND ND ND ND 1193 112 425 2

118 ND ND ND ND ND ND 3873 242 418 3

128 ND ND ND 330 342 500 391 24.3 1207 162 427 6

132 NA NA NA NA NA NA 533 -- -- -

138 (+163+164) ND ND ND 392 459 783 545 38.4 7743 1492 474 5149 323 262 227 241 263 458 271 17.9 321 37.2 1447 615 379 1151 ND ND ND ND ND ND 424 -- 388 1153 1647 1231 1306 419 475 1050 1395 15.9 648 53.9 13136 7785 468 1156 ND ND ND 277 259 329 288 12.6 68 -- 424 2

170 (+190) 2091 1586 1501 297 297 206 1726 18.5 267 19.7 1603 153 429 2180 7395 5441 5238 339 359 267 6025 19.8 322 15.0 6003 300 470 2183 138 96 104 261 292 324 113 19.8 292 10.8 1322 627 412 3187 595 433 412 277 290 437 480 20.9 335 26.6 2047 858 417 3194 1246 891 1089 264 315 382 1075 16.5 320 18.5 1046 80 393 1195 279 431 238 284 295 442 316 32.2 340 25.9 247 55 392 2201 ND ND ND ND ND ND 397 6206 438 364 359 252 252 328 387 11.4 277 15.8 433 39 373 1209 NA NA NA NA NA NA 216 -- 344 266 334 323 299 259 361 568 319 5.6 396 39.8 331 -- 424 295 478 415 399 ND ND ND 431 9.7 441 48 -- -

Cate



2 t



SRM 1958 MMCM-1 SRM 1958

Data as Submitted by Laboratory (pg/g wet mass) Material Reference Values (pg/g wet mass) 

MMCM-1 SRM 1958 MMCM-1
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: MMCM-1 and SRM 1958

PESTICIDE, PBDE, AND 

LIPID ANALYSES Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements pg/g wet %RSD pg/g wet %RSD Value Value 2,4’-DDT <524 <541 <527 <362 <402 <462 144 -- 321 5

4,4’-DDT 870 932 880 <364 <404 <464 894 3.7 1306 11253 296 22,4’-DDE <529 <546 <532 436 416 <466 426 3.3 450 -- 464 2

4,4’-DDE 202000 204000 199000 1120 1090 1140 201667 1.2 1117 2.3 201667 18994 1280 112,4’-DDD <528 <545 <531 424 455 476 452 5.8 77 -- 344 34,4’-DDD 2520 2540 2420 <369 <409 <470 2493 2.6 3226 7283 417 1HCB <527 <544 <529 <364 <405 <464 450 4

HCH <554 <572 <557 <383 <425 <488 47 -- 266 4CH 1660.00 1620.00 1590.00 <380 <422 <484 1623 2.2 1940 -- 284 4

HCH <528 <545 <530 <365 <405 <465 53 -- 322 4

Heptachlor Epoxide <529 <546 <532 <366 <406 <466 510 -- -- -Cis-Chlordane <528 <545 <530 <365 <405 <465 656 -- 420 2Trans-Chlordane 5450 5430 5390 <368 <408 <469 5423 0.6 2773 -- 422 2Oxychlordane <1410 <1450 <1410 <973 <1080 <1240 454 40 230 4Cis-Nonachlor 1450 1470 1440 <374 <416 <477 1453 1.1 1725 208 431 3Trans-Nonachlor 5450 5430 5390 <368 <408 <469 5423 0.6 5809 729 479 1Dieldrin 898 1140 955 420 440 <465 998 12.7 430 3.3 998 -- -- -Mirex <533 <550 <536 <369 <409 <470 245 -- 389 5PBDE 47 7270 7220 7160 <782 <823 <850 7217 0.8 9608 1293 661 3PBDE 99 2140 2090 2060 <781 <821 <848 2097 1.9 2095 414 499 1PBDE 100 3680 3630 3470 <781 <821 <848 3593 3.1 3605 290 482 2PBDE 153 <986 <1020 <1030 <778 <819 <845 739 384 460 5PBDE 154 <995 <1020 <1040 <785 <826 <853 1298 -- 450 3

Cate



2 t



SRM 1958 MMCM-1

Data as Submitted by Laboratory (pg/g wet mass) Material Reference Values (pg/g wet mass) 

MMCM-1 SRM 1958 MMCM-1 SRM 1958
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: MMCM-1 and SRM 1958

PCB CONGENER 

ANALYSES Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements pg/g wet %RSD pg/g wet %RSD Value Value 18 <533 <550 <535 491 466 494 484 3.2 30 -- 387 7

28 <534 <551 <536 526 483 495 501 4.4 415 131 <402 <414 <404 <278 <308 <354 -- -

44 <532 <549 <535 428 416 <469 422 2.0 104 -- 417 149 <530 <547 <533 408 <407 <468 408 264 -- 426 152 561 <547 <533 444 434 <468 561 439 1.6 629 57 407 266/95* no data no data no data no data no data no data87 663 620 638 373 <410 <470 640 3.4 373 657 48 406 499 2280 2380 2300 <366 <407 <467 2320 2.3 2408 323 391 2101 (+90) 2120 2100 2040 422 411 <471 2087 2.0 417 1.9 2066 391 415 2105 1390 1330 1350 392 355 341 1357 2.3 363 7.3 1193 112 425 2118 3620 3780 3500 500 479 504 3633 3.9 494 2.7 3873 242 418 3128 1240 1200 1180 383 <413 <474 1207 2.5 383 1207 162 427 6 132 no data no data no data no data no data no data 533 -- -- -138 (+163+164) 9760 9920 9560 563 507 562 9747 1.9 544 5.9 7743 1492 474 5149 1450 1490 1440 428 <409 <470 1460 1.8 428 1447 615 379 1151 <538 <555 <540 <372 <413 <474 424 -- 388 1153 1420 1450 1400 <552 <613 <703 1423 1.8 13136 7785 468 1156 <134 <139 <135 <92.8 <103 <118 68 -- 424 2170 (+190) 1600 1670 1540 <366 <407 <467 1603 4.1 1603 153 429 2180 6130 6050 5830 413 <410 <470 6003 2.6 413 6003 300 470 2183 1320 1330 1300 <366 <407 <467 1317 1.2 1322 627 412 3187 1970 1940 1900 <367 <408 <468 1937 1.8 2047 858 417 3194 983 904 834 <370 <411 <472 907 8.2 1046 80 393 1195 <536 <553 <539 <371 <412 <473 247 55 392 2201 no data no data no data no data no data no data 397 6206 <538 <555 <541 <372 <413 <474 433 39 373 1209 <534 <552 <537 <369 <410 <471 216 -- 344 266 <530 <547 <533 <367 <407 <468 331 -- 424 295 404 441 386 <185 <206 <236 410 6.8 441 48 -- -

Cate



2 t



SRM 1958 MMCM-1 SRM 1958

Data as Submitted by Laboratory (pg/g wet mass) Material Reference Values (pg/g wet mass) 

MMCM-1 SRM 1958 MMCM-1
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: MMCM-1 and SRM 1958

PESTICIDE, PBDE, AND 

LIPID ANALYSES Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements pg/g wet %RSD pg/g wet %RSD Value Value 2,4’-DDT 25 38 28 no data no data 30 21.3 144 -- 321 5

4,4’-DDT 193 258 250 no data no data 234 15.2 1306 11253 296 2

2,4’-DDE 80 119 102 no data no data 100 19.3 450 -- 464 24,4’-DDE 36400 56800 50100 no data no data 47767 21.8 201667 18994 1280 112,4’-DDD 17.1 22.5 18.6 no data no data 19 14.4 77 -- 344 3

4,4’-DDD 491 681 584 no data no data 585 16.2 3226 7283 417 1

HCB 30.70 15.80 16.40 no data no data 21 40.2 450 4HCH 23.10 20.90 27.20 no data no data 24 13.5 47 -- 266 4CH 1370.00 1350.00 1480.00 no data no data 1400 5.0 1940 -- 284 4

HCH 27.90 28.20 36.50 no data no data 31 15.8 53 -- 322 4

Heptachlor Epoxide NA NA NA no data no data 510 -- -- -

Cis-Chlordane 126 270 196 no data no data 197 36.5 656 -- 420 2Trans-Chlordane 6 11 18 no data no data 12 51.0 2773 -- 422 2Oxychlordane NA NA NA no data no data 454 40 230 4Cis-Nonachlor 232 398 334 no data no data 321 26.1 1725 208 431 3Trans-Nonachlor 798 1330 1040 no data no data 1056 25.2 5809 729 479 1Dieldrin 262 300 252 no data no data 271 9.3 998 -- -- -Mirex 15 30 24 no data no data 23 32.5 245 -- 389 5PBDE 47 7270 7220 7160 <782 <823 <850 7217 0.8 9608 1293 661 3PBDE 99 2140 2090 2060 <781 <821 <848 2097 1.9 2095 414 499 1PBDE 100 3680 3630 3470 <781 <821 <848 3593 3.1 3605 290 482 2PBDE 153 <986 <1020 <1030 <778 <819 <845 739 384 460 5PBDE 154 <995 <1020 <1040 <785 <826 <853 1298 -- 450 3

Cate



2 t



SRM 1958 MMCM-1

Data as Submitted by Laboratory (pg/g wet mass) Material Reference Values (pg/g wet mass) 

MMCM-1 SRM 1958 MMCM-1 SRM 1958
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: MMCM-1 and SRM 1958

PCB CONGENER 

ANALYSES Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements pg/g wet %RSD pg/g wet %RSD Value Value 18 9.1 9.6 11.0 no data no data no data 9.88 10.0 30.5 -- 387 728 18.5 22.2 22.2 no data no data no data 21.0 10.2 415 131 9.50 8.74 7.6 no data no data no data 8.61 11.1 -- -44 19.2 26.7 25.3 no data no data no data 23.7 16.8 104 -- 417 149 no data no data no data no data no data no data 264 -- 426 152 86.9 127 115 no data no data no data 110 18.8 629 57 407 266/95* no data no data no data87 103 157 139 no data no data no data 133 20.7 657 48 406 499 439 688 606 no data no data no data 578 22.0 2408 323 391 2101 (+90) no data no data no data no data no data no data 2066 391 415 2105 184 272 250 no data no data no data 235 19.5 1193 112 425 2118 605 920 822 no data no data no data 782 20.6 3873 242 418 3128 150 238 210 no data no data no data 199 22.6 1207 162 427 6 132 56.5 91.1 77.4 no data no data no data 75 23.2 533 -- -- -138 (+163+164) 1330 2130 1790 no data no data no data 1750 22.9 7743 1492 474 5149 159 247 207 no data no data no data 204 21.6 1447 615 379 1151 34.8 52.6 44.5 no data no data no data 44.0 20.3 424 -- 388 1153 1450 2330 1980 no data no data no data 1920 23.1 13136 7785 468 1156 9.5 13.5 9.9 no data no data no data 10.9 20.3 68 -- 424 2170 (+190) 176 304 239 no data no data no data 240 26.7 1603 153 429 2180 621 1030 813 no data no data no data 821 24.9 6003 300 470 2183 134 225 184 no data no data no data 181 25.2 1322 627 412 3187 200 333 275 no data no data no data 269 24.8 2047 858 417 3194 98 157 132 no data no data no data 129 23.1 1046 80 393 1195 22.5 36.7 30.1 no data no data no data 30 23.9 247 55 392 2201 117 190 158 no data no data no data 155 23.6 397 6 206 41.0 NA 53 no data no data no data 47.2 18.6 433 39 373 1209 18.9 32.4 24.8 no data no data no data 25.4 26.7 216 -- 344 266 62.0 82.8 78.1 no data no data no data 74.3 14.7 331 -- 424 295 69.9 109 98.0 no data no data no data 92.3 21.8 441 48 -- -

Cate



2 t



SRM 1958 MMCM-1 SRM 1958

Data as Submitted by Laboratory (pg/g wet mass) Material Reference Values (pg/g wet mass) 

MMCM-1 SRM 1958 MMCM-1
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: MMCM-1 and SRM 1958

PESTICIDE, PBDE, AND 

LIPID ANALYSES Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements pg/g wet %RSD pg/g wet %RSD Value Value 2,4’-DDT 200 160 180 430 460 400 180 11.1 430 7.0 144 -- 321 54,4’-DDT 1420 1470 1380 290 270 250 1423 3.2 270 7.4 1306 11253 296 22,4’-DDE 420 400 410 520 510 510 410 2.4 513 1.1 450 -- 464 24,4’-DDE 208500 212000 208000 1410 1360 1390 209500 1.0 1387 1.8 201667 18994 1280 112,4’-DDD < 100 < 100 < 100 400 440 450 430 6.2 77 -- 344 34,4’-DDD 2900 3050 2900 370 360 360 2950 2.9 363 1.6 3226 7283 417 1HCB < 50 < 50 < 50 400 410 370 393 5.3 450 4HCH 45.00 45.00 50.00 245.00 240.00 240.00 47 6.2 242 1.2 47 -- 266 4CH 1950.00 1870.00 2000.00 235.00 240.00 230.00 1940 3.4 235 2.1 1940 -- 284 4

HCH 45.00 60.00 55.00 330.00 300.00 310.00 53 14.3 313 4.9 53 -- 322 4

Heptachlor Epoxide no data no data no data no data no data no data 510 -- -- -Cis-Chlordane no data no data no data no data no data no data 656 -- 420 2Trans-Chlordane no data no data no data no data no data no data 2773 -- 422 2Oxychlordane 440 440 460 190 190 200 447 2.6 193 3.0 454 40 230 4Cis-Nonachlor no data no data no data no data no data no data 1725 208 431 3Trans-Nonachlor 5060 5090 5160 360 370 380 5103 1.0 370 2.7 5809 729 479 1Dieldrin no data no data no data no data no data no data 998 -- -- -Mirex no data no data no data no data no data no data 245 -- 389 5PBDE 47 9950 10010 9920 575 585 580 9960 0.5 580 0.9 9608 1293 661 3PBDE 99 2060 2130 2090 410 410 420 2093 1.7 413 1.4 2095 414 499 1PBDE 100 3560 3680 3610 390 400 400 3617 1.7 397 1.5 3605 290 482 2PBDE 153 640 635 650 360 350 365 642 1.2 358 2.1 739 384 460 5PBDE 154 see below see below see below see below see below see below 1298 -- 450 3

Cate



2 t



SRM 1958 MMCM-1

Data as Submitted by Laboratory (pg/g wet mass) Material Reference Values (pg/g wet mass) 

MMCM-1 SRM 1958 MMCM-1 SRM 1958
2007 EXERCISE FOR ORGANOCHLORINES IN MARINE MAMMAL TISSUES 

SAMPLES: MMCM-1 and SRM 1958

PCB CONGENER 

ANALYSES Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3 lab mean lab lab mean lab Assigned 95% CL Target Unc

Date(s) of measurements pg/g wet %RSD pg/g wet %RSD Value Value 18 < 50 < 50 < 50 no data no data no data 30.5 -- 387 728 < 50 < 50 < 50 no data no data no data 415 1

31 < 50 < 50 < 50 no data no data no data -- -

44 < 20 < 20 < 20 410 360 420 397 8.1 104 -- 417 149 380 400 410 660 620 530 397 3.9 603 11.0 264 -- 426 152 640 650 690 480 510 510 660 4.0 500 3.5 629 57 407 266/95* resolved resolved resolved resolved resolved resolved

87 670 760 730 410 420 450 720 6.4 427 4.9 657 48 406 499 2620 2660 2660 390 380 380 2647 0.9 383 1.5 2408 323 391 2101 (+90) 2480 2520 2500 380 400 400 2500 0.8 393 2.9 2066 391 415 2105 1210 1150 1220 365 370 385 1193 3.2 373 2.8 1193 112 425 2118 3860 3890 3870 420 400 410 3873 0.4 410 2.4 3873 242 418 3128 1410 1550 1400 430 370 400 1453 5.8 400 7.5 1207 162 427 6 132 550 520 530 < 20 < 20 < 20 533 2.9 533 -- -- -138 (+163+164) 7630 7880 7720 440 470 433 7743 1.6 448 4.4 7743 1492 474 5149 1640 1620 1670 480 410 480 1643 1.5 457 8.8 1447 615 379 1151 510 540 500 380 400 360 517 4.0 380 5.3 424 -- 388 1153 13510 13485 13600 420 400 420 13532 0.4 413 2.8 13136 7785 468 1156 < 40 < 40 < 40 440 530 480 483 9.3 68 -- 424 2170 (+190) 1835 1810 1820 345 350 350 1822 0.7 348 0.8 1603 153 429 2180 6400 6205 6249 395 395 405 6285 1.6 398 1.4 6003 300 470 2183 1495 1495 1510 310 300 335 1500 0.6 315 5.7 1322 627 412 3187 2425 2400 2510 350 350 370 2445 2.4 357 3.2 2047 858 417 3194 1080 1010 1010 260 360 380 1033 3.9 333 19.3 1046 80 393 1195 220 250 270 no data no data no data 247 10.2 247 55 392 2201 1430 1440 1480 330.00 360.00 380.00 1450 1.8 357 7.1 397 6 206 450 450 400 < 50 < 50 < 50 433 6.7 433 39 373 1209 no data no data no data no data no data no data 216 -- 344 266 no data no data no data no data no data no data 331 -- 424 295 500 520 550 < 20 < 20 < 20 523 4.8 441 48 -- -

Cate



2 t



SRM 1958 MMCM-1 SRM 1958

Data as Submitted by Laboratory (pg/g wet mass) Material Reference Values (pg/g wet mass) 

MMCM-1 SRM 1958 MMCM-1
Appendix B

Graphical results of PCB congener and lipid data reported by all laboratories. 

The Z-scores for Homogenate VIII represent 25 % of the assigned value so 

that z = +1 is the assigned value plus 25 %, z = -1 is the assigned value minus 

25 % and so forth. Error bars are ± 1 standard deviation.
0

5

10

15

20

25

30

35

40

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 18

Assigned value = 13.6 ng/g SD = 7.8 ng/g 95% CI = ± 6.8 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 5

Homogenate VIII (Female Pilot Whale)

0

1

2

3

4

5

6

7

8

9

10

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 18

Value = 4.4 ± 0.56 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

5

10

15

20

25

30

35

40

45

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 28

Assigned value = 24.5 ng/g SD = 4.5 ng/g 95% CI = ± 3.3 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 7

Homogenate VIII (Female Pilot Whale)

0

2

4

6

8

10

12

14

16

18

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 28

Value = 13.1 ± 1.1 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0.0

2.0

4.0

6.0

8.0

10.0

12.0

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 31

Assigned value = 2.74 ng/g SD = 1.7 ng/g 95% CI = ± 1.64 ng/g (wet basis)

Reported Results: 6 Quantitative Results: 4

Homogenate VIII (Female Pilot Whale)

0

1

2

3

4

5

6

7

8

9

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 31

Value = 3.6 ± 0.36 ng/g (wet basis)

Reported Results: 9 

SRM 1945
0

10

20

30

40

50

60

70

80

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 44

Assigned value = 35.9 ng/g SD = 8.3 ng/g 95% CI = ± 5.4 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 9

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 44

Value = 12.1 ± 0.51 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

20

40

60

80

100

120

140

160

180

200

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 49

Assigned value = 100 ng/g SD = 12 ng/g 95% CI = ± 7.4 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 49

Value = 18.3 ± 0.1 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

100

200

300

400

500

600

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 52

Assigned value = 309 ng/g SD = 29 ng/g 95% CI = ± 18 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

10

20

30

40

50

60

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 52

Value = 40.7 ± 1.3 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

50

100

150

200

250

300

350

400

450

500

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 87

Assigned value = 234 ng/g SD = 98 ng/g 95% CI = ± 68 ng/g (wet basis)

Reported Results: 8 Quantitative Results: 8

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 87

Value = 20.6 ± 2.6 ng/g (wet basis)

Reported Results: 9 

SRM 1945
0

200

400

600

800

1000

1200

1400

1600

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 99

Assigned value = 699 ng/g SD = 217 ng/g 95% CI = ± 134 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

10

20

30

40

50

60

70

80

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 99

Value = 58.5 ± 5.2 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

500

1000

1500

2000

2500

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 101 (+90)

Assigned value = 1192 ng/g SD = 410 ng/g 95% CI = ± 284 ng/g (wet basis)

Reported Results: 8 Quantitative Results: 8

Homogenate VIII (Female Pilot Whale)

0

20

40

60

80

100

120

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 101 (+90)

Value = 78 ± 12 ng/g (wet basis)

Reported Results: 9 

SRM 1945
0

100

200

300

400

500

600

700

800

900

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 105

Assigned value = 376 ng/g SD = 144 ng/g 95% CI = ± 94 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 9

Homogenate VIII (Female Pilot Whale)

0

10

20

30

40

50

60

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 105

Value = 28.6 ± 1.2 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

500

1000

1500

2000

2500

3000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 118

Assigned value = 1264 ng/g SD = 435 ng/g 95% CI = ± 269 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

20

40

60

80

100

120

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 118

Value = 76.5 ± 2.9 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

200

400

600

800

1000

1200

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 128

Assigned value = 474 ng/g SD = 171 ng/g 95% CI = ± 101 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 11

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

35

40

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 128

Value = 23.0 ± 1.1 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

100

200

300

400

500

600

700

800

900

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 132

Assigned value = 456 ng/g SD = 225 ng/g 95% CI = ± 220 ng/g (wet basis)

Reported Results: 4 Quantitative Results: 4

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 132

Value = 21.1 ± 4.8 ng/g (wet basis)

Reported Results: 5 

SRM 1945
0

1000

2000

3000

4000

5000

6000

7000

8000

9000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 138 (+163+164)

Assigned value = 4414 ng/g SD = 1124 ng/g 95% CI = ± 833 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 7

Homogenate VIII (Female Pilot Whale)

0

50

100

150

200

250

300

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 138 (+163+164)

Value = 146 ± 13 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

1000

2000

3000

4000

5000

6000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 149

Assigned value = 2610 ng/g SD = 727 ng/g 95% CI = ± 475 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 9

Homogenate VIII (Female Pilot Whale)

0

20

40

60

80

100

120

140

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 149

Value = 89.0 ± 6.9 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

200

400

600

800

1000

1200

1400

1600

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 151

Assigned value = 802 ng/g SD = 234 ng/g 95% CI = ± 145 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

35

40

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 151

Value = 28.6 ± 1.3 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

2000

4000

6000

8000

10000

12000

14000

16000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 153

Assigned value = 6967 ng/g SD = 2440 ng/g 95% CI = ± 1594 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 9

Homogenate VIII (Female Pilot Whale)

0

50

100

150

200

250

300

350

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 153

Value = 228 ± 10 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

50

100

150

200

250

300

350

400

450

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 156

Assigned value = 230 ng/g SD = 57 ng/g 95% CI = ± 42 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 7

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 156

Value = 11 .4 ± 0.9 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

500

1000

1500

2000

2500

3000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 170 (+190)

Assigned value = 1302 ng/g SD = 404 ng/g 95% CI = ± 250 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

10

20

30

40

50

60

70

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 170 (+190)

Value = 42.6 ± 2.2 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

1000

2000

3000

4000

5000

6000

7000

8000

9000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 180

Assigned value = 3754 ng/g SD = 1233 ng/g 95% CI = ± 806 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 9

Homogenate VIII (Female Pilot Whale)

0

20

40

60

80

100

120

140

160

180

200

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 180

Value = 138 ± 10 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

200

400

600

800

1000

1200

1400

1600

1800

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 183

Assigned value = 856 ng/g SD = 268 ng/g 95% CI = ± 175 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 9

Homogenate VIII (Female Pilot Whale)

0

10

20

30

40

50

60

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 183

Value = 38.0 ± 1.8 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

1000

2000

3000

4000

5000

6000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 187

Assigned value = 2696 ng/g SD = 810 ng/g 95% CI = ± 502 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

20

40

60

80

100

120

140

160

180

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 187

Value = 121 ± 11 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

100

200

300

400

500

600

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 194

Assigned value = 321 ng/g SD = 65 ng/g 95% CI = ± 40 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

10

20

30

40

50

60

70

80

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 194

Value = 53.5 ± 5.2 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

50

100

150

200

250

300

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 195

Assigned value = 110 ng/g SD = 24 ng/g 95% CI = ± 21 ng/g (wet basis)

Reported Results: 9 Quantitative Results: 5

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 195

Value = 14.3 ± 2.2 ng/g (wet basis)

Reported Results: 10 

SRM 1945
0

50

100

150

200

250

300

350

400

450

500

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 201

Assigned value = 94 ng/g SD = 34 ng/g 95% CI = ± 38 ng/g (wet basis)

Reported Results: 9 Quantitative Results: 3

Homogenate VIII (Female Pilot Whale)

0

20

40

60

80

100

120

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 201

Value = 16.8 ± 1.3 ng/g (wet basis)

Reported Results: 10 

SRM 1945
0

10

20

30

40

50

60

70

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 206

Assigned value = 35 ng/g SD = 7 ng/g 95% CI = ± 6 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 6

Homogenate VIII (Female Pilot Whale)

0

20

40

60

80

100

120

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 206

Value = 44.9 ± 4.2 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

5

10

15

20

25

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 209

Assigned value = 14 ng/g SD = 2 ng/g 95% CI = ± 2 ng/g (wet basis)

Reported Results: 9 Quantitative Results: 6

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 209

Value = 17.2 ± 1.9 ng/g (wet basis)

Reported Results: 10 

SRM 1945
0

50

100

150

200

250

300

350

400

450

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 66

Assigned value = 157 ng/g SD = 67 ng/g 95% CI = ± 50 ng/g (wet basis)

Reported Results: 8 Quantitative Results: 7

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

35

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 66

Value = 22.4 ± 0.5 ng/g (wet basis)

Reported Results: 9 

SRM 1945
0

100

200

300

400

500

600

700

800

900

1000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PCB 95

Assigned value = 532 ng/g SD = 117 ng/g 95% CI = ± 94 ng/g (wet basis)

Reported Results: 7 Quantitative Results: 6

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

35

40

45

50

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PCB 95

Value = 33.9 ± 0.5 ng/g (wet basis)

Reported Results: 8 

SRM 1945
Appendix C

Graphical results of pesticide and lipid data reported by all laboratories. The 

Z-scores for Homogenate VIII represent 25 % of the assigned value so that z = 

+1 is the assigned value plus 25 %, z = -1 is the assigned value minus 25 % and 

so forth. Error bars are ± 1 standard deviation.
0

500

1000

1500

2000

2500

3000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

2,4’-DDT

Assigned value = 1200 ng/g SD = 128 ng/g 95% CI = ± 89 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 8

Homogenate VIII (Female Pilot Whale)

0

20

40

60

80

100

120

140

160

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

2,4’-DDT

Value = 91 ± 13 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

1000

2000

3000

4000

5000

6000

7000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

4,4’-DDT

Assigned value = 2078 ng/g SD = 280 ng/g 95% CI = ± 173 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

50

100

150

200

250

300

350

400

450

500

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

4,4’-DDT

Value = 233 ± 8 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

100

200

300

400

500

600

700

800

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

2,4’-DDE

Assigned value = 410 ng/g SD = 78 ng/g 95% CI = ± 46 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 11

Homogenate VIII (Female Pilot Whale)

0

2

4

6

8

10

12

14

16

18

20

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

2,4’-DDE

Value = 14 .2 ± 1.4 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

5000

10000

15000

20000

25000

30000

35000

40000

45000

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

4,4’-DDE

Assigned value = 22633 ng/g SD = 2655 ng/g 95% CI = ± 1569 ng/g (wet basis)

Reported Results: 13 Quantitative Results: 11

Homogenate VIII (Female Pilot Whale)

0

100

200

300

400

500

600

700

800

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

4,4’-DDE

Value = 497 ± 19 ng/g (wet basis)

Reported Results: 13 

SRM 1945
0

100

200

300

400

500

600

700

800

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

2,4’-DDD

Assigned value = 383 ng/g SD = 73 ng/g 95% CI = ± 45 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

2,4’-DDD

Value = 19.5 ± 1.2 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

500

1000

1500

2000

2500

3000

3500

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

4,4’-DDD

Assigned value = 1708 ng/g SD = 223 ng/g 95% CI = ± 138 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

20

40

60

80

100

120

140

160

180

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

4,4’-DDD

Value = 120 ± 5 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

50

100

150

200

250

300

350

400

450

500

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

HCB

Assigned value = 262 ng/g SD = 66 ng/g 95% CI = ± 39 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 11

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

35

40

45

50

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

HCB

Value = 30.6 ± 1.5 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

5

10

15

20

25

30

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

alpha-HCH

Assigned value = 9 ng/g SD = 3 ng/g 95% CI = ± 2 ng/g (wet basis)

Reported Results: 8 Quantitative Results: 7

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

35

40

45

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

alpha-HCH

Value = 16.9 ± 1.4 ng/g (wet basis)

Reported Results: 10 

SRM 1945
0

10

20

30

40

50

60

70

80

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

beta-HCH

Assigned value = 39 ng/g SD = 5 ng/g 95% CI = ± 4 ng/g (wet basis)

Reported Results: 9 Quantitative Results: 6

Homogenate VIII (Female Pilot Whale)

0

2

4

6

8

10

12

14

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

beta-HCH

No Value

Reported Results: 5 

SRM 1945
0

10

20

30

40

50

60

70

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

gamma-HCH

Assigned value = 5 ng/g SD = 20 ng/g 95% CI = ± 16 ng/g (wet basis)

Reported Results: 8 Quantitative Results: 6

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

35

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

gamma-HCH

Value = 3 .8 ± 0.01 ng/g (wet basis)

Reported Results: 8 

SRM 1945
0

20

40

60

80

100

120

140

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

Heptachlor Epoxide

Assigned value = 42 ng/g SD = 32 ng/g 95% CI = ± 31 ng/g (wet basis)

Reported Results: 8 Quantitative Results: 4

Homogenate VIII (Female Pilot Whale)

0

2

4

6

8

10

12

14

16

18

20

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

Heptachlor Epoxide

Value = 10.7 ± 0.01 ng/g (wet basis)

Reported Results: 9 

SRM 1945
0.0

20.0

40.0

60.0

80.0

100.0

120.0

140.0

160.0

180.0

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

Cis-Chlordane

Assigned value = 92 ng/g SD = 27 ng/g 95% CI = ± 22 ng/g (wet basis)

Reported Results: 9 Quantitative Results: 6

Homogenate VIII (Female Pilot Whale)

0

10

20

30

40

50

60

70

80

90

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

Cis-Chlordane

Value = 48 .1 ± 1.6 ng/g (wet basis)

Reported Results: 10 

SRM 1945
0

5

10

15

20

25

30

35

40

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

Trans-Chlordane

Assigned value = 10 ng/g SD = 9 ng/g 95% CI = ± 6 ng/g (wet basis)

Reported Results: 9 Quantitative Results: 8

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

35

40

45

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

Trans-Chlordane

Value = 11.8 ± 0.5 ng/g (wet basis)

Reported Results: 10 

SRM 1945
0

20

40

60

80

100

120

140

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

Oxychlordane

Assigned value = 69 ng/g SD = 13 ng/g 95% CI = ± 9 ng/g (wet basis)

Reported Results: 9 Quantitative Results: 8

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

Oxychlordane

Value = 21.2 ± 1.1 ng/g (wet basis)

Reported Results: 10 

SRM 1945
0

50

100

150

200

250

300

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

Cis-Nonachlor

Assigned value = 155 ng/g SD = 47 ng/g 95% CI = ± 33 ng/g (wet basis)

Reported Results: 8 Quantitative Results: 8

Homogenate VIII (Female Pilot Whale)

0

10

20

30

40

50

60

70

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

Cis-Nonachlor

Value = 48.5 ± 3.3 ng/g (wet basis)

Reported Results: 9 

SRM 1945
0

100

200

300

400

500

600

700

800

900

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

Trans-Nonachlor

Assigned value = 439 ng/g SD = 124 ng/g 95% CI = ± 86 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 8

Homogenate VIII (Female Pilot Whale)

0

50

100

150

200

250

300

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

Trans-Nonachlor

Value = 198 ± 16 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

200

400

600

800

1000

1200

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

Dieldrin

Assigned value = 411 ng/g SD = 221 ng/g 95% CI = ± 153 ng/g (wet basis)

Reported Results: 9 Quantitative Results: 8

Homogenate VIII (Female Pilot Whale)

0

10

20

30

40

50

60

70

80

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

Dieldrin

Value = 50 .1 ± 4.1 ng/g (wet basis)

Reported Results: 10 

SRM 1945
0

10

20

30

40

50

60

70

80

90

100

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

Mirex

Assigned value = 50 ng/g SD = 13 ng/g 95% CI = ± 9 ng/g (wet basis)

Reported Results: 8 Quantitative Results: 8

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

35

40

45

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

Mirex

Value = 31.0 ± 3.4 ng/g (wet basis)

Reported Results: 8 

SRM 1945
0

20

40

60

80

100

120

140

0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

Lipid

Assigned value = 68 ng/g SD = 3 ng/g 95% CI = ± 2 ng/g (wet basis)

Reported Results: 12 Quantitative Results: 15

Homogenate VIII (Female Pilot Whale)

Labs 14, 15, and 16 are 1fa, 2fa and 3fa, respectively

0

10

20

30

40

50

60

70

80

90

100

0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

Lipid

Value = 71.9 ± 1.3 ng/g (wet basis)

Reported Results: 15 

SRM 1945

Labs 14, 15, and 16 are 1fa, 2fa and 3fa, respectively
Appendix D

Graphical results of PBDE congener data reported by all laboratories. The Zscores for Homogenate VIII represent 25 % of the assigned value so that z = 

+1 is the assigned value plus 25 %, z = -1 is the assigned value minus 25 % and 

so forth. Error bars are ± 1 standard deviation.
0

50

100

150

200

250

300

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PBDE 47

Assigned value = 147 ng/g SD = 31 ng/g 95% CI = ± 20 ng/g (wet basis)

Reported Results: 12 Quantitative Results: 9

Homogenate VIII (Female Pilot Whale)

0

10

20

30

40

50

60

70

80

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PBDE 47

Value = 39.6 ± 0.18 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

10

20

30

40

50

60

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PBDE 99

Assigned value = 23 ng/g SD = 9 ng/g 95% CI = ± 5 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PBDE 99

Value = 18.9 ± 2.3 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0

10

20

30

40

50

60

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PBDE 100

Assigned value = 29 ng/g SD = 3 ng/g 95% CI = ± 2 ng/g (wet basis)

Reported Results: 11 Quantitative Results: 9

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PBDE 100

Value = 10.3 ± 1.1 ng/g (wet basis)

Reported Results: 12 

SRM 1945
0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PBDE 153

Assigned value = 7 ng/g SD = 1 ng/g 95% CI = ± 1 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 10

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

30

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PBDE 153

Value = 8.34 ± 0.55 ng/g (wet basis)

Reported Results: 11 

SRM 1945
0

5

10

15

20

25

30

35

40

45

50

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Assigned Value

± 1 Z

± 2 Z

± 3 Z

PBDE 154

Assigned value = 22 ng/g SD = 4 ng/g 95% CI = ± 3 ng/g (wet basis)

Reported Results: 10 Quantitative Results: 8

Homogenate VIII (Female Pilot Whale)

0

5

10

15

20

25

0 1 2 3 4 5 6 7 8 9 10 11 12 13

ng/g wet basis

Laboratory

Certified or Reference Value

± Uncertainty

± 30 % of Ceritfied or Reference Value

PBDE 154

Value = 13.3 ± 1.7 ng/g (wet basis)

Reported Results: 10 

SRM 1945
Appendix E

Tabular summary of methods used for analysis by each laboratory.
Summary of Methods Used

Laboratory Procedure used to measure Lipid

Unknown SRM 1945 SRM 1945 Homog. VII

1 1 1

Subsampled the dichloromethane extract,

evaporated the solvent and weighed the remaining

residue. wet wet

2 1 1

Gravimetrically remove approx. 1/10 of the extract 

and allow solvent to evaporate off. Check mass 

until stable for 24h period. wet wet

3 1 1

Gravimetric determination; ASE extraction using 

dichloromethane. Iatroscan (TLC/FID) 

determination also reported (uses same extract). wet wet

4 2.32 to 2.86 2.84 to 4.32

After extraction with dichloromethane, the 

extracts of Homognate IV and SRM 1945 were 

concentrated to 10 mL. Then, 20% by volume of 

these extracts was added to a previously weighed 

and dried aluminum pan. The contents were 

allowed to evaporate, and the pan was reweighed. wet wet

5 1 1 gravimetric wet wet

6 2.97, 2.93, 2.95 4.09, 4.00, 4.03

Total extractable lipids (gravimetric from Soxhlet

extract) wet wet

7 avg = 0.2295 avg = 0.2271

Extraction of sample via mixing with sodium 

sulfate (50 g), grinding via mortar and pestle. 

Transfer to glass column and elution with 300 mL 

1:1 dichloromethane and Hexane. Evaporation of 

solvent and weighing of remaining lipid extract. wet wet

8 1 Gravimeteric wet wet

9 0.8 0.8

Lipid content was determined gravimetrically 

using the 10% of the extract wet wet

10 1 1 Gravimeteric wet wet

11 0.15 - 0.23 0.13 - 0.18 Gravimeteric wet wet

12 1.2 1.2 Gravimeteric wet wet

13 1 1 Not measured wet wet

1s 5 5 Not requested wet wet

2s 3 3 Not requested wet wet

3s 1.5 1.5 Not requested wet wet

4s 4.42 Not requested wet wet

5s 1 1 Not requested wet wet

1fa 1 1

Iatroscan (TLC/FID) determination also reported

(uses same extract). Iatroscan (TLC/FID)

determination also reported (uses same extract). wet wet

2fa 1 1 Gravimeteric wet wet

3fa 0.035 0.039

Lipid extracted with chloroform/methanol (2:1)

using Homogenizer with Teflon grinding pestle.

The moisture was taken out from the extract using

anhydrous Sodium Sulfate; an aliquot was taken

into pre-weighed aluminum cup for gravimetric

analysis. wet wet

Approximate mass of sample 

extracted (g):

Were "wet" or "dry" samples 

extracted?
Summary of Methods Used

Laborator

y Extraction Method

Extraction 

Solvent

Extraction 

Time Extraction Other Sample Extract Cleanup Method

1

Pressurized Fluid 

Extraction (Dionex, ASE) Dichloromethane 15 min

Sample dried with 45 g sodium sulfate, 

then packed into a 33 mL PFE cell. 

PFE Conditions: cell temp 100 °C. 

equilibration 5 min, static time 5 min, 

cell pressure 2000 psi and there were 

three cylces. Samples were first run 

through a Gel Permeation chrom

Samples were first run through a size 

exclusion chromatogramphy (SEC) column 

(Phenomenex) using DCM . as the mobile 

phase. Eluent containing orgaonochlorines 

was further refined by passing though a ca. 2

g alumina solid phase extraction cartridge 

eluting with 12 mL 25% DCM:75% hexane 

(volume fraction)

2

Pressurized Fluid 

Extraction (Dionex, ASE) Dichloromethane 15 min 100 °C; 2000 psi, 3 cycles; 90 sec purge

Sulfuric acid to remove lipids - back extract 

into hexane concentrate and elute through 

silica SPE column using 15 mL of 10% 

dichloromethane in hexane.

3

Pressurized Fluid 

Extraction (Dionex, ASE) Dichloromethane ~16 min.

ASE conditions: Pressure = 2000 psi, 

temperature = 100 °C

Gravity flow column with silca and neutral 

alumina, followed by HPLC-SEC to elute 

fraction containing pesticides, PCB and 

PBDE congeners.

4

Dionex Model 300 

Accelerated Solvent 

Extractor (ASE) Dichloromethane 20 min

The extraction temperature was 100 °C 

at a pressure of 1500-psi. Each sample 

was extracted three times. The first 

cycle used a static time of 10 min. The 

last two cycles used a static time of 5 

min. 

Each extract was eluted through a glass 

chromatography column packed with 

florisil, alumina, and silica and was 

concentrated to 10 mL. A single, 2 mL. 

portion of this eluate was diluted to 5 mL 

with methylene chloride. The unused 

portion of each sample was stored away as a 

reserve. Each 5 mL portion was manually 

injected into a single Phenogel, size 

exclusion HPLCcolumn (60 cm x 2.1 cm). 

Each HPLC-cleaned fraction was 

concentrated, the solvent was exchanged to 

hexane, and the sample column (60 cm x 

2.1 cm). Each HPLC-cleaned fraction was 

concentrated, the solvent was exchanged to 

hexane, and the sample volume was 

adjusted to 5 mL for initial GC screening. 

After screening, each sample was 

concentrated to 1mL for final data collection 

on DB-5 0.25 mm ID x 60 m L x 0.25 um 

film thickness fused silica capillary column.

5

Pressurized Fluid 

Extraction (Dionex, ASE) Dichloromethane 20 min Gel permeation and florisil chromatography.

6 Soxhlet

Hexane:acetone 

(1:1)

Alumina cleanup followed by silica gel 

fractionation.

7

Extraction of sample via 

mixing with sodium 

sulfate (50 g), grinding 

via mortar and pestle , 

transfer to glass column.

300 ml 1:1 

DCM:Hexane. 3 hours

PCBS / PBDEs / PCDD/Fs -change solvent 

from 1:1 to Hexane Utilize FMS 

instrumentation and specific programs with 

Acidic Silica Columns ; Acid Base Neutral 

Silica Columns ; Basic Alumina Columns ; 

Carbon Fibre Columns . Pesticides-----Add 

extracts to conditioned neutral Florisil (pass 

extracts through three columns).

8

Mix with sodium sulphate 

and extract in glass 

column

300 mL of 

DichlormethaneHexane (1:1) 1 hour Rotovap to fixed volume

As per our method MET-CHEM-OC-06B 

(May 2007). Spiked with a mixture of 13C 

surrogates and placed on GPC for lipid and 

other Biogenic removal GPC column is 

made up with Biobeads SX-3, sample dump 

140 mL. sample collect 200 mlx DCM/ 

Hexane (1:1) Rot-A-Vap for final clean-up 

on Florisil column. (100 ml of 

DCM/Hexane, 1:1) Rot-A-Vap and made 

up to a final voume of 570 μL.
9

Pressurized Fluid 

Extraction (Dionex, ASE) Dichloromethane

5 min/cycle; 4 

cycles (20 min 

total extraction 

time)

34 mL stainless steel extraction cells; 

temp: 100 °C; pres: 1500 psi; flush 

volume: 60%; Purge time: 100 s

Lipid removal by gel permeation 

chromatography (40 g SX-3 Bio-beads) 

GPC elution profile: 1:1 

dichloromethane/hexane (v:v) collecting the 

fraction eluting between 100 to 220 mL. 

Additional purification by silica/alumina 

packed column chromatography (3% water 

deactivated silica gel/alumina; 2:1). Elution 

profile: 50 mL CDM/hexane (3:7 v:v).

10

Pressurized Fluid 

Extraction (Dionex, ASE) Dichloromethane 15 min

OC- GPC, Florisil, Salicic Acid, PCBH411E column cleanup (sulfuric acid/silica 

gel).

11 Hot Soxhlet

Hexane:Acetone=

3:1 (v/v) 2 hours

Samples were mixed with sodium 

sulphate 

column chromatography on silica/acid silica 

elution with 15 ml hexane and 10 ml 

dichloromethane.

12 Soxhlet

Dichloromethane/

Acetone 18 hours Alumin-b/Silica

13

Dionex ASE200 

Accelerated Solvent 

Extractor Hexane 20 Min

Silica Gel 60 Column cleanup. Two 

fractions eluted by hexane and benzene, 

respectively, were collected

1s Open focused microwave 

5 mL sample + 5 

mL formic acid + 

6 mL 20% 

dichloromethane:h

exane (V:V), 

repeat once

250 W, 10 min 

ramp, 3 min 

hold, 90 o

C, max 

pressure was 

1.72 MPa with 

stirring and 

PowerMax on

Biphasic H2SO4 impregnated silica columns 

eluted with dichloromethane and hexane

2s

As per our method METWTD-ORGRES-MultRes (Sept. 2007)

6M HCl, 2-

propanol, 

MtBE:Hexane(1:1

), 1% KCl, 1M 

KOH (in 1:1 

ethanol:water) 127.5 minutes

1) The sample was placed in a 50mL 

screw top centrifuge tube, mixed with 

by vortexing & then left to stand for 30 

minutes (mins). 2) 1 mL of 6M 

hydrochloric acid was added to the 

sample & then vortexed for 30 seconds 

(secs). 3 mL of 2-propanol was added 

& then the sample was vortexed for 

another 30 secs. 3) 6 mL of 

MtBE:Hexane (1:1) was added, the 

sample vortexed for 1 min, then 

sonicated in an ultrasonic bath for 20 

mins. The sample was vortexed for 30 

secs & then centrifuged at 1000 rpm for 

10 mins. The solvent layer was 

transferred to a 60 mL separatory 

funnel. Step #3 was repeated 2 more 

times.4) 6 mL of 1% KCl was added to 

the separatory funnel and shaken for 1 

min. The aqueous layer was 

drained/discarded and the organic phase 

was collected in a 125 mL round 

bottom flask. The sample was 

concentrated by rotary evaporation to ~ 

1.0 mL & tranferred to a 60 mL 

separatory funnel.5) 6 mL of 1.0 M 

KOH in 1:1 ethanol (95%):water 

(deionized) was added to the 

concentrate & mixed for 1 min.6) The 

aqueous phase was transferred into a 50 

mL centrifuge tube. Step #6 was 

repeated another two times.7) The 

sample was concentrated by rotary 

evaporation down to ~5 mL.

1) Silica Gel (SiOH) solid phase extraction 

(SPE) cartridges were used (500 mg, 6 mL 

capacity). 2) SPE cartridges were 

conditioned with 6 mL of 10% methanol in 

dichloromethane (DCM), followed by 8 mL 

of 5% DCM in hexane. 3) After 

conditioning of the column, the sample was 

loaded onto the cartridge and eluted with 8 

mL 5% DCM:Hexane into a 15 mL tube. 4) 

The sample is concentrated to ~ 1 mL under 

nitrogen, then solvent exchanged to 

trimethylpentane and blown down to 200 

μL.

3s

Accelerated solvent 

extraction (ASE) Dichloromethane ~16 min.

ASE conditions: Pressure = 2000 psi, 

temperature = 100 o

C

Gravity flow column with silica gel and 

neutral alumina, followed by HPLC-SEC to 

elute fraction containing pesticides, PCB 

and PBDE congeners.
4s

Extraction of sample via 

mixing with sodium 

sulfate (200g), grinding 

via mortar and pestle , 

transfer to glass column

325 ml 1:1 

DCM:Hexane 3 hours

Note that after extraction, the extracts 

were split by weight 75:25 (75% for 

PCB, PBDE and PCDD/F analysis 

....25% for pesticide analysis)

PCBS / PBDEs / PCDD/Fs -change solvent 

from 1:1 to Hexane Utilize FMS 

instrumentation and specific programs with 

Acidic Silica Columns ; Acid Base Neutral 

Silica Columns ; Basic Alumina Columns ; 

Carbon Fibre Columns Pesticides-----Add 

extracts to conditioned neutral Florisil (pass 

extracts through three columns).

5s

SPE with Oasis HLB 

cartridges (500 mg, 6 mL)

elution solvent: 

dichloromethane

clean-up on 0.5 g acidified silica, elution 

with 6 mL hexane and 6 ml 

dichloromethane

1fa

Accelerated solvent 

extraction (ASE) Dichloromethane ~16 min.

ASE conditions: Pressure = 2000 psi, 

temperature = 100 degrees C

Details of the sample extraction and 

transesterification procedure for fatty acid 

analyses can be found in Herman et al. 

(2005) Mar. Ecol. Prog. Ser. 32:275-291.

2fa

solvent extraction at room 

temperature hexane 12hours

water removed with anhydrous sodium 

sulfate

3fa

Lipid extracted with 

chloroform/methanol 

(2:1) using Homogenizer 

with Teflon grinding 

pestle. 

Chloroform/metha

nol (2:1) 

Lipids were 

extracted from 

sample 3 times 

for 35 seconds 

with 2 ml 

Chloroform:Met

hanol (2:1)

 FAMEs were extracted twice using 2 

ml Hexane

A portion of wet sample of 30 to 40 mg was 

taken for extraction using an Homogenizer 

with Teflon grinding pestle. The extraction 

was done 3 times using 

Chloroform/Methanol (2:1). The moisture 

was taken out from the extract by anhydrous 

Sodium Sulfate. A portion of the extract was 

taken for percetage lipids by gravimetry and 

the rest was evaporated to dryness with 

nitrogen gas. Before methylation, 1.5 ml 

Toluene was added to the dry sample in a 

screw cap tube. The tube was recaped and 

vortexed for 10 seconds to completely 

dissolve the lipids. Then, 2 ml of methanolsulphuric acid (1%) reagent was added into 

the tube. The tube was flushed with 

nitrogen, recaped and vortexed for 10 

seconds before incubation overnight for 16 

hours at 50°C in the water bath.

After methylation, 2 mL of KHCO3 solution 

(2% w/v) was added to sample, and then, 

Sample tube was recaped and vortexed. The 

upper organic layer (toluene) was then 

transferred to another labeled precalibrated 

tube. And then 2 mL hexane was added 

twice to the original tube; abd the upper 

layer was added to the other tube as before.

The solvents were then evaporated to less 

than 2 mL, and 50 μL of BHT solution 

(0.2mg/mL) was added as a normalization 

standard and as antioxidant. The final 

volume was brought to exactly 2 mL before 

injection.
Summary of Methods Used

Laboratory Instrument Column Phase

Length 

(m)

Column i.d. 

(mm)

Film 

Thickness 

(μm) Points Conc. Range

Analytes Outside of 

Calibration Range

1 Pest. GC-MS DB-XLB 30 0.18 0.18 6 0.01 ng to 800 ng none

PCB GC-MS DB-XLB 30 0.18 0.18 6 0.02 ng to 1500 ng none

PBDE GC-MS DB-XLB 30 0.18 0.18 6 0.001 ng to 330 ng none

2 Pest. GC/MS XLB 60 0.25 0.25 6

PCB GC/MS XLB 60 0.25 0.25 6

PBDE GC/MS 5% phenyl 15 0.25 0.25 6

3 Pest. GC/MS (SIM) DB-5 60 0.25 25 5 to 10 0.001-20 ng/μL

p,p'-DDE; o,p'-DDD, in 

QC00-WB4 only.

PCB GC/MS (SIM) DB-5 60 0.25 25 5 to 9 0.001-10 ng/μL

CBs 87, 95, 99, 149, 151, 

156, 158, 171, 177, 183, 

194, 199, in QC00-WB4 

only.

PBDE GC/MS (SIM) DB-5 60 0.25 25 4 0.0025-1.0 ng/μL n/a

4 Pest. GC-ECD DB-5 60 0.25 0.25 1 100 ng/ml

4,4’-DDE and 4,4’-DDT 

(All Homog IV & All SRM 

1945 analyses)

PCB GC-ECD DB-5 60 0.25 0.25 1 100 ng/ml

PBDE GC-MSD DB-5 60 0.25 0.25 1 109-545 ng/ml

5 Pest. GC-MS DB-5 30 0.25 0.25 5 0.2, 1, 2, 5, 15 ng/μL

PCB GC-MS DB-5 30 0.25 0.25 5 0.2, 1, 2, 5, 9.25 ng/μL

PBDE GC-MS DB-5 30 0.25 0.25 5 0.2, 0.5, 1, 2, 3 ng/μL

6 Pest. GC-ECD DB-5 50 0.20 0.33 7 0.5-100 ng/ml

PCB GC-ECD DB-5 50 0.20 0.33 7 0.5-100 ng/ml

PBDE GC-NICI DB-5 50 0.25 0.25 7 0.1-50 ng/ml

7 Pest. GC-HRMS (EI) DB-5 50 0.25 0.1 1 32-66 pg/μL

PCB GC-HRMS (EI) DB-5 (CP-Sil 19CB) 60(60) 0.25(0.25) 0.1(0.15) 5 0.8-460pg/μL

PBDE GC-HRMS (EI) DB-5 HT 15 0.25 0.1 3 5-500 pg/μL

8 Pest. GC/MSD DB-5 30 0.25 0.25

PCB GC/MSD DB-5 30 0.25 0.25

PBDE GC/MSD DB-5HT 15 0.25 0.10

9 Pest. GC-MS(EI) DB-5 60 0.25 0.25 6 10 ppb- 600 ppb

PCB GC-MS(EI/NCI) DB-XLB 30 0.25 0.25 8 2 ppb- 500 ppb

PBDE GC-MS(EI/NCI) DB-XLB 30 0.25 0.25 9 0.2 ppb- 200 ppb

Pest. GC-ECD CLPesticides 30 0.25 0.25 4 2pg/μL - 200pg/μL Dilute until inside curve

10 PCB GC-ECD XLB 60 0.25 0.25 5 2pg/μL - 100pg/μL Dilute until inside curve

PBDE GC-ECD CLPesticides2 30 0.25 0.20 5 2pg/μL - 200pg/μL Dilute until inside curve

11 Pest. GC/MS (EI) HT-8 25 0.22 0.25 6

PCB GC/MS (EI) HT-8 25 0.22 0.25 8

PBDE GC/MS (ECNI) DB-5 30 0.25 0.25 6

12 Pest. GCMS-EI DB-5 60 0.25 0.25 5 20ng to 800ng

PCB GCMS-EI DB-5 60 0.25 0.25 5 20ng to 800ng

PBDE GCMS-NCI DB-5 60 0.25 0.25 5 20ng to 800ng

13 Pest. GC-ECD DB608/1701 30/15 0.32/0.32 0.5/0.25 6 1 - 1000 ppb

1s Pest. GC/MS (EI+NCI) DB-5ms 30 0.18 0.18

PCB GC/MS (EI) DB-5ms 30 0.18 0.18

PBDE GC/MS (EI) DB-5ms 30 0.18 0.18

2s Pest. GC-MS(EI) DB-5 30 0.25 0.25

PCB GC-MS(EI) DB-5 30 0.25 0.25

PBDE GC-MS(ECNI) DB-5 HT 15 0.25 0.10

3s Pest. GC/MS (SIM) DB-5 60 0.25 25

PCB GC/MS (SIM) DB-5 60 0.25 25

PBDE GC/MS (SIM) DB-5 60 0.25 25

4s Pest. GC-HRMS (EI) DB-5 50 0.25 0.1

PCB GC-HRMS (EI) DB-5 (CP-Sil 19CB) 60(60) 0.25(0.25) 0.1(0.15)

PBDE GC-HRMS (EI) DB-5 HT 15 0.25 0.1

5s Pest. GC/MS (EI) HT-8 25 0.22 0.25

PCB GC/MS (EI) HT-8 25 0.22 0.25

PBDE GC/MS (ECNI) DB-5 30 0.25 0.25

GC/MS (SIM) DB-23 60 0.25 25

1fa

2fa

GC-FID for quantitation; 

GC-MS for identification DB-225 30 0.25 0.25

3fa GC-FID SP-2560 100 0.25 0.2 4

2.45-19.6 ppm to 2.5-60 ppm
Summary of Methods Used

Laboratory

Method of 

Quantitation Added Prior to Extraction 

Indentity of Internal Standards Added Prior to 

Chromatographic Analysis

1 Pest. IS

13C labeled trans-chlordane, trans-nonachlor, oxychlordane, HCB, 4,4’-DDT, 4,4-

DDE, and methyl-triclosan and deuterated 4,4’-DDD

PCB IS 13C 28, 52, 77, 118, 126, 153, 169, 180, 194, and 206

PBDE IS 13C 28, 47, 99, 100, 153, 154, 209

2 Pest. IS 13C 4,4’-DDE, 4,4'-DDT, lindane, and trans -nonachlor 

PCB IS PCB 103 and PCB 198

PBDE IS Fluorinated BDE 47

3 Pest. IS CB103 tetrachloro-o-xylene

PCB IS CB103 tetrachloro-o-xylene

PBDE IS CB103 tetrachloro-o-xylene

4 Pest. IS Ronnel Tetrachloro-m-xylene (TCMX)

PCB IS 4,4' Dibromooctafluorobiphenyl (DOB) & PCB 198 PCB 103 & 3,3',4,4'-Tetrabromobiphenyl (TBB). 

PBDE ES

5 Pest. IS 13C HCB. Cis-chlordane and p,p'-DDE. phenanthrene d10

PCB IS 13C PCB28, 52,118,153,180,194 and 209 phenanthrened10

PBDE IS 13C BDEs 28, 100, and 183 phenanthrene d10

6 Pest. IS PCB53

PCB IS PCB53

PBDE IS PCB200

7 Pest. IS

Persistent Pesticide Spiking Solution (ES 5021 from Cambridge Isotopes) + Tri 

(D3) / Tetra (13C) Chlorobenzene 13C PCB 47

PCB IS

13C 15 ;38 (D5) ; 13C 77 ; 126 ; 169 ; 28 ; 105 ; 118 ; 156 ; 52 ; 101 ; 128 ; 180 ; 

194 ; 208 ; 209 13C PCB 111

PBDE IS

13C 3 ; 13C 15 ; 13C 28 ; 13C 47 ; 13C 99 ; 13C 100 ; 13C 118 ; 13C 153 ; 13C 

183 ; 13C 209 13C BDE 77 ; 13C BDE 126

8 Pest. ES 13C-HCB, 13C-DDE and 13C-DDT

PCB ES 13C-PCB 28, 52,118,153, 180,194

PBDE IS BDE-30 and BDE-71

9 Pest. ES PCB 30; PCB 205

PCB ES PCB 30; PCB 205

PBDE ES BDE 71; BDE 172

10 Pest. ES

PCB ES

PBDE ES

11 Pest. IS PCB 143 and e-HCH

PCB IS PCB 143

PBDE IS BDE 77 and BDE 128

12 Pest. IS TCMX, PCB030, PCB112, PCB198 2,2'-5,5'-Tetrabromobiphenyl

PCB IS TCMX, PCB030, PCB112, PCB198 2,2'-5,5'-Tetrabromobiphenyl

PBDE IS 2,2'-5,5'-Tetrabromobiphenyl

13 Pest. ES

PCB NA

PBDE NA

1s Pest. IS

13C labeled HCB, oxychlordane, 4,4'-DDE, 4,4'-DDD, trans-chlordane, transnonachlor, 4,4'-DDT

PCB IS 13C labeled PCB 28, 52, 118, 153, 180, 194, 206

PBDE IS 13C labeled BDE 28, 47, 153, 99, 100, 154, 209

2s Pest. ES Surrogates: 13C-1,2,4,5-hexachlorobenzene

PCB ES Surrogates: 13C-PCB-28, PCB-52, PCB-118, PCB-153, PCB-180 and PCB-192

PBDE IS BDE-30 (IS and surrogate)

3s Pest. IS CB103 tetrachloro-o-xylene

PCB IS CB103 tetrachloro-o-xylene

PBDE IS CB103 tetrachloro-o-xylene

4s Pest. IS

Persistent Pesticide Spiking Solution (ES 5021 from Cambridge Isotopes) + Tri 

(D3) / Tetra (13C) Chlorobenzene 13C PCB 47

PCB IS

13C 15 ; 38 (D5) ; 13C 77 ; 126 ; 169 ; 28 ; 105 ; 118 ; 156 ; 52 ; 101 ; 128 ; 180 ; 

194 ; 208 ; 209 13C PCB 111

PBDE IS

13C 3 ; 13C 15 ; 13C 28 ; 13C 47 ; 13C 99 ; 13C 100 ; 13C 118 ; 13C 153 ; 13C 

183 ; 13C 209 13C BDE 77 ; 13C BDE 126

5s Pest. IS PCB 143 and e-HCH

PCB IS PCB 143

PBDE IS BDE 77 and BDE 128

1fa Fatty Acids IS C11:1 (as triglyceride) C13:0 (as methyl ester)

2fa Fatty Acids ES

3fa Fatty Acids IS Cholestane BHT
Summary of Methods Used

Laboratory

Any Other Internal 

Standards? Added When?

IS Surrogate Standards Used 

for Quantitation Were Added:

If the 

IS/surrogates 

Added After 

Extraction/Cleanu

p, Were Results 

Corrected for 

Recovery?

1 Prior to extraction

2 Prior to extraction

3 Pest. tetrachloro-m-xylene

Just before taking aliquot 

for lipid analysis, prior to 

HPLC-SEC separation. Prior to extraction

PCB tetrachloro-m-xylene

PBDE tetrachloro-m-xylene

4 Pest.

1,2,3-Trichlorobenzene 

(123-TCB) after extraction No

PCB PCB 192

PBDE

5 Prior to extraction

6

Not thosue added prior to 

extraction

7 Prior to extraction

8 Pest.

13C-HCB, 13C-DDE and 

13C-DDT

After extraction and before 

GPC clean-up

PCB

13C-PCB 28, 52,118,153, 

180,194

PBDE BDE-30 and BDE-71

11 Prior to extraction

12

Added after extraction/cleanup 

and prior to chromatographic 

analysis

1s Prior to extraction

2s Prior to extraction

3s Pest. tetrachloro-m-xylene

Just before taking aliquot 

for lipid analysis, prior to 

HPLC-SEC separation. Prior to extraction

PCB tetrachloro-m-xylene

PBDE tetrachloro-m-xylene

4s Prior to extraction

5s Prior to extraction

1fa fatty acids

C13:1 (as acid), added just 

before derivatization.

those added after 

extraction/cleanup and just prior 

to chromatographic analysis 

(C13:1, added as acid

3fa fatty acids Yes
Summary of Methods Used

Laboratory Recovery Range (% )

Were PCBs Separated 

From Pesticides Prior 

to GC?

Does PCB 132 coelute with PCB 

153 or with PCB 105 or is it 

separated from both?

1 No Separates

2 No Separates

3 Pest. 106-116 No Coelutes with PCB 153

PCB 106-116

PBDE 106-116

4 Pest.

Ronnel: SRM1945 (160 

± 53%); 123-TCB: 

SRM1945 (97 ± 8%) No Coelutes with PCB 153

PCB

DOB: SRM1945 (94 ± 

5%); PCB 198: 

SRM1945 (79 ± 9%)

PBDE

PCB 192: SRM1945 ( 57 ± 

2%); See note 2 for the 

recoveries for Homogenate IV 

at the end of this report.

5 No Coelutes with PCB 153

6 Yes

7 Pest. 40-120 No Separates

PCB 45-115

PBDE 45-110

8 No Separates

9 No

To our knowledge, PCB 

132 does not coelute with 

either 105 and 153 using 

our method (GC-NCI-MS 

using DB-XLB)

10 Yes

PCB 132 was a shoulder of 

PCB 153 

11 Pest. 75-90% No Separates

PCB 75-90%

PBDE 75-90%

12 No Separates

1s No Coelutes with PCB 153

2s Pest.

80 - 93 % (two samples had 

recoveries of 15% & 118%) No Separates

PCB

49 - 86 % (one sample had 

recoveries of <13 %)

PBDE

66 - 103 % (one sample had a 

recovery of 14 %)

3s Pest. 93-102 No Coelutes with PCB 153

PCB 93-102

PBDE 93-102

4s Pest. 50-120 No Separates

PCB 45-110

PBDE 45-120

5s Pest. 80-95% No Separates

PCB 80-95%

PBDE 80-95%

1fa Fatty Acid 101-111

3fa Fatty Acid 93% to 99%
Appendix F

Additional analyte data and notes reported by individual laboratories.
Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

1 PCB 74 15.7 14.8 15.6 97.8 97.5 98.0

PCB 70 10.5 9.9 9.9 2.84 2.66 2.81

PCB 56 5.7 5.5 5.8 7.8 7.6 7.5

PCB 92+84+89 25.9 26.5 24.9 374 379 381

PCB 79 <LOD <LOD <LOD <LOD <LOD <LOD

PCB 119 4.72 4.40 4.33 69.1 71.0 71.3

PCB 112 <LOD <LOD <LOD <LOD <LOD <LOD

PCB 154 3.80 4.03 3.86 140 144 145

PCB 82 3.65 3.76 3.33 63.7 65.1 65.2

PCB 106 3.84 3.79 3.43 6.89 7.31 6.34

PCB 114 <LOD <LOD <LOD 58.1 59.2 55.7

PCB 146 41.6 42.7 41.5 1117 1135 1147

PCB 137 6.34 6.36 6.30 140 145 143

PCB 176 5.97 5.57 5.16 112 114 115

PCB 130 10.3 10.4 10.0 230 238 236

PCB 163 41.5 40.4 38.7 1017 1043 1058

PCB 158 10.0 9.78 8.89 191 201 199

PCB 178 21.0 22.4 21.3 478 487 488

PCB 166 6.1 5.24 5.56 33.5 34.1 35.3

PCB 167 13.6 12.7 13.4 190 192 193

PCB 185 3.43 3.52 3.33 68.4 68.3 70.8

PCB 174 25.2 25.3 25.1 737 752 749

PCB 177 29.4 29.4 29.2 768 780 782

PCB 202 27.1 32.1 28.0 125 125 126

PCB 157 2.91 2.71 2.82 47.8 49.1 50.5

PCB 172 12.9 12.7 11.9 248 252 256

PCB 197 5.15 5.22 4.50 26.0 27.2 27.6

PCB 193 7.73 7.43 6.90 177.2 182.4 181.0

PCB 191 2.07 1.89 2.05 30.1 32.9 34.4

PCB 200 4.05 4.04 4.12 23.8 24.3 24.8

PCB 199 88.9 91.1 88.3 540 546 545

PCB 196+203 81.6 81.0 80.9 413 418 418

PCB 189 4.16 4.31 4.01 30.4 31.3 31.7

PCB 208 25.2 26.0 25.2 19.9 19.7 18.9

PCB 207 16.2 16.6 15.8 16.0 15.7 15.5

PCB 205 2.2 2.1 2.4 9.6 10.2 10.4

pentachlorobenzene 1.74 1.95 1.84 8.49 9.24 9.99

BDE 28 2.61 2.51 2.65 2.66 2.98 3.12

BDE 155 4.69 4.86 4.36 8.91 9.43 9.52

2 PCB 138 4544 4449 4521 149 151 149

PCB 163 1005 1045 1034 43.3 44.5 40.7

3 Nonachlor III 75.1 75.4 77.3 25.3 25.7 25.7

CB17 4.21 4.33 4.22 1.14 1.32 1.19

CB70 2.53 2.55 2.53 10.3 10.3 10.5

CB74 108 109 110 15.6 15.8 15.8

CB82 11.5 12.0 12.0 4.37 4.28 4.34

CB110 41.9 42.5 42.8 35.9 36.0 36.3

CB158 265 266 270 11.5 11.5 11.5

CB171 265 267 267 12.0 11.9 12.1

CB177 815 818 823 31.3 32.0 32.2

CB191 48.9 49.4 49.6 1.61 1.71 1.61

CB199 442 443 442 83.4 85.0 85.5

CB205 12.8 13.3 13.0 1.95 2.05 1.81

CB208 17.2 17.3 17.4 25.5 26.7 26.9

BDE28 6.61 6.60 6.55 2.25 2.29 2.05

BDE49 1.88 1.85 1.93 2.91 2.80 2.94

BDE66 2.8 2.8 3.07 <1.82 1.69 1.65

BDE183 <1.22 <1.43 <1.22 2.08 1.83 1.85

Penta-BDE (IUPAC # unknown) 4.44 4.42 4.42 <1.82 <1.65 <1.59
4 Notes for the PCB and Pesticide Analysis:

1. We prepared each sample by weighing out a portion of 

each sample to a mortar and and adding diatomaceous earth 

(Hydromatrix) to remove water from the sample. After 

mixing each sample, this mixture was transferred to the 

extraction cell and internal standards were added. We used 

these conditions in the ASE method for the first extraction of 

each sample: Pressure: 1500-psi; 5-min heating cycle at 

100oC; 10-min static cycle at 100oC using 100% (v) 

methylene chloride; Flush Volume: 60%; Purge Time: 60-sec

For the method used for the last two extractions, the static 

heating time was reduced to 5-min.; all other parameters were 

the same. For each sample, the three extractions were run in 

a schedule in which there was no methylene chloride rinses 

during the first and second extractions; there was a rinse cycle 

after the third extraction. After the extraction, we added 

anhydrous sodium sulfate to remove water from the extracts in 

each collection bottles. Finally, the three extracts for each 

sample were combined together and concentrated to 10-ml for 

the lipid determination and sample cleanup.

2. The internal instandard recoveries for the Homogenate 

IV samples were very high due to the interference of coeluting 

peaks in the chromatograms.

3. To prepare the calibration solutions for this 

intercomparison exercise, we used these solutions: SRM 2261 

and SRM 2274 from NIST as the sources for. the chlorinated 

pesticides. From Accustandard, Inc, New Haven, CT., we 

purchased the 20 PCB mixture C-CCSEC and the individual 

PCBs: 87, 132, and 201. We also purchased the 

supplementary PCB solution SRM 2275 from NIST. 

4. We used hydrogen gas as the carrier gas at a linear 

velocity of 40 cm/min for the GC-ECD analysis of the 

pesticides and PCBs. We report the concentrations for the 

optional pesticides and PCBs in Table 1. 

5. Using our gas chromatographic conditions, PCB 153 and

PCB 132 elute very closely to each other when a calibration 

solution is run. In the samples, the peak in this region of the 

chromatogram is very broad making identification and 

quantification of PCB 132 very difficult. PCB 105 is 

separated from both PCB 153 and PCB 132. Conservatively, 

the concentration of PCB 153 given in the table should be 

treated as the sum of PCB 153 and PCB 132.

6. We would like to acknowlege the work done by Tom 

Cleary and John McCarthy during the preparation and cleanup

of these samples.

7. In GC-ECD analysis, a peak in the vicinity of retention 

time of lindane was detected. This peak was not confirmed as 

lindane in the GC-MS analysis.

The Meaning of Other found in the Tables for the 

Pesticide and PCB Concentrations: We found the 

following pairs of analytes coelute from our DB-5 column:

Other

A : 4,4’-DDD and cis-Nonachlor

Other

B : PCB 8 and alpha-HCH 

Other

C : PCB 87 and dieldrin

Other

D : PCB 169 and Mirex

Other

E : PCB 101 and Endosulfan I

OtherF : PCBs 132 and 153 elute closely to each other. 

Conservatively, the concentration of PCB 153 given in the 

table should be treated as the sum of 

 PCB 153 and PCB 132.

Table 1: Optional Pesticide and PCB Results

Additional Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Pesticides and PCBs Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

Heptachlor DL DL DL 0.53 1.26 DL

Endrin DL DL DL DL DL DL

Endosulfan I OtherE OtherE OtherE OtherE OtherE OtherE

Endosulfan II 296.4 222.9 219.7 13.3 13.4 13.6

Endosulfan Sulfate 573.7 553.7 538.3 7.78 8.29 9.13

BZ 8 OtherB OtherB OtherB OtherB OtherB OtherB

BZ 77 OtherG OtherG OtherG OtherG OtherG OtherG

BZ 110 OtherG OtherG OtherG OtherG OtherG OtherG

BZ 126 507.2 508.9 476.9 1.95 2.26 2.16

BZ 169 OtherD OtherD OtherD OtherD OtherD OtherD

Other: We found the following pairs of analytes coelute 

from our DB-5 column:
4 Other

B : PCB 8 and alpha-HCH 

Other

D : PCB 169 and Mirex

Other

E : PCB 101 and Endosulfan I

OtherG : Since PCB 77and PCB 110 coelute from our column 

and the response of each congener vary from each other, the 

relative ratios of two congeners can not be determined. We 

do not report the concentrations of either PCB 77 or PCB 110.

Notes for the PBDE Analysis:

1. SRM1945 extract was concentrated to 1 ml. This 

extract was used for both PCB/pesticide and PBDE analyses.

2. Unknown sample extract for PCB and pesticide analyses 

was also used for PBDE analyses.

3. To prepare the PBDEcalibration solutions for this 

intercomparison exercise, we purchased the standard solution, 

BDE-MXE, a mixture of 27 polybrominated diphenyl ethers 

(PBDE), from TerraChem, Shawnee Mission, KS; the US 

distributor for Wellington Laboratories, Guelph, Ontario 

Canada.

4. The PBDE analyses were conducted using a 60 m 

column, higher flow rate, and accelerated oven temperature 

program to minimize the degradation of higher brominated 

congeners. analyses were conducted using a short column, 

higher flow rate, and accelerated oven temperature program to 

minimize the degradation of higher brominated congeners. 

Target PBDE congeners were base-line separated using these 

chromatographic conditions. Two microliters of sample wer

injected into the GC-MS for PBDE analyses. 

5 28/31 coelute 26.0 34.1 37.3 25.5 24.1 25.5

95/88 coelute 489 509 457 31.0 32.1 30.6

87/115 coelute 341 336 292 50.0 54.3 51.8

101/89/90/ coelute 1742 1842 1610 110 116 111

118/106/123 coelute 3700 3904 3457 262 286 269

128/167 coelute 899 933 850 76.86 83.57 83.75

132/153/165 coelute 11183 11737 10812 305 319 306

138/163/158/164 coelute 8075 8249 8094 267 279 262

180/193 coelute 3646 3827 3709 128 117 116

45 8.63 9.40 9.53 7.24 7.17 7.31

48 104 110 94.2 20.9 21.1 21.6

74/61 296 307 287 51.4 39.0 46.0

56/60 41.9 45.9 44.9 28.0 28.1 29.6

92 232 249 220 19.9 20.2 19.8

84 56.3 36.8 48.6 16.4 15.5 14.0

119 43.8 48.4 43.6 12.0 12.4 12.6

110 34.4 37.1 34.0 33.0 33.7 32.9

114 37.0 30.4 38.2 17.2 17.9 17.9

146 1067 1136 1039 53.6 53.3 52.1

141 159 171 152 27.0 27.7 27.1

159 70.8 77.8 69.0 7.36 7.27 9.23

157 49.2 42.3 42.4 0.820 2.54 1.89

184 15.0 16.1 14.8 <2.15 <2.15 <2.15

174 625 723 694 17.7 14.4 14.4

177 612 689 652 15.7 14.0 13.8

172 170 183 175 12.8 13.1 13.1

189 35.5 38.2 36.5 9.8 9.8 9.8

202 98.9 98.5 98.0 21.0 20.1 20.9

200 57.0 58.4 59.1 12.5 12.8 13.0

207 9.10 9.7 9.22 10.8 10.5 10.6

6 BRIEF DESCRIPTION OF PROCEDURES USED:

Mass of sample extracted: Homogenate IV 2.97+2.93+2.95 g, WET basis SRM 1945 4.09+4.00+4.03 g, WET basis

Method used for determining percentage lipid:

Total extractable 

lipids (gravimetric 

from Soxhlet 

extract)

Were "wet" or "dry" samples extracted? Homogen. IV Wet SRM 1945 Wet

Extraction method Soxhlet

Extraction solvent:

Hexane:acetone 

[1:1]

Sample extract cleanup method:

Gel Permeation 

Chromatography 

followed by sulfuric 

acid clean-up

Analytical method used (e.g., GC-MS (include ionization 

type), GC-ECD):

Analyt. Instr. Column Phase Col. Length, m Col. i.d., mm

Col. film thickness, 

μm

HBCD diastereoisomers LC-MS C18 0.1 2.0 n/a
6

Method of quantitation (IS = internal standard, ES = external 

standard):

HBCD diastereoisomers IS

IF internal standard method was used, please complete the 

following section:

Identity of internal standards/surrogates used that were added 

PRIOR to extraction of sample:

HBCD diastereoisomers

 Added after extraction/cleanup and JUST PRIOR to 

chromatographic analysis:

HBCD diastereoisomers

 Any others? Added at what point in analyses:

Added prior to 

clean-up

HBCD diastereoisomers

d18 -HBCD, d18 

-HBCD and d18-

HBCD

 IS/surrogate standards used for quantitation calculations 

were: 

those added prior to 

extraction

Not

those added after 

extraction/cleanup 

and just prior to 

chromatographic 

analysis

 were results corrected for percent recovery? No

HBCD 

diastereoisomers

Points Conc. Range

curve calibration 

range

HBCD diastereoisomers 6 10-500 ng/ml

Please note any differences in procedures used for SRM 1945 

analyses from those used for Whale Blubber Homogenate V 

described above:

RESULTS:

PERCENT LIPID (List each result if determined more than 

once. Enter results as a number, for example 90.0. DO NOT 

change format of cell to percent.)

Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

(percent) (percent) (percent) (percent) (percent) (percent)

Lipid 67.9 68 68 72 73 73

Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

HBCD Analysis A Analysis B Analysis C Analysis A Analysis B Analysis C

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

-HBCD 35.6 38 39 8 7 8

-HBCD <4.0 <4.0 <5.0 <4.0 <4.0 <5.0

-HBCD <4.0 <4.0 <5.0 <4.0 <4.0 <5.0

total HBCD 35.6 38 39 8 7 8

7

Analytical method used (e.g., GC-MS (include ionization 

type), GC-ECD):

Analyt. Instr. Column Phase Col. Length, m Col. i.d., mm

Col. film thickness, 

μm

 PCDD/F Congeners GC-HRMS (EI) DB-5 60 0.25 0.1

Points Conc. Range

 PCDD/F Congeners 5 0.25-500 pg/ul

curve calibration 

range

PCB CONGENER ANALYSES Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

Congener

43/49 84.4 88.5 83.5 15.2 15.2 15.9

101 1240 1260 1310 81.7 82.6 87.1
7 77 <0.474 <0.269 <1.63 0.284 0.357 0.352

126 <0.594 <0.250 <1.27 0.0559 <0.0826 0.0435

169 1.69 1.72 1.67 0.134 0.135 0.117

2378 PCDD/F CONGENER ANALYSES Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

Congener

(pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt)

2378/2348/2347/2346/1246/1249-TeCDF <1.70 <4.31 <3.31 4.46 <1.94 4.81

12378-PeCDF <1.37 <2.63 <2.40 <0.890 <1.07 <1.49

23478/12489/13489/12369-PeCDF <1.37 <2.63 <2.40 <0.890 <1.07 <1.49

123478-HxCDF <1.21 <1.64 <1.04 1.41 1.41 <0.935

123678-HxCDF <1.21 <1.64 <1.04 <1.08 <1.24 <0.935

123689/234678-HxCDF <1.21 <1.64 <1.04 <1.08 <1.24 <0.935

123789-HxCDF <1.21 <1.64 <1.04 <1.08 <1.24 <0.935

1234678-HpCDF <0.737 <3.14 <1.01 1.36 <0.751 <2.06

1234789-HpCDF <0.737 <3.14 <1.01 <1.12 <0.751 <2.06

OCDF <1.13 <5.31 <1.54 <1.61 <1.73 <0.838

2378-TeCDD <1.01 <1.82 <2.04 <1.12 <0.865 <1.40

12378-PeCDD <1.29 <2.95 <2.09 <1.16 <1.36 <1.58

123478-HxCDD <1.73 <2.68 <1.46 <1.39 <1.24 <1.12

123678-HxCDD <1.73 <2.68 <1.46 <1.39 <1.24 <1.12

123789-HxCDD <1.73 <2.68 <1.46 <1.39 <1.24 <1.12

1234678-HpCDD <1.86 <3.27 <1.86 <1.70 <1.15 2.06

OCDD 2.20 <2.23 2.60 5.58 3.66 5.75

The blubber samples were extracted in 2 batches: the first for 

PCBS, PCDD/Fs, PBDEs ....then a second set of blubber 

samples were extracted for pesticides

9 PESTICIDE ANALYSES

Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Pesticide Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

Heptachlor <10.0 <10.0 <10.0 <10.0 <10.0 <10.0

Chlordene <10.0 <10.0 <10.0 <10.0 <10.0 <10.0

Aldrin <10.0 <10.0 <10.0 <10.0 <10.0 <10.0

Endrin <10.0 <10.0 <10.0 <10.0 <10.0 <10.0

PCB CONGENER ANALYSES Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Congener Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

37 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0

70 <10.0 <10.0 <10.0 11.9 15.3 11.6 

74 139 133 124 14.6 19.9 17.1

77 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0

81 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0

110 58.8 64.9 67.7 27.3 29.1 29.0 

114 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0

119 69.6 79.3 75.1 3.19 3.59 2.76 

123 14.4 19.7 14.3 4.99 6.29 5.06 

126 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0

157 104 112 111 2.74 2.86 2.52 

158 424 496 471 8.75 8.72 8.24 

167 315 370 324 6.76 7.84 6.65 

169 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0

177 1290 1540 1350 25.5 28.4 24.1 

189 129 158 136 7.7 7.6 7.7 

199 870 1060 905 81.4 100 82.6 

PBDE CONGENER ANALYSES Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Congener Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

15 <0.1 <0.1 <0.1 <0.1 <0.1 0.16 

28 4.29 3.79 3.84 1.52 1.27 1.62 

33 3.27 2.93 3.48 12.0 11.8 11.6 

49 <=0.026 <0.1 <0.1 1.89 1.63 2.73 

66 0.71 2.49 1.80 2.76 1.63 1.04 

75 1.50 0.99 0.51 0.41 0.30 0.20 

119 <0.1 <0.1 <0.1 <0.1 <0.1 0.14 

155 <0.1 <0.1 <0.1 4.89 4.22 3.75 

183 <0.1 <0.1 <0.1 5.00 1.68 2.34 

<= detected at concentration less than reported MDL

TOXAPHENE ANALYSES Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Congener Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

26 400 498 346 72.9 74.4 66.3 

32 7.94 9.61 6.99 <5.00 <5.00 <5.00

50 1020 1240 889 159 162 146 

62 214 275 193 46.6 48.1 44.6 

11 PCB 74 117 112 117 17.2 16.6 16.7

PCB 110 34.3 35.4 34.5 31.1 31.1 30.5

PCB 138 4070 4241 4100 123 126 123

PCB 170 1193 1239 1225 34.2 35.2 33.7

PCB 174 779 814 807 23 23.3 22.9
11 PCB 177 717 748 732 24.3 25.3 24.9

BDE 28 25.6 26.3 25.4 8 8 8

BDE 66 3.1 2.4 1.9 1.6 1.5 2

BDE 155 < 0.5 < 0.5 < 0.5 2.6 2.6 2.5

BDE 183 < 0.5 < 0.5 < 0.5 1.1 1 1

2-MeO-BDE 68 22.6 24.1 30.2 68 74.5 77.4

6-MeO-BDE 47 269 273 278 64.1 66.6 65

12 PBDE CONGENER ANALYSES Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Congener Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt) (ng/g wet wt)

12/13 15.2 13.8 9 5.32 4.69 5.23

25/17 25.2 18.8 28.4 <1 <1 <1

33/28 5.7 7.8 6.6 2.6 2.7 2

66 <1 <1 <1 2.9 6.6 3.7

77 12.9 9.3 10.1 11 17 18.6

119 <1 <1 <1 3.1 3.8 3.4

118 118 119 137 <1 <1 <1

138 230 222 182 <1 <1 <1

 1s ADDITIONAL ANALYTICAL RESULTS MMCM-1 MMCM-1 MMCM-1 SRM 1958 SRM 1958 SRM 1958

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt)

BDE_17 1800 1633 1687 519 513 518

BDE_28 <200 <200 <200 444 435 443

BDE_66 147 150 159 352 367 352

BDE_85 <200 <200 <200 470 409 423

BDE_155 198 199 199 <200 <200 <200

BDE_183 <200 <200 <200 300 248 269

PCB_44 114 98.3 98.2 382 386 381

PCB_74 353 332 322 364 351 364

PCB_146 1625 1616 1616 336 327 336

PCB_163 2150 2163 2175 <25 <25 <25

PCB_158 517 538 534 503 452 502

PCB_178 565 541 547 316 312 315

PCB_167 71.4 68.7 68.7 322 315 322

PCB_174 670 646 668 292 283 291

PCB_177 948 914 945 413 400 412

PCB_202 405 393 407 <25 <25 <25

PCB_157 49.7 50.4 49.7 307 299 306

PCB_172 370 369 381 304 297 303

PCB_199 1294 1268 1239 337 324 336

PCB_196 1325 1287 1270 621 617 620

 3s MMCM-1 MMCM-1 MMCM-1 SRM 1958 SRM 1958 SRM 1958

Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt)

Nonachlor III 659 645 574 <368 <408 <469

CB110 1050 1140 1020 492 489 <470

CB199 1270 1220 1170 <278 <308 <354

Total Lipid (%) (Gravimetric) n/a 0.239 0.256 0.239 0.214 0.195

Iatroscan (TLC/FID) Lipid results:

Total Lipid (%) 0.160 0.140 0.140 0.110 0.130 0.160

Wax and sterol esters (% of total lipid) 76.2 76.7 75.3 65.7 66.7 67.0

Triglycerides (% of total lipid) 2.20 1.80 2.20 16.8 17.3 17.3

Free Fatty Acids (% of total lipid) 2.90 2.30 3.30 3.00 2.60 2.00

Cholesterol (% of total lipid) 16.9 17.0 16.1 13.8 13.5 13.1

Phospholipid (% of total lipid) 1.80 2.20 2.90 0.700 0.000 0.700

Please also note that we resolve PCB170 and PCB190, but do 

not quantitate PCB190. We also believe that PCB187 colutes 

with other congeners (159 and 182?). We also analyzed for 

the following compounds, which were not detected at levels 

above the lower limit of quantitation: aldrin, endosulfan I, 

heptachlor, CB17, CB33, CB70, CB74, CB82, CB158, 

CB171, CB177, CB191, CB205, CB208, BDE28, BDE49, 

BDE66, BDE85, BDE183, and several other BDE congeners 

whose IUPAC numbers are unknown. PCB and PBDE 

congeners are designated using the IUPAC numbering system.

 4s

Analytical method used (e.g., GC-MS (include ionization 

type), GC-ECD):

Analyt. Instr. Column Phase Col. Length, m Col. i.d., mm

Col. film thickness, 

μm

 PCDD/F Congeners GC-HRMS (EI) DB-5 60 0.25 0.1

Calibration Curve

Points Conc. Range

curve calibration 

range

 PCDD/F Congeners 5 0.25-500 pg/ul
 4s PCB CONGENER ANALYSES MMCM-1 MMCM-1 MMCM-1

Sample 1 Sample 2 Sample 3

Congener (pg/g wet wt) (pg/g wet wt) (pg/g wet wt)

43/49 50.9 68.4 65.7

101 350.0 547.0 469.0

77 <0.541 <0.532 <0.597

126 <6.33 <1.07 <1.04

169 0.830 0.670 0.660

2378 PCDD/F CONGENER ANALYSES MMCM-1 MMCM-1 MMCM-1

Sample 1 Sample 2 Sample 3

Congener

(pg/g wet wt) (pg/g wet wt) (pg/g wet wt)

2378/2348/2347/2346/1246/1249‐TeCDF <1.70 <4.31 <3.31

12378‐PeCDF <1.37 <2.63 <2.40

23478/12489/13489/12369‐PeCDF <1.37 <2.63 <2.40

123478‐HxCDF <1.21 <1.64 <1.04

123678‐HxCDF <1.21 <1.64 <1.04

123689/234678‐HxCDF <1.21 <1.64 <1.04

123789‐HxCDF <1.21 <1.64 <1.04

1234678‐HpCDF <0.737 <3.14 <1.01

1234789‐HpCDF <0.737 <3.14 <1.01

OCDF <1.13 <5.31 <1.54

2378‐TeCDD <1.01 <1.82 <2.04

12378‐PeCDD <1.29 <2.95 <2.09

123478‐HxCDD <1.73 <2.68 <1.46

123678‐HxCDD <1.73 <2.68 <1.46

123789‐HxCDD <1.73 <2.68 <1.46

1234678‐HpCDD <1.86 <3.27 <1.86

OCDD 2.20 <2.23 2.60

Note that the serum was spiked, extracted and split (75:25) 

before further workup.

 5s MMCM-1 MMCM-1 MMCM-1 SRM 1958 SRM 1958 SRM 1958

Congener Sample 1 Sample 2 Sample 3 Sample 1 Sample 2 Sample 3

(pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt) (pg/g wet wt)

PCB 74 410 460 440 520 470 490

PCB 110 990 1000 1030 400 440 400

PCB 138 7630 7880 7720 440 470 433

PCB 174 460 460 440 < 30 < 30 < 30

PCB 177 900 920 900 380 380 380

BDE 28 120 125 115 430 420 400

BDE 49 < 10 < 10 < 10 445 445 425

BDE 66 95 85 90 445 455 440

BDE 85 < 10 < 10 < 10 445 465 485

BDE 154 + BB 153 835 850 860 750 740 750

BDE 155 145 146 150 < 10 < 10 < 10

BDE 183 20 20 20 245 235 270

Lipids (g/L) MMCM-1 SRM 1958

Total cholesterol 1.61 - - 1.1 - -

Triglycerides < 0.10 - - 0.87 - -

 1fa Homog VIII Homog VIII Homog VIII SRM 1945 SRM 1945 SRM 1945

Analysis A Analysis B Analysis C Analysis A Analysis B Analysis C

(mass percent) (mass percent) (mass percent) (mass percent) (mass percent) (mass percent)

C10:0 0.0267 0.0256 0.0249 0.0278 0.0280 0.0277 Capric acid

C11:0 0.00461 0.00411 0.00443 0.00459 0.00473 0.00464

C12:1 0.00716 0.00735 0.00722 <0.00463 0.00487 <0.00422

4,8,12-trimethyl C13:0* 0.00701 0.00694 0.00675 0.0185 0.0193 0.0188

iso-C14:0 0.0920 0.0885 0.0882 0.0467 0.0470 0.0457

11-methyl C14:0* 0.00364 0.00347 0.00345 0.00412 0.00416 0.00381

C14:1n5 0.423 0.412 0.405 0.461 0.464 0.452

C14:1n7* 0.0946 0.0918 0.0930 0.121 0.124 0.120

C14:1n9* 0.0683 0.0663 0.0670 0.0896 0.0912 0.0893

iso-C15:0 0.253 0.246 0.245 0.212 0.218 0.210

anteiso-C15:0* 0.0473 0.0459 0.0448 0.0605 0.0613 0.0590

2,6,10,14-tetramethyl C15:0* 0.0172 0.0164 0.0169 0.0466 0.0474 0.0443

C15:1n5 <0.00195 <0.00183 <0.00163 0.00291 0.00287 0.00261

iso-C16:0 0.241 0.235 0.237 0.0796 0.0814 0.0776

anteiso-C16:0* 0.00442 0.00467 0.00446 0.00383 0.00405 0.00392

C16:1n5* 0.152 0.148 0.148 0.182 0.183 0.177

C16:1n9* 2.55 2.49 2.48 2.01 2.04 1.96

C16:1n11* 0.213 0.211 0.213 0.150 0.161 0.145

7-methyl C16:1 0.0669 0.0639 0.0669 0.0481 0.0469 0.0438

C16:2n4* 0.0929 0.0906 0.0986 0.135 0.138 0.133

C16:2n6* 0.0192 0.0185 0.0188 0.0175 0.0176 0.0152

C16:3n4* 0.0133 0.0122 0.0112 0.0196 0.0191 0.0190

C16:3n6* <0.00602 <0.00565 <0.00605 <0.00715 <0.00652 <0.00653

C16:4n1* 0.0139 0.0132 0.0134 0.0180 0.0187 0.0188

C16:4n3* 0.102 0.0990 0.0987 0.137 0.143 0.137

iso-C17:0 0.178 0.173 0.173 0.128 0.131 0.123

anteiso-C17:0* 0.0660 0.0629 0.0637 0.0561 0.0580 0.0538

C17:1n7 0.00417 0.00420 0.00405 0.00554 0.00554 0.00508

C17:1(unk)* 0.478 0.461 0.464 0.350 0.360 0.341

iso-C18:0 0.0352 0.0289 0.0291 0.0179 0.0192 0.0209

anteiso-C18:0* 0.00595 0.00566 0.00603 0.00313 0.00321 0.00264

C18:1n5* 0.190 0.185 0.180 0.246 0.249 0.233

C18:1n7* 1.74 1.70 1.69 1.91 1.94 1.83 Vaccenic acid

C18:1n11* 0.834 0.799 0.784 2.54 2.57 2.45

C18:1n13* 0.0616 0.0546 0.0571 0.0397 0.0395 0.0354
1fa C18:2n4* 0.0504 0.0487 0.0502 0.0432 0.0442 0.0400

C18:2n7* 0.0231 0.0259 0.0244 0.0195 0.0224 0.0211

C18:3n1* <0.00779 <0.00732 <0.00651 <0.00926 <0.00844 <0.00845

C18:3n4* 0.0242 0.0217 0.0259 0.0220 0.0205 0.0202

C18:4n1* <0.0111 0.0134 0.0143 <0.0132 <0.0120 <0.0120

C19:0 0.0438 0.0426 0.0439 0.0354 0.0367 0.0330

C20:1n5* 0.0265 0.0260 0.0274 0.0384 0.0409 0.0360

C20:1n15 0.0106 0.00965 0.0101 0.0131 0.0145 0.0118

C20:2n9* 0.00638 0.00662 0.00704 0.00470 0.00503 0.00543

C20:2n11* 0.132 0.126 0.139 0.155 0.153 0.123

C20:3n6 0.0434 0.0425 0.0429 0.0316 0.0353 0.0285

C20:4n3* 0.206 0.198 0.202 0.174 0.174 0.164

C22:0 0.0183 0.0185 0.0187 0.0212 0.0215 0.0185 Behenic acid

Compounds marked with an asterisk (*) are not present in our 

standards, and are tentatively identified based on retention 

times and quantitated using the point-to-point calibration of a 

similar compound. The other compounds are in our standards 

and are positively identified and quantitated using a point-topoint calibration. All the additional compounds are cisconfiguration fatty acids; no trans isomers were quantitated.

 3fa C10:0 267681 282162 259715 272212 264100 230992 capric acid

C11:0 ND ND ND ND ND ND undecanoic acid

C13:0 262609 269207 279531 297273 306593 299177 tridecanoic acid

C14:1(n-5) 3640557 3802969 3712663 3988092 4122656 4045462 myristoleic acid

C15:1 ND ND ND ND ND ND cis-10-pentadecanoic acid

C17:1 ND ND ND ND ND ND cis-10-heptadecanoic acid

C18:2(n-6)t ND ND ND ND ND ND linolelaidic acid

C21:0 ND ND ND ND ND ND heneicosanoic acid

C22:0 388875 430853 416250 450333 442295 427697 behenic acid

C20:3(n-6) 535964 568196 564206 459951 441356 439375 homo-γ-linolenic acid

C23:0 ND ND ND ND ND ND tricosanoic acid

C24:0 112172 132543 122408 136707 135086 133188 lignoceric acid