International sediment exchange for tests on organic contaminants

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(1)WAGENINGEN EVALUATING PROGRAMS FOR ANALYTICAL LABORATORIES. International Sediment Exchange for Tests on Organic Contaminants. Quarterly Report 2012.1. January - March 2012. Dd.

(2) Introduction Dear WEPAL-participants, It is getting more difficult to get samples to different countries. Sometimes shipment is delayed by customs, quarantine services (or other sometimes obscure reasons). For us it is impossible to keep track of all changing regulations. Please contact us if you need special permits or other documents to receive your samples. Our aim is to have the samples in your possession at the start of each round. Contact us if you do not receive the samples in time. Please do not wait until a few weeks before the deadline because we will not be able to send new samples in time. Enquiry 2012 We are interested in your ideas and questions about the WEPAL proficiency testing programmes. To make it easier for your to give your response we have placed an enquiry on our website. We have kept it short so it will not take up much of your time. Your feedback is much appreciated. We decided to remove the section new members from the reports because it could be possible to link new members to Labnumbers or Labcodes. Many laboratories are open with their identity in the labcode while others prefer to hide their identity. Of course this does not mean that laboratories who hide their identity do not trust there own quality. There may be many reasons not to show the identity of a laboratory. Anyway it is not allowed to use the results of the WEPAL proficiency tests for publicty or other promotional activities. Use of the results for scientific purposes is only allowed when approved by WEPAL. The WEPAL programs are organised to help you to improve the quality of your results. When you have ideas or remarks on the programs that can help us to improve them please feel free to contact us. We are always looking forward to hear from you, Yours sincerely,. Bram Eijgenraam Manager WEPAL. Calculated 03-04-2012 (13:50) Approved by Bram Eijgenraam, manager WEPAL. Important Information The results of the April - June 2012 period will be processed in the first week of July 2012. Participants are kindly requested to take care that the results of this series are in Wageningen before the first of July 2012. All results, which are received later, will not be reported. The 2012.3 samples will be mailed at the end of May 2012.. page 1 of 98.

(3) Introduction .......................................................................................................................................................1 General Information ..........................................................................................................................................3 Accreditation .................................................................................................................................................3 Homogeneity of the distributed samples ..........................................................................................................5 Homogeneity tests .....................................................................................................................................5 Check of results .........................................................................................................................................6 The quarterly report ..........................................................................................................................................6 Reporting of data .......................................................................................................................................6 Statistics ...........................................................................................................................................................6 Normal Distribution Approximation (NDA) .................................................................................................6 Median and MAD .......................................................................................................................................7 Z-score ......................................................................................................................................................7 Evaluation of results ..................................................................................................................................7 Uncertainty of the assigned value .............................................................................................................8 Rounding of results ...................................................................................................................................8 Materials Analysed ...........................................................................................................................................8 Method Indicating Code (MIC)..........................................................................................................................8 References and related literature .................................................................................................................. 10 Used abbrevations and symbols ................................................................................................................... 11 Analysis SETOC 2012.1 ............................................................................................................................... 12 Polycyclic aromatic hydrocarbons.............................................................................................................. 13 Polychlorobiphenyls ................................................................................................................................... 28 Organochlorine pesticides ......................................................................................................................... 37 Other parameters ....................................................................................................................................... 48 Metals ......................................................................................................................................................... 51 Dibenzo-P Dioxin ....................................................................................................................................... 57 Dibenzofuran .............................................................................................................................................. 59 Experimental .............................................................................................................................................. 62 SETOC 2012.1 Z - Scores ............................................................................................................................ 63 Per Participant............................................................................................................................................ 64 Errors and Corrections SETOC 2011 Period 4 ............................................................................................. 95. page 2 of 98.

(4) General Information Accreditation The Wageningen Evaluating Programmes for Analytical Laboratories organisation is accredited for the organisation of Interlaboratory Studies by the Dutch Accreditation Council RvA since April 26, 2000. The accreditation is based on the ILAC-requirements (Guidelines for the requirements for the competence of providers of proficiency testing schemes, ISO/IEC 17043). In the following table the scope is given for all WEPAL programs. Table 1 Scope of the WEPAL programs. IPE. Group. (Determinands in bold are in the scope of the accreditation). Determinand. Inorganic Chemical Composition. Ag, As, B, Ba, Be, Bi, Br, Ca, Cd, Cl, Co, Cr, Cs, Cu, F, Fe, Ga, Hg, I, K, Li, Mg, Mn, Mo, N - Kjeldahl, N - NH4 (as N), N - NO3, Na, Ni, P, Pb, Pd, Pt, Rb, Rh, S, Sb, Se, Sn, SO4, Sr, Ti, V, Zn. Real totals. Al, C - elementary, N - elementary, Si. Acid extractable (So-called totals). Al, Si. Other determinations. delta. Nutritional values. ADF-ash-containing, ADF-ash-free, Crude fibre, NDF-ash-containing, NDF-ash-free, Polysaccharides (starch), TDF, TDF-non-soluble, TDF-soluble, Total ash, Total Disaccharides, Total fat, Total monosaccharides. ISE. Determinand. Group. 13. C, delta. 15. N. Real totals. Ag, Al, As, B, Ba, Be, Bi, Br, C - elementary, Ca, Cd, Ce, Co, Cr, Cs, Cu, F, Fe, Ga, Ge, Hg, I, K, La, Li, Mg, Mn, Mo, N - elementary, Na, Nb, Nd, Ni, P, Pb, Pd, Pt, Rb, Rh, S, Sb, Sc, Se, Si, Sn, Sr, Te, Th, Ti, Tl, U, V, W, Y, Zn, Zr. Acid extractable (So-called totals). Ag, Al, As, B, Ba, Be, Bi, Br, Ca, Cd, Ce, Co, Cr, Cu, F, Fe, Ga, Hg, I, K, La, Li, Mg, Mn, Mo, N, Na, Nb, Nd, Ni, P, Pb, Pt, Rb, S, Sb, Sc, Se, Si, Sn, Sr, Te, Th, Ti, Tl, U, V, Y, Zn, Zr. Aqua Regia (ISO 11466). Ag, Al, As, B, Ba, Be, Bi, Br, Ca, Cd, Ce, Co, Cr, Cu, F, Fe, Ga, Hg, I, K, La, Li, Mg, Mn, Mo, N, Na, Nb, Nd, Ni, P, Pb, Pt, Rb, S, Sb, Sc, Se, Si, Sn, Sr, Te, Th, Ti, Tl, U, V, Y, Zn, Zr. Extraction with boiling 2M HNO3. Cd, Co, Cr, Cu, Hg, Mo, Ni, Pb, Tl, Zn. Extraction with 0.1M NaNO3. Cd, Cu, Ni, Pb, Zn. Extraction with 0.01M CaCl2 1:10. Al, B, Cd, CN, Co, Cr, Cu, Fe, K, Mg, Mn, N - NH4, N - NO3, N total soluble, Na, Ni, P, Pb, SO4, Zn. Soil characteristics. C - org others (W&B a.o.), EC-SC (ISO 11265), Fraction < 16 µm, Fraction < 2 µm, Fraction < 63 µm, Fraction > 63 µm, Org.matter (L.O.I.), pH - CaCl2, pH - H2O, pH - KCl, TC=Total C (org.+inorg.), TIC=Tot.Inorg C(CaCO3), TOC=Total Org. C. Other determinations. B - Hot water, CN - Free, CN - Total, delta K - HCl, Mg - NaCl, Moisture-content. Fluoride (Swiss standard procedure). F - Total. Digestion with conc. HNO3 + conc. HCl + H2O2 (UNEP-UN/EC 91075A). Al, As, B, Ba, Be, Br, Ca, Cd, Co, Cr, Cu, F, Fe, Ga, Hg, I, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Rb, S, Sb, Se, Si, Sn, Sr, Tl, V, Y, Zn, Zr. Pot. CEC using 1M NH4-acetate at pH=7. Al, Ca, CEC, K, Mg, Na. Pot. CEC using 1M or 0.1M BaCl2-TEA Al, Ca, CEC, K, Mg, Na at pH=8.1 (ISO 13536 OR BZE). page 3 of 98. 13. C, delta. 15. N,.

(5) ISE. Group. Determinand. Pot. CEC using 1M NH4Cl (BZE). Al, Ca, CEC, Fe, H, K, Mg, Mn, Na. Act. CEC using 0.01M BaCl2 (ISO 11260). Al, Ca, CEC, Fe, H, K, Mg, Mn, Na. Act. CEC using 0.1M BaCl2 (UNEP-UN/EC 91065A). Al, Ca, CEC, Fe, H, K, Mg, Mn, Na. Act. CEC using cobaltihexamine (AFNOR NFX 31 130). Al, Ca, CEC, Fe, H, K, Mg, Mn, Na. Mehlich-3. Al, As, B, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, P, Pb, Zn. Extraction with Ca-lactate (VDLUFA). K, P. Extraction with double lactate (VDLUFA). K, P. Water soluble 1:10 (w/v) (EN-12457-4). Br, Cl, F, N - NO3. Extraction with 0.01M CaCl2 + 0.005M DTPA 1:10 (w/v). Cu, Fe, Mn, Zn. Extraction with 1M KCl 1:10 (w/v). N - NH4, N - NO3. Phosphorus and related analysis. Al - Ox, Fe - Ox, P - Ox, P - AL, P - Bray, P - Olsen, Pw. Extraction with 1M HCl (Polish standard). B, Cu, Fe, Mn, Zn. Water soluble 1:10 (w/v) (NL VPR C85-06) Br, Cl, F, SO4. UK Soil Methods. K - NH4NO3 (1/5), Mg - NH4NO3 (1/5), P – NaHCO3 (1/20), pH - H2O (2/5). SETOC. Determinand. Group. Polycyclic aromatic hydrocarbons. acenaphtene, acenaphtylene, anthracene, benz(a)anthracene, benzo(a)pyrene, benzo(b)fluoranthene, benzo(ghi)perylene, benzo(k)fluoranthene, chrysene, dibenz(ah)anthracene, fluoranthene, fluorene, indeno(1,2,3-cd)pyrene, naphtalene, phenanthrene, pyrene. Polychlorobiphenyls. PCB 028, PCB 031, PCB 052, PCB 077, PCB 081, PCB 101, PCB 105, PCB 114, PCB 118, PCB 123, PCB 126, PCB 128, PCB 138, PCB 149, PCB 153, PCB 156, PCB 157, PCB 167, PCB 169, PCB 180, PCB 189. Organochlorine pesticides. 1,2,3 trichlorobenzene, 1,2,3,4 tetrachlorobenzene, 1,2,3,5 tetrachlorobenzene, 1,2,4 trichlorobenzene, 1,2,4,5 tetrachlorobenzene, 1,3,5 trichlorobenzene, aldrin, alpha-endosulfan, alpha-HCH, beta-endosulfan, beta-HCH, chlordane, cis-chlordane, delta-HCH, dieldrin, endosulfan, endosulfan sulfate, endrin, gamma-HCH, heptachlor, heptachlor epoxide, hexachlorobenzene, hexachlorobutadiene, isodrin, o,p`-DDD, o,p`-DDE, o,p`-DDT, p,p`-DDD, p,p`-DDE, p,p`-DDT, pentachlorobenzene, pentachlorophenol, Sum tetrachlorobenzenes, Sum trichlorobenzenes, telodrin, toxaphene, trans-chlord. Other parameters. AOX, CN - Free, CN - Total, EOX, Inorganic carbon, Mineral oil, GC, Mineral oil, IR, Organic carbon, Particles < 2 µm, Particles < 63 µm, Particles > 63 µm. Metals (aqua regia). As, Ba, Cd, Co, Cr, Cu, Hg, Mo, Ni, Pb, Zn. Dibenzo-P Dioxin. 1,2,3,4,6,7,8 Cl7DD, 1,2,3,4,7,8 Cl6DD, 1,2,3,6,7,8 Cl6DD, 1,2,3,7,8 Cl5DD, 1,2,3,7,8,9 Cl6DD, 2,3,7,8 Cl4DD, Cl8DD. Dibenzofuran. 1,2,3,4,6,7,8 Cl7DF, 1,2,3,4,7,8 Cl6DF, 1,2,3,4,7,8,9 Cl7DF, 1,2,3,6,7,8 Cl6DF, 1,2,3,7,8 Cl5DF, 1,2,3,7,8,9 Cl6DF, 2,3,4,6,7,8 Cl6DF, 2,3,4,7,8 Cl5DF, 2,3,7,8 Cl4DF, Cl8DF. page 4 of 98.

(6) SETOC. Group. Determinand. Brominated Flame Retarders. BDE 028, BDE 047, BDE 066, BDE 085, BDE 099, BDE 100, BDE 153, BDE 154, BDE 183, BDE 209. Experimental. DEHP, Tributyl Tin (TBT). MARSEP. Group. Determinand. Real totals. Ag, Al, As, B, Ba, Be, Bi, Br, C, Ca, Cd, Co, Cr, Cu, F, Fe, Ga, Hg, I, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Sb, Se, Si, Sn, Sr, Ti, Tl, V, Zn. Acid extractable (So-called totals). Ag, Al, As, B, Ba, Be, Bi, Br, C, Ca, Cd, Cl, Co, Cr, Cu, F, Fe, Ga, Hg, I, K, Li, Mg, Mn, Mo, N, N - NH4 (as N), N - NO3 (as N), Na, Ni, P, Pb, S, S - SO4, Sb, Se, Si, Sn, Sr, Ti, Tl, V, Zn. Other determinations. AOX, loss-on-ignition. BIMEP. Determinand. Group. General Analysis. ash, calorific value, moisture, Volatile Matter. Elementary Analysis. Carbon (C), Cl, Hydrogen (H), Nitrogen (N), S. Water Soluble Elements. Cl, K, Na. Major Elements. Al, Ca, Fe, K, Mg, Na, P, Si. Minor Elements. As, Ba, Be, Cd, Co, Cr, Cu, F, Hg, Mn, Mo, Ni, Pb, Sb, Se, Sn, Te, Ti, Tl, V, Zn. The selection of determinands included in the scope of accreditation is based on information about the homogeneity and stability of the samples. This information is available when sufficient participants have reported results for a determinand in the past 3 years. Determinands which are not reported regularly in sufficient numbers to have a statistical evaluation are not (yet) included in the scope of the accreditation. Subcontracting Some aspects of the proficiency testing scheme may from time to time be subcontracted. When subcontracting occurs it is placed with a competent subcontractor. WEPAL is responsible to the scheme participants for the subcontractor's work. The analysis for the homogeneity tests of the samples used in this proficiency test are carried out by a subctractor. Confidentiality of results The confidentiality of the results is extremely important in the Wepal programs. The participants may opt for a code name that indicates their laboratory, or one that ensures their anonymity. In the reports, only the code names will be mentioned. When an accrediting body or a regulatory authority requires the proficiency test results to be provided by Wepal the participants shall be notified and asked for permission Complaints and or remarks The reports of WEPAL are assembled with the utmost care. Please contact us on info.wepal@wur.nl if you feel that the reports are not at a satisfactory standard or if you encountered errors in your results. Also feel free to contact us if you have any other complaints, remarks and or suggestions.. Homogeneity of the distributed samples Homogeneity tests WEPAL has developed special equipment for the production of representative subsamples (Houba, 1993) from a bulk material. The proper functioning of this equipment is tested by a homogeneity test in the final subsamples. To perform this test, samples are collected at regular intervals during the preparation of the page 5 of 98.

(7) the samples. The collected samples, with a minimum of 10, are analysed in duplicate measurements under repeatability conditions. A selection of critical determinands is chosen for the tests. The results of the homogeneity tests are published in the annual reports. All samples used in this round of the proficiency test have passed the homogeneity test.. Check of results Before distribution of the periodic reports to the participants, a final check is made based on the results found by the participants. This check is made for all reported determinands. The variations between laboratories and concentrations are compared with the patterns as found in the previous 5 years. The expected pattern is a high CV at a low concentration and a gradually decreasing CV at higher concentrations till a more or less constant level of CV-values is reached (Houba et al., 1986). Deviations from this expected pattern are mentioned in the periodic reports. This might be an indication of inhomogeneity of the material for the determinand. All data of this period are compared with the general patterns as published in the latest year report. No deviating values were found.. The quarterly report In order to evaluate the accuracy and precision of the analytical procedures used, five proficiency testing programs have been established. At this moment the WEPAL Exchange Programs comprises approximately 600 laboratories in many countries. The participating laboratories receive four air-dried samples every three months and analyse the samples according to their own procedures. The results of the determinations are collected and processed at Wageningen University and published every three months. The participating laboratories are informed of the results in the third week of the next three-month period. Each participant can compare his results with those of all the other members of the exchange program. WEPAL will not comment on results unless asked to do so.. Reporting of data °. The analysed components must be reported in ovendry (105 C) material. For this purpose the moisture content has to be determined separately and the analytical results have to be recalculated (see the form to report the results). To get reproducible results of these moisture contents we recommend you to dry the ° material during at least 3 hours at 105 C and let cool down in a desiccator before weighing.. Statistics Normal Distribution Approximation (NDA) Interlaboratory studies like the WEPAL proficiency testing ringtests frequently give rise to datasets that have complex distributions including excessive tailing and multiple modes. Consequently, sophisticated statistical methods are required to obtain meaningful assessments. The strategy that was used until r2009 made use of an outlier test followed by straightforward statistics. Problem with this strategy is that removal of outliers causes an underestimation of variance of the dataset. Therefore a methodology was needed that does not rely on arbitrary outlier removal or subjective manual interpretations. Ideally the used methodology must provide the characteristics of the highest mode of the dataset. The model that is chosen tcalculates population characteristics (mean and standard deviation) from experimental datasets (Cofino 2000). The model uses an estimate for the probability density function (pdf) of the measurement process and calculates a best fit based on all observed values. The implementation of the model that is used does not require uncertainty estimates for all data points. Instead it uses a normal distribution approximation (NDA) for the pdf of the individual data points. In essence, the pdf’s of the individual datapoints are superposed on each other to create a continuous pdf representing the entire distribution (all datapoints). With the mathematical model coefficients can be obtained by looking for the combination of data points that has the highest probability in the basis set. This maximization amounts to the identification of the first mode of the dataset. The coefficients can be used to calculate the weighted mean and standard deviation. Subsequent calculations give additional modes of the distribution and for each mode the expectation value (mean), the standard deviation and a percentage indicating the fraction of observations encompassed. In this report only mean and standard deviation for the first mode (combination with the highest probability in the dataset) are given.. page 6 of 98.

(8) The model is tested on simulated data sets and datasets of several interlaboratory studies. It is demonstrated that the model is robust and insensitive to outliers. It can cope with asymmetric, strongly tailing and multimodal distributions. Publications describing the procedure in more detail and results of the tests are in preparation. With the NDA model mean and standard deviation are calculated using all reported data when at least 8 results are left after removal of reported 'lower than' (<) and 0 (= zero) values. No outliers are removed. Table 2. The model summarised • • • •. •. Each observation is attributed an ‘ Observation measurement function’ (OMF, φi) An OMF is defined as the square root of the probability density function appropriate for the 2 observation. If normal distributions are used: φi=√N(µi,σi ) The set of φi ‘s constitutes a basic set in which the population measurement function Ψ is constructed: Ψi=∑cik φk The coefficients are obtained by finding the combination which renders highest probability 2 density (maximise ∫Ψ dx, x being concentration). Mathematically this amounts to solving the eigenvector-eigenvalue equation Sc=λc, Sij being an overlap integral defined as ∫ φi φjdx, 0≤ Sij ≤ 1 Mean and standard deviation of Ψi are calculated from the first and second moment of the 2 probability density function Ψi. ∫ xΨ dx , m = ∫ Ψ dx ∫ x Ψ dx − m s = ∫ Ψ dx 2 i. i. 2 i. 2. 2 i. •. 2 i. 2 i. 2 i. When the NDA approximation is used the variance calculated by the model represents the sum of the estimates for the within-laboratory and between-laboratory variances, i.e. 2 2 si2 = s between labs ,i + s within labs ,i. Median and MAD For each determinand a median value and a median of absolute deviations (MAD) are calculated using all reported data except the reported '<' values. Deviating results like stragglers and outliers are not removed. The median is the middle observation of the sorted observations. In the case of an even number of observations it is the mean of the two middle observations. Using the median instead of mean, extreme data have less influence. MAD is the median of the absolute values of the observations minus their median.. Z-score For all analytical data a Z-score is calculated according to the formula:. Z- score =. X- X mean Sd. in which: X = the reported value Xmean = the mean of all values calculated with the NDA model Sd = standard deviation calculated with the NDA model. Evaluation of results For the evaluation of results the absolute value of the Z-score is used. Questionable results 2 < | Z | < 3 are marked as stragglers (*). Deviating results with | Z | > 3 are marked as outliers (**).. page 7 of 98.

(9) Results reported as ‘smaller than’ (<) are also evaluated. When this ‘smaller than’ value is lower than the mean a Z-score is calculated. Based on this z-score these ‘smaller than’ values can also be marked as straggler or outlier. In these cases the ‘smaller than’ value is set too low.. Uncertainty of the assigned value The aim of this proficiency testing scheme is to establish comparability among laboratories. Results for measurands in this scheme are dependent on the methods which are used. It is not feasible to establish metrological traceability of the assigned value. Assigned values are therefore based on consensus values. In this proficiency test the robust standard deviation is used as standard deviation for proficiency assessment. The uncertainty in the assigned value is calculated as :. ux = s / √N s = robust standard deviation N = number of results The uncertainty in the assigned value may influence the evaluation of the results (calculated Z-scores). This influence is considered to be negligible if the following conditions is met:. ux ≤ 0.3 * σpt ux = uncertainty in the assigned value σpt = standard deviation for proficiency assessment ( = s) Because σpt = s this evaluation reverts to : s / √N ≤ 0.3 * s or √N ≥ 3 The influence of uncertainty on the evaluation of the results is therefore dependent on the number of results. Above 10 results of uncertainty on the assigned value is negligible. From 8 to 10 results uncertainty of the consensus value is larger than 0.3 σpt and therefore may influence the evaluation of the results. Below 8 results no consensus value is given.. Rounding of results Rounding interval is set to have at least three significant digits for the results. This is based on the value of the mean. If no mean value is available (less than 8 results) the median is used. In cases where between laboratory variation is small (based on the standard deviation) an extra digiti shown. For the statistical results (mean, standard deviation, median and MAD) one extra digit is shown. Note that larger results are also rounded (e.g. 1809 may be rounded as 1810).. Materials Analysed Table 3 Sample 1 2 3 4. Materials analysed in this period. Sample ID Type 791 Marine Sediment 792 Marine Sediment 784 Sediment 776 Marine Sediment. Country Netherlands Netherlands Netherlands Italy. Method Indicating Code (MIC) In order to evaluate the analytical results for each reported determinand (see Table 4 for the different element groups), a Method Indicating Code (MIC) is used. Details of the analytical procedures used by the individual participants are indicated by characters, added at the end of each row with results. The first character indicates the method of extraction or digestion according to the codes explained in Table 5. The next two characters describe clean-up procedure (Table 6) and separation technique (Table 7). The last characters indicate the method of detection of the element in the extracts or digests (Table 8). In this way it. page 8 of 98.

(10) is possible for all participants to compare the results of their analytical procedures more specifically with the results of other participants. This could be a further valuable tool in judgement of the individual results. Table 4 Method 1 2 3 4 5 6 7 8. Used abbreviations Abbreviation Method PAH Polycyclic aromatic hydrocarbons PCB Polychlorobiphenyls OCB Organochlorine pesticides OD Other parameters MET Metals DD Dibenzo-P Dioxin DF Dibenzofuran EXP Experimental. Table 5 Code A B C D E F J Q T U V Y Z. Extraction Extraction No extraction Supercritical fluid extraction (SFE) Soxhlet extraction Pentane Dichloromethane Freon Petroleum ether Ultrasonic extraction Shaking Microwave aqua regia (using boiling under reflux) Aqua Regia (using a Microwave system) Aqua Regia Other (specify). Table 6 Code A E H K N R U V W X Y Z. Clean-up procedure Clean up Procedure No Clean-Up Liquid-liquid partition Liquid-liquid partition, sulphur removal Liquid-liquid partition, column chromatography Liquid-liquid partition, sulphur removal, column chromatography Sulphur removal Column chromatography Sulphur removal, column chromatography Filtration Solid phase extraction (SPE) Removal of polar compounds with Florisil Gel permeation chromatography (GPC) Others (specify). Table 7 Code A E H I J K Z. Separation technique Separation Technique No Separation HPLC, C-18 HPLC, C-8 GC, splitless GC, splitless (2 columns) GC, split (2 columns) GC, on-column Others (specify). page 9 of 98.

(11) Table 8 Code A AA AC AE AG AJ AL AN AP B BA BC BE BG BJ BL BN BP C CC CE D E F G H IA IB JA JB JC KA KB L M MA N O OP P Q R S T Y YA YB YC Z *. Detection technique Detection Technique AAS-FLAME without background correction using air-acetylene without background correction using N2O-acetylene with deuterium background correction using air-acetylene with deuterium background correction using N2O-acetylene with Zeeman background correction using air-acetylene with Zeeman background correction using N2O-acetylene with pulsed hollow cathode lamp background correction using air-acetylene with pulsed hollow cathode lamp background correction using N2O-acetylene AAS-ETA without background correction without chemical modifier without background correction with chemical modifier* with deuterium background correction without chemical modifier with deuterium background correction with chemical modifier* with Zeeman background correction without chemical modifier with Zeeman background correction with chemical modifier* with pulsed hollow cathode lamp without chemical modifier with pulsed hollow cathode lamp with chemical modifier* Flame emission ICP-AES (different wavelengths are possible; indicate the used wavelength other excitation source (dif. wavelengths possible;indicate used wavelength ICP-MS Spectrophotometry Hydride technique (similar techniques using analyte volatilization;specify) Cold vapour technique Ion selective electrode Direct voltammetry Stripping voltammetry Gas chromatography Liquid chromatography Ion chromatography X-ray fluorescence with material melted X-ray fluorescence with material pressed Neutron Activation Analysis Titrimetric Coulometry Near Infrared UV-absorption UV-absorption + fluorescence (O+P) Fluorescence Electron capture Mass selective Flame ionisation Infrared Fractions < 2 µm , < 63 µm and > 63 µm Pipet and sieve method Hydrometer method Instrumental methods (e.g. counters) Others specify concentration, type of chemical modifier and µl injected sample and modifiers. References and related literature -. -. Cofino, W.P., I. van Stokkum, D.E. Wells, R.A.L. Peerboom, F. Ariese (2000). A new model for the inference of population characteristics from experimental data using uncertainties. Application to interlaboratory studies. Chemom. Intell. Lab. Syst. 53, 37-55. Dijk, D. van and V.J.G. Houba (2000). Homogeneity and Stability of Materials Distributed Within the Wageningen Evaluating Programmes for Analytical Laboratories. Commun. Soil Sci. Plant Anal. 31 (11-14), 1745 -1756. page 10 of 98.

(12) -. -. Dijk, D. van, V.J.G. Houba and J.P.J. van Dalen (1996). Aspects of quality assurance within the Wageningen Evaluating Programmes for Analytical Laboratories (WEPAL). Commun. Soil SCi. Plant Anal. 27, 433 - 439. Eurachem (2000). Selection, use and interpretation of proficiency testing (PT) schemes by laboratories. Eurachem Nederland, task group ‘proficiency testing schemes’ and Laboratory of the Government Chemist (LGC), United Kingdom. Feinberg, M., E. Bugner, G. Theiller, V.J.G. Houba and F. Kadijk (1995). Expression of the reference value for proficiency tests. J. Chemometrics 9,197-209. Houba, V.J.G. (1993). A device for automatic subsampling of soil, sediment and plant material for proficiency testing. Fresenius J. Anal. Chem. 345, 156 -157. Houba, V.J.G., W.J. Chardon and K. Roelse (1993). Influence of grinding of soil on apparent chemical composition. Commun. Soil Sci. Plant Anal. 24, 1591 - 1602. Houba, V.J.G., J.J. van der Lee and I. Novozamsky (1996). Evaluating the state-of-the-practice in soil measurements in relation to environmental regulations. Accred. Qual. Assur. 1, 92 - 98. Houba, V.J.G. and I. Novozamsky (1998). Influence of storage time and temperature of air-dried soils on pH and extractable nutrients using 0.01 M CaCl2. Fresenius J. Anal. Chem. 360, 362 - 365. Houba, V.J.G., I. Novozamsky and J.J. van der Lee (1994a). Status and future of soil and plant analysis. Commun. Soil Sci. Plant Anal. 25, 753 - 765. Houba, V.J.G., I. Novozamsky and J.J. van der Lee (1994b). Standardization and validation of methods of soil and plant analysis as conditions for accreditation. Commun. Soil Sci. Plant Anal. 25, 827 - 841. Houba, V.J.G., I. Novozamsky and J.J. van der Lee (1994c). Aspects of pre-treatment of soils for inorganic chemical analysis. QuRmica AnalitRca 13, 94 - 99. Houba, V.J.G., I. Novozamsky and J.J. van der Lee (1995). Influence of storage of plant samples on their chemical composition. The Science of the Total Environment 176, 73 - 79. Houba, V.J.G., I. Novozamsky and J.J. van der Lee (1996). Quality aspects in laboratories for soil and plant analysis. Commun. Soil Sci. Plant Anal. 27, 327 - 348. Houba, V.J.G., J. Uittenbogaard and P. Pellen (1996). Wageningen Evaluating Programmes for Analytical Laboratories (WEPAL), organisation and purpose. Commun. Soil Sci. Plant Anal. 27, 421 - 431. ILAC-G13 (2007). ILAC Guidelines for the Requirements for the Competence of Providers of Proficiency Testing Schemes. 23 p. Montfort, M. A.J. van (1996). Statistical remarks on laboratory-evaluating programs for comparing laboratories and methods. Commun. Soil Sci. Plant Anal. 27, 463 - 478. Novozamsky, I., V.J.G. Houba, R.Ch. Daniel and the members of CII (1993). Certification of cabbage and carnation samples and their use in an international proficiency study. Fresenius J. Anal. Chem. 345, 198 - 201. Thompson, M. and R. Wood (1993). The international harmonized protocol for the proficiency testing of (chemical ) analytical laboratories. Pure and Appl. Chem. 65, 2123 - 2144.. Used abbrevations and symbols Table 9 Where. Used abbreviations and symbols Abbreviation. Results Results Results Results, Z-scores Results, Z-scores Results, Z-scores Results, Z-scores Results statistical values Z-scores Errors Errors Errors Errors Errors Errors. MIC MAD Sd < * ** # C D E M N R. Explanation method indicating code median absolute deviation standard deviation value smaller than straggler outlier no result was submitted not calculated less than 8 values, no mean and Sd calculated Correction participant Results received after deadline (before publication date) Error WEPAL Modified results New results Results removed. page 11 of 98.

(13) Analysis SETOC 2012.1. page 12 of 98.

(14) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample acenaphtene (µg/kg) BOANALHOAG (2) MLABTW (4) Alconheinr (7) ANM (8) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) ANATEK (29) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) TAMPERE (911) SHI (912) WANDSCH (958) PA2010LAB (1058). NDA mean NDA st dev N Median MAD. acenaphtylene (µg/kg) BOANALHOAG (2) MLABTW (4) Alconheinr (7) ANM (8) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21). NDA mean NDA st dev N. 791. 25.0 60.0 50.0 39.9 47.0 37.0 46.8 54.3 39.0 74.5 50.0 43.9 50.0 103.0 42.0 50.0 24.0 50.0 27.0 100.0 43.0 38.0 50.0 30.0 32.0 49.6 47.0 40.9 32.0 29.6 56.4 46.4 40.2 29.5 22.0 36.4 51.0 69.0 47.5 21.4 29.8. 792. <. * <. <. < <. <. *. 45.0 100.0 90.0 83.9 89.7 78.0 94.4 101.4 73.0 128.7 80.0 84.6 90.0 102.0 65.0 100.0 51.0 73.2 81.0 100.0 92.0 81.1 86.0 62.0 71.0 111.0 83.0 84.1 63.6 68.9 73.6 99.8 64.3 71.8 59.0 76.4 108.0 32.9 102.0 45.5 74.3. 784. * <. **. <. <. * *. 113 8028 210 231 203 175 282 198 163 364 240 167 220 230 203 240 145 143 225 226 221 187 187 216 180 186 159 231 236 144 202 252 240 182 212 209 179 194 199 269 149 187. 776. * **. *. **. 5393 216 6700 7701 7842 6036 7448 6224 3760 10042 8630 5754 8190 6480 5230 8220 7100 5786 5332 13400 4121 6276 5972 6980 5600 6344 5090 7663 6605 195 6433 7550 5737 7145 7130 5349 6621 6372 8330 7420 7030 5147. MIC. **. * *. **. **. QWH R ZWAOP Q-K R Q-HR BWK R ZUH R Z-H R D-AOP DNZ R Q-H R QZH R BRHR FHAOP ZVAOP --Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P D-H R QRH R Q-HR JAHR B-HR ZUH R J-K R Q-HR QAH R Q-JR ZWH R. ================= Statistical Results ================= 40.34 79.92 202.3 6547 12.73 16.11 37.5 1379 35 38 42 42 40.89 80.50 203.0 6457 8.89 10.50 25.5 978 ====================================================. 19.0 520.0 70.0 16.9 9.3 24.0 65.2 100.0 30.0. < **. ** <. ================= 20.72 9.76 30. 38.0 260.0 80.0 38.1 14.2 47.0 106.2 100.0 51.0. < *. ** <. 192 170 < 410 209 62 302 732 ** 100 < 287. 864 165 < 1300 616 212 960 2049 ** 165 648. Summary Statistics ================== 40.03 235.0 637.2 17.47 88.4 391.5 33 36 41 page 13 of 98. QWH R ZWAOP Q-A R Q-HR BWK R ZUH R Z-H R D-A O DNZ R. (cont.).

(15) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample. 791. acenaphtylene (µg/kg) (cont.) ANATEK (29) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) TAMPERE (911) SHI (912) WANDSCH (958) PA2010LAB (1058). NDA mean NDA st dev N Median MAD. anthracene (µg/kg) ZINDZIWE (1) BOANALHOAG (2) MLABTW (4) AL-West (5) Alconheinr (7) ANM (8) BLAUWHUIS (14) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) EXACT (28) ANATEK (29) ELML (33) WELLAB (35) US (39) LAS (48). NDA mean NDA st dev N. 19.2 50.0 27.9 37.0 310.0 10.0 70.0 24.0 50.0 25.0 100.0 25.0 25.5 50.0 22.0 16.0 30.4 13.0 7.8 17.0 20.0 19.6 20.0 48.8 18.3 10.0 14.8 20.0 56.3 34.4 12.1 13.2. 792. <. < < **. < <. <. < < * <. **. 33.0 50.0 47.0 64.0 306.0 10.0 120.0 42.0 50.0 66.0 100.0 52.0 55.9 87.0 39.0 37.0 47.5 27.0 17.2 35.5 20.0 31.5 35.9 60.0 44.4 14.0 29.0 35.0 26.8 68.1 27.0 31.4. 784. <. < < **. < <. *. <. 166 280 262 329 305 100 570 280 100 220 235 240 262 279 538 300 218 175 205 126 204 197 209 302 302 123 168 205 393 353 160 173. 776. < < ** <. **. MIC. 576 770 1075 1024 452 101 2000 ** 790 252 650 705 449 908 585 1500 * 875 621 394 569 303 636 257 483 496 1208 1070 335 341 740 1030 1290 543 279. Q-H R QZH R BRHR FHAOP ZVAOP --Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R Q-HR QAH R Q-JR ZWH R. ================= Statistical Results ================= 20.72 40.03 235.0 637.2 9.76 17.47 88.4 391.5 30 33 36 41 23.00 39.00 237.5 636.0 7.00 12.00 62.5 272.0 ====================================================. 49 87 74 150 108 101 124 145 125 143 181 110 787 ** 150 181 130 168 ================= 112.6 35.2 47. 88 191 250 210 207 221 351 * 206 254 307 230 1274 ** 260 310 220 300. 720 347 * 432 680 727 834 682 784 976 683 722 710 4826 ** 860 795 720 861. 250 506 683 670 670 824 673 895 1228 697 625 870 6792 1490 1866 1040 658. *. ** ** **. Summary Statistics ================== 207.0 704.4 583.9 64.4 161.6 290.8 47 48 48 page 14 of 98. --A E QWH R ZWAOP ZRAOP Q-K R Q-HR --BWK R ZUH R Z-H R D-AOP DNZ R Q-K R Q-H R QZH R BRHR FHAOP ZVAOP. (cont.).

(16) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample. 791. 792. 784. anthracene (µg/kg) (cont.) CHEMLABSIT (52) ATM (54) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) CHE (887) TAMPERE (911) SHI (912) WANDSCH (958) LUNLAB (1052) PA2010LAB (1058). 87 110 170 81 105 105 81 100 < 95 152 146 93 99 91 97 106 120 96 148 119 174 76 75 103 115 75 188 * 129 57 176 101. 131 170 310 135 221 189 242 165 214 317 262 156 176 163 163 196 230 178 242 230 146 146 153 232 205 122 93 241 114 317 207. 623 660 960 540 557 689 837 703 481 896 913 580 804 476 718 716 685 613 806 760 826 692 543 517 605 430 791 861 425 1174 * 587. NDA mean NDA st dev N Median MAD. benz(a)anthracene (µg/kg) ZINDZIWE (1) BOANALHOAG (2) MLABTW (4) AL-West (5) Alconheinr (7) ANM (8) BLAUWHUIS (14) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) EXACT (28) ANATEK (29) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) ATM (54). NDA mean NDA st dev N. 776. 360 350 1900 390 462 657 1050 645 770 18016 26600 600 655 298 480 337 689 426 580 468 545 485 441 426 650 243 760 1430 422 4081 437. MIC. **. ** **. * **. --F-A P Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R ZYHR Q-HR QAH R Q-JR TWHR ZWH R. ================= Statistical Results ================= 112.6 207.0 704.4 583.9 35.2 64.4 161.6 290.8 47 47 48 48 110.0 210.0 712.8 655.8 23.0 43.6 110.5 214.5 ====================================================. 90 ** 278 203 280 317 234 295 293 313 289 322 240 556 ** 240 323 290 358 246 350 ================= 270.3 52.3 47. 221 ** 647 660 872 * 541 736 694 638 555 635 600 1500 ** 600 709 726 758 536 780. 3600 1416 ** 2456 * 3600 3952 3249 4196 3027 4994 3662 3000 3400 6715 ** 3650 3048 3923 4230 3770 4360. 1900 1122 * 3678 ** 2000 2598 1638 2005 2057 2478 2155 1658 2000 3574 ** 1820 2112 2336 2390 1840 2430. Summary Statistics ================== 635.9 3775 2096 95.4 618 403 46 47 47 page 15 of 98. --A E QWH R ZWAOP ZRAOP Q-K R Q-HR --BWK R ZUH R Z-H R D-AOP DNZ R Q-K R Q-H R QZH R BRHR FHAOP ZVAOP --F-A P. (cont.).

(17) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample benz(a)anthracene (µg/kg) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) TAMPERE (911) SHI (912) WANDSCH (958) LUNLAB (1052) PA2010LAB (1058). NDA mean NDA st dev N Median MAD benzo(a)pyrene (µg/kg) ZINDZIWE (1) BOANALHOAG (2) MLABTW (4) AL-West (5) Alconheinr (7) ANM (8) BLAUWHUIS (14) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) EXACT (28) ANATEK (29) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) ATM (54) 32A (56) HILL (58) ARCHIMEDES (59). NDA mean NDA st dev N. 791. 792. 784. 776. 3670 4700 4030 4149 3963 3749 3197 3942 4410 3560 4584 2917 3945 4319 3960 3316 4253 3558 4002 5170 * 2228 * 2943 3706 3790 4050 3198 5406 * 3598. 2140 1570 2008 2278 2490 1793 1693 2475 2260 1800 2605 1598 2242 2310 2309 1707 2644 1960 2111 1930 2766 1773 2166 1940 2810 1924 2874 2053. MIC. (cont.) 310 155 265 256 193 250 200 329 296 230 247 176 272 256 290 259 317 276 290 216 377 221 280 535 439 210 261 261. *. *. ** **. 690 400 623 568 615 622 489 834 658 590 776 424 575 628 670 547 695 638 730 568 662 513 627 198 1040 569 815 630. *. *. *. ** **. Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R Q-HR QAH R Q-JR TWHR ZWH R. ================= Statistical Results ================= 270.3 635.9 3775 2096 52.3 95.4 618 403 47 46 47 47 276.0 632.6 3770 2111 36.0 64.7 426 279 ====================================================. 209 236 215 240 255 223 227 264 198 223 280 200 451 ** 220 273 286 293 249 290 250 122 * 210 ================= 228.4 41.6 48. 327 496 480 552 460 447 601 382 464 483 440 1079 ** 430 520 609 522 462 530 470 270 * 478. 4300 2554 1681 ** 3500 3390 3491 3488 3628 4535 4134 3080 3500 7442 ** 3340 3345 4210 3560 3670 4800 * 3500 4300 3231. 1200 1534 4162 ** 1200 1450 1157 1073 1677 1325 1625 1156 1200 2657 ** 1110 1429 1618 1340 1190 1560 1300 890 1112. Summary Statistics ================== 465.1 3594 1255 80.6 527 244 47 48 48 page 16 of 98. --A E QWH R ZWAOP ZRAOP Q-K R Q-HR --BWK R ZUH R Z-H R D-AOP DNZ R Q-K R Q-H R QZH R BRHR FHAOP ZVAOP --F-A P Z-HS ZXHR Z-H R. (cont.).

(18) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample. 791. 792. benzo(a)pyrene (µg/kg) (cont.) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) CHE (887) TAMPERE (911) SHI (912) WANDSCH (958) LUNLAB (1052) PA2010LAB (1058). 205 197 220 167 280 288 194 191 193 285 188 240 233 281 212 330 * 185 213 205 213 244 401 ** 302 152 205 241. 392 518 503 336 661 * 541 475 373 378 473 408 518 458 536 403 542 433 357 414 447 437 168 ** 623 379 456 505. NDA mean NDA st dev N Median MAD. 3722 3856 3657 2746 3950 4310 3740 4087 2814 3047 3754 3614 3654 4115 2399 * 5909 ** 4160 1453 ** 3072 3368 3590 3540 2830 2950 3805 3534. 776. 1278 1800 1126 1039 2558 1590 1150 1045 965 1846 1304 1392 1324 1531 921 2136 1330 1201 1105 1264 962 1120 1280 1151 1541 1198. MIC. *. **. *. **. ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JKZ R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R ZYHR Q-HR QAH R Q-JR TWHR ZWH R. ================= Statistical Results ================= 228.4 465.1 3594 1255 41.6 80.6 527 244 48 47 48 48 225.0 464.3 3575 1279 27.7 55.7 360 168 ====================================================. benzo(b)fluoranthene (µg/kg) BOANALHOAG (2) MLABTW (4) Alconheinr (7) ANM (8) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) 32A (56) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92). NDA mean NDA st dev N. 784. 162 323 530 475 334 349 624 * 393 478 420 421 365 383 499 550 410 340 350 280 482 638 * 280 258 219. ================= 387.1 118.3 40. 312 * 563 1000 929 571 609 1050 605 728 950 743 742 639 848 950 720 1040 638 547 894 1180 * 595 577 438. 2124 3456 4900 3761 3172 2768 7424 ** 3706 3460 6320 * 3455 4055 3810 4790 5120 5371 4350 4139 3891 3146 4577 6670 * 3420 4087 2610. 2436 3146 3600 3306 2229 2722 4943 * 2978 2490 3270 2806 3182 2800 2850 3970 3808 3550 3092 2451 2441 6205 ** 4510 * 2450 2152 1971. Summary Statistics ================== 699.2 3923 2942 178.8 953 711 40 41 41 page 17 of 98. QWH R ZWAOP Q-K R Q-HR BWK R ZUH R Z-H R D-AOP DNZ R QZH R BRHR FHAOP ZVAOP --Z-HS Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R. (cont.).

(19) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample. 791. benzo(b)fluoranthene (µg/kg) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) TAMPERE (911) SHI (912) WANDSCH (958) LUNLAB (1052) PA2010LAB (1058). NDA mean NDA st dev N Median MAD benzo(ghi)perylene (µg/kg) ZINDZIWE (1) BOANALHOAG (2) MLABTW (4) AL-West (5) Alconheinr (7) ANM (8) BLAUWHUIS (14) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) EXACT (28) ANATEK (29) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) ATM (54) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110). NDA mean NDA st dev N. 792. (cont.) 406 291 347 308 444 421 493 236 394 325 307 663 * 523 383 313 570. 784. 664 627 649 536 871 764 999 525 651 601 611 311 * 983 853 632 1005. 776. 3879 3930 4750 3261 5563 3253 6818 ** 4140 1838 * 3368 3416 4260 3660 4760 4092 5601. MIC. 2602 2977 2778 2449 4569 * 2491 4771 * 2460 3209 2630 2687 2810 3390 4116 3468 3908. JKZ R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R Q-HR QAH R Q-JR TWHR ZWH R. ================= Statistical Results ================= 387.1 699.2 3923 2942 118.3 178.8 953 711 40 40 41 41 388.1 657.5 3930 2977 80.6 108.5 647 491 ====================================================. 125 342 210 250 216 194 221 214 288 281 320 210 209 210 288 330 516 220 230 250 163 231 233 189 200 182 287 258 205 185 295 271 217 234. * *. *. * <. ================= 228.6 42.8 47. 192 861 470 375 359 375 429 488 414 492 400 398 380 468 600 728 411 440 420 310 471 432 477 385 362 590 483 405 377 557 424 376 450. ** **. * **. *. 3500 1728 2935 2600 1745 2200 2536 2983 3661 3150 2670 2800 2470 2510 2564 3790 4120 2860 3540 2570 2300 2206 2939 2934 2768 2489 2817 2870 2520 3133 2380 3010 2210 1790. *. *. * **. 3100 1638 3847 1700 1232 1444 1512 2037 1975 2043 1709 1700 2609 1270 1618 2230 2410 1520 1900 1710 1400 1282 1883 1764 1536 1688 1956 1770 1450 1398 1438 2003 1510 1370. ** **. *. *. Summary Statistics ================== 419.7 2659 1629 69.6 464 357 47 48 48 page 18 of 98. --A E QWH R ZWAOP ZRAOP Q-K R Q-HR --BWK R ZUH R Z-H R D-AOP DNZ R Q-K R Q-H R QZH R BRHR FHAOP ZVAOP --F-A P Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JKZ R BHK R ZRH R. (cont.).

(20) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample benzo(ghi)perylene (µg/kg) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) CHE (887) TAMPERE (911) SHI (912) WANDSCH (958) LUNLAB (1052) PA2010LAB (1058). NDA mean NDA st dev N Median MAD. 792. 784. 218 279 241 306 256 184 232 204 247 341 * 196 124 * 196 252. 391 470 387 480 518 259 * 420 388 405 148 ** 363 240 * 397 463. 776. MIC. (cont.) 2533 2672 1909 3704 * 3580 996 ** 2508 2399 2740 2550 1700 * 1775 3102 2751. 1607 1761 1341 1933 1900 1178 1775 1620 1300 1250 1190 1071 2107 1638. QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R ZYHR Q-HR QAH R Q-JR TWHR ZWH R. ================= Statistical Results ================= 228.6 419.7 2659 1629 42.8 69.6 464 357 47 47 48 48 230.0 413.5 2635 1663 28.0 49.2 302 250 ====================================================. benzo(k)fluoranthene (µg/kg) ZINDZIWE (1) BOANALHOAG (2) MLABTW (4) AL-West (5) Alconheinr (7) ANM (8) BLAUWHUIS (14) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) EXACT (28) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) ATM (54) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134). NDA mean NDA st dev N. 791. 59 ** 182 158 230 342 ** 162 209 166 221 188 200 190 160 164 222 197 171 200 160 89 * 174 152 138 150 115 169 195 105 183 104 206 127 152 152 166 164. ================= 171.1 35.9 46. 111 325 450 727 284 357 294 382 335 336 370 300 363 409 355 341 340 310 200 310 299 319 316 347 408 301 275 377 212 338 297 337 279 355 289. **. * **. *. *. 2100 803 1604 2100 3400 1866 1982 1403 2712 2011 1660 2100 1880 1613 1839 2230 2190 2040 1790 2800 1473 1827 1865 1896 2134 1553 1870 1640 2228 1195 2012 2017 1370 1749 1875 1332. **. **. *. *. 1400 913 1775 1600 2475 ** 1298 1393 1361 1718 1405 1129 1500 1140 1144 1476 1410 1270 1520 1230 920 979 1251 1131 1087 1282 2505 ** 1370 1050 1366 650 * 1350 1371 1140 1173 1463 933. Summary Statistics ================== 331.2 1874 1306 48.3 340 262 45 46 46 page 19 of 98. --A E QWH R ZWAOP ZRAOP Q-K R Q-HR --BWK R ZUH R Z-H R D-AOP DNZ R Q-K R QZH R BRHR FHAOP ZVAOP --F-A P Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R. (cont.).

(21) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample. 791. benzo(k)fluoranthene (µg/kg) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) TAMPERE (911) SHI (912) WANDSCH (958) LUNLAB (1052) PA2010LAB (1058). NDA mean NDA st dev N. (cont.) 183 118 223 142 165 284 ** 227 156 148 211. 365 326 347 262 335 123 ** 432 * 341 327 480 **. 784. 776. 2547 2530 928 * 1562 1785 1870 1850 1625 2062 2410. 1352 1140 1626 1197 1340 1150 1580 1293 1626 1663. MIC. Q-HR JAHR B-HR ZUH R J-K R Q-HR QAH R Q-JR TWHR ZWH R. ================= Statistical Results ================= 171.1 331.2 1874 1306 35.9 48.3 340 262 46 45 46 46 166.1 335.0 1870 1345 24.0 34.0 230 185 ====================================================. NDA mean NDA st dev N Median MAD. chrysene (µg/kg) ZINDZIWE BOANALHOAG MLABTW AL-West Alconheinr ANM BLAUWHUIS FRIDOLIN HIDU PAULINE RIZA-IMLO ANALGEO EXACT ANATEK ELML WELLAB US LAS CHEMLABSIT ATM 32A HILL ARCHIMEDES GGM ULS COMALAB QSANAL BOREALIS TECHHK EPILAB-1A GAL STCRSC VERITAS RECKENHOLZ THO1808MAS APVROPAVA ORGDIMCH HHAFU CH-SAMEN ECCM LAB607. 792. (1) (2) (4) (5) (7) (8) (14) (15) (16) (18) (20) (21) (28) (29) (33) (35) (39) (48) (52) (54) (56) (58) (59) (60) (61) (67) (76) (78) (79) (87) (91) (92) (101) (108) (110) (112) (120) (134) (469) (841) (862). 117 321 261 300 430 324 411 322 413 414 340 240 613 340 327 336 516 261 1160 400 160 343 392 255 261 272 296 355 325 341 180 368 233 266 299 410 272 330 224 443. *. **. < **. ================= 318.5 80.9 46. 242 767 680 1099 743 894 741 777 775 632 640 1241 820 776 991 672 531 2510 830 410 748 846 776 627 670 698 681 780 786 431 687 622 635 629 782 589 679 619 772. **. *. **. ** *. *. 4300 1495 2662 3800 4538 4075 4402 3436 5144 3593 2990 3400 5400 3830 3497 5041 3740 3530 9220 4080 4400 3362 4100 3996 3709 3532 2823 4600 4240 4658 2851 3760 3648 2787 3585 4204 3050 4864 3990 1934. **. *. **. *. 2300 1418 3984 2600 3751 2649 2770 2756 3173 2730 1870 2300 3963 2070 2630 2628 1850 2110 6890 2910 1600 2205 3100 2504 2317 2235 1678 3060 2750 2781 1838 2221 2553 2045 2242 2982 2027 2482 2550 3569. * *. *. *. **. Summary Statistics ================== 723.3 3811 2508 134.8 766 535 46 47 47 page 20 of 98. --A E QWH R ZWAOP ZRAOP Q-K R Q-HR --BWK R ZUH R Z-H R D-AOP DNZ R Q-K R Q-H R QZH R BRHR FHAOP ZVAOP --F-A P Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR. (cont.).

(22) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample chrysene (µg/kg) CNRLBR LABAMB TAMPERE SHI WANDSCH LUNLAB PA2010LAB. NDA mean NDA st dev N Median MAD. (cont.) (875) (878) (911) (912) (958) (1052) (1058). 792. 239 325 716 ** 380 289 289 377. 521 712 287 ** 884 739 844 885. 784. 776. 2967 3715 4330 3320 3070 5472 * 4281. 2129 2675 2740 2840 2294 3176 2916. MIC. ZUH R J-K R Q-HR QAH R Q-JR TWHR ZWH R. ================= Statistical Results ================= 318.5 723.3 3811 2508 80.9 134.8 766 535 46 46 47 47 325.0 740.0 3760 2600 57.0 95.0 521 365 ====================================================. dibenz(ah)anthracene (µg/kg) BOANALHOAG (2) MLABTW (4) Alconheinr (7) ANM (8) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) ANATEK (29) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) TAMPERE (911) SHI (912) WANDSCH (958) LUNLAB (1052) PA2010LAB (1058). NDA mean NDA st dev N. 791. 44.0 60.0 80.0 63.8 50.3 50.0 82.0 43.6 83.0 59.1 50.0 61.2 100.0 206.0 42.0 60.0 35.0 70.1 51.0 100.0 36.0 51.3 74.0 61.0 50.0 101.0 48.0 57.5 52.4 47.9 79.4 72.6 361.0 35.1 34.0 54.0 62.0 97.8 70.9 24.0 300.0 61.4. <. < * <. <. *. **. *. <. ================= 56.83 17.71 37. 36 92 100 108 85 121 125 74 128 110 80 99 190 204 75 100 74 135 125 128 84 108 122 125 111 181 85 102 93 86 136 111 436 80 49 101 110 43 122 36 300 101. *. * <. *. **. * <. 318 373 590 604 397 698 854 486 674 682 670 580 980 981 519 570 550 411 720 695 625 439 505 590 840 645 794 667 502 362 538 642 547 3081 608 152 574 674 706 673 239 582. *. * *. ** **. *. 362 435 400 413 339 526 537 315 484 842 370 453 760 913 287 410 380 299 460 394 413 352 477 529 525 609 536 462 398 351 473 473 433 1562 335 238 429 485 381 521 215 419. **. ** **. **. *. Summary Statistics ================== 101.8 599.7 423.2 29.4 132.5 93.9 40 42 42. page 21 of 98. QWH R ZWAOP Q-K R Q-HR BWK R ZUH R Z-H R D-AOP DNZ R Q-H R QZH R BRHR FHAOP ZVAOP --Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R Q-HR QAH R Q-JR TWHR ZWH R. (cont.).

(23) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample. 791. 792. 784. 776. MIC. dibenz(ah)anthracene (µg/kg) (cont.) ================= Statistical Results ================= NDA mean 56.83 101.8 599.7 423.2 NDA st dev 17.71 29.4 132.5 93.9 N 37 40 42 42 Median 59.10 101.3 597.0 431.0 MAD 11.80 20.7 88.3 65.0 ==================================================== fluoranthene (µg/kg) ZINDZIWE (1) BOANALHOAG (2) MLABTW (4) AL-West (5) Alconheinr (7) ANM (8) BLAUWHUIS (14) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) EXACT (28) ANATEK (29) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) ATM (54) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) CHE (887) TAMPERE (911) SHI (912) WANDSCH (958) LUNLAB (1052) PA2010LAB (1058). NDA mean NDA st dev N Median MAD. 289 554 464 630 630 515 643 500 672 596 727 600 779 580 639 600 617 607 640 640 320 548 535 397 486 580 690 312 458 535 355 600 492 567 524 652 561 674 432 424 524 553 397 1310 728 488 534 578. *. *. *. *. **. 685 1316 1400 1660 1125 1420 1131 1377 1195 1547 1500 1714 1480 1506 1580 1530 1420 1410 1590 890 1256 1287 1414 1175 1157 2056 891 1435 1281 955 1318 1343 1580 1191 1558 1310 1575 1310 1002 1232 1429 888 427 1870 1455 1266 1489. **. *. ** *. * ** *. 7800 3676 9471 6700 6837 6722 7653 4745 9442 7127 6050 6700 10161 8220 6726 7440 7330 7440 7610 7400 9300 6816 7650 7256 7365 6347 7676 7590 6540 8514 5601 6938 7433 6570 6910 7937 5815 7676 10500 6306 6239 7464 5370 8000 6680 6442 9281 6626. ** *. * *. **. *. **. *. 8100 7347 6977 8200 8822 7634 8728 7973 10400 9807 6800 9100 11900 8630 8151 8780 8640 8520 9570 8970 9100 7445 8550 9112 7347 7505 9781 7560 7600 8553 6393 7110 9140 8210 8196 9293 6023 9853 8950 5203 9210 9211 4700 9440 8340 7955 8438 7461. **. *. **. **. ================= Statistical Results ================= 564.4 1372 7117 8429 107.2 225 891 1069 48 47 48 48 564.0 1377 7293 8479 73.2 153 603 732 ==================================================== page 22 of 98. --A E QWH R ZWAOP ZRAOP Q-K R Q-HR --BWK R ZUH R Z-H R D-AOP DNZ R Q-K R Q-H R QZH R BRHR FHAOP ZVAOP --F-A P Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R ZYHR Q-HR QAH R Q-JR TWHR ZWH R.

(24) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample fluorene (µg/kg) BOANALHOAG MLABTW Alconheinr ANM FRIDOLIN HIDU PAULINE RIZA-IMLO ANALGEO ANATEK ELML WELLAB US LAS CHEMLABSIT 32A HILL ARCHIMEDES GGM ULS COMALAB QSANAL BOREALIS TECHHK EPILAB-1A GAL STCRSC VERITAS RECKENHOLZ THO1808MAS APVROPAVA ORGDIMCH HHAFU CH-SAMEN ECCM LAB607 CNRLBR LABAMB TAMPERE SHI WANDSCH LUNLAB PA2010LAB. NDA mean NDA st dev N Median MAD. 791. (2) (4) (7) (8) (15) (16) (18) (20) (21) (29) (33) (35) (39) (48) (52) (56) (58) (59) (60) (61) (67) (76) (78) (79) (87) (91) (92) (101) (108) (110) (112) (120) (134) (469) (841) (862) (875) (878) (911) (912) (958) (1052) (1058). 34.0 60.0 < 90.0 62.2 72.7 74.0 82.0 63.2 85.0 136.7 ** 80.0 78.8 100.0 77.4 57.0 90.0 41.0 82.5 59.0 100.0 < 61.0 53.1 79.0 51.0 52.0 67.0 63.0 53.0 45.0 50.4 83.4 75.9 87.6 50.3 64.0 57.7 78.0 82.7 67.3 35.0 91.0 61.8. 54 96 120 103 126 147 123 93 128 197 * 130 135 140 132 84 160 69 122 114 100 < 110 87 124 92 80 108 89 99 80 88 134 132 142 79 122 100 136 50 * 113 64 156 121. 784. 139 8929 250 247 226 217 351 201 227 429 290 236 250 270 212 300 154 161 260 275 260 179 190 285 240 192 169 229 201 170 210 278 258 277 274 262 175 236 205 268 164 341 224. 776. **. *. **. *. 7814 199 8000 9150 9765 7340 9971 8506 5330 13050 1130 7387 11130 6930 7240 9460 8600 7314 9435 15013 4783 7344 6214 8830 9200 6994 6772 8001 8153 7685 7689 8552 8064 9018 11200 8025 7681 8710 9610 8650 8922 8409 6965. MIC. **. * ** ** *. ** *. *. QWH R ZWAOP Q-K R Q-HR BWK R ZUH R Z-H R D-AOP DNZ R Q-H R QZH R BRHR FHAOP ZVAOP --Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK Z BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R Q-HR QAH R Q-JR TWHR ZWH R. ================= Statistical Results ================= 68.28 111.9 232.4 8183 19.99 30.5 52.1 1249 40 41 43 43 67.15 114.0 236.0 8064 14.08 20.8 35.5 858 ====================================================. indeno(1,2,3-cd)pyrene (µg/kg) ZINDZIWE (1) BOANALHOAG (2) MLABTW (4) AL-West (5) Alconheinr (7) ANM (8) BLAUWHUIS (14) FRIDOLIN (15). NDA mean NDA st dev N. 792. 52 * 346 243 280 226 195 210. ================= 239.9 66.3 48. 108 ** 648 * 420 351 371 245 *. 3500 1432 * 2568 2400 1626 2302 2478. 3200 ** 1387 3298 ** 1600 1297 1523 1550. Summary Statistics ================== 420.4 2746 1683 81.2 645 371 47 48 48 page 23 of 98. --A E QWH R ZWAOP ZRAOP Q-K R Q-HR --BWK R. (cont.).

(25) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample indeno(1,2,3-cd)pyrene (µg/kg) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) EXACT (28) ANATEK (29) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) ATM (54) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) CHE (887) TAMPERE (911) SHI (912) WANDSCH (958) LUNLAB (1052) PA2010LAB (1058). NDA mean NDA st dev N Median MAD naphtalene (µg/kg) ZINDZIWE (1) BOANALHOAG (2) MLABTW (4) AL-West (5) Alconheinr (7) ANM (8) BLAUWHUIS (14) FRIDOLIN (15) HIDU (16) PAULINE (18). NDA mean NDA st dev N. 791. 792. (cont.) 254 314 270 300 210 252 190 276 296 320 334 280 220 115 292 193 194 216 182 350 308 157 227 236 301 202 220 230 253 252 508 ** 180 144 203 162 363 343 211 203 185 281. 474 500 447 480 370 501 410 440 577 431 580 460 380 250 487 355 475 380 336 735 564 365 432 461 437 411 412 398 450 385 678 441 227 369 333 576 144 398 375 354 487. 784. *. **. ** *. **. 3124 4016 2834 2690 2700 3165 2770 2714 3632 3180 3840 3050 2390 2000 2163 2589 2948 2819 2512 3619 3430 2380 3520 2081 3219 2520 2593 2671 4507 * 1923 5125 ** 3220 754 ** 2222 2215 3910 2730 1770 2965 2695 3042. 776. 1995 2139 1911 1744 1700 3419 ** 1460 1787 2334 2050 1800 2120 1580 1220 1323 1764 1792 1413 1718 2678 * 2250 1400 1715 1335 1994 1708 1768 1634 2326 1441 3244 ** 1560 1151 1574 1523 1860 1350 1350 1974 1909 1835. MIC. ZUH R Z-H R D-AOP DNZ R Q-K R Q-H R QZH R BRHR FHAOP ZVAOP --F-A P Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R ZYHR Q-HR QAH R Q-JR TWHR ZWH R. ================= Statistical Results ================= 239.9 420.4 2746 1683 66.3 81.2 645 371 48 47 48 48 233.0 420.0 2707 1731 45.0 55.0 437 264 ====================================================. 45 149 65 190 121 118 207 123 152 ================= 139.7 56.2 45. 53 164 140 127 100 232 153 146. 360 127 1750 ** 400 372 366 632 667 476. 2200 1366 326 2300 2469 2028 3314 2813 2297. Summary Statistics ================== 153.3 442.0 2382 66.0 217.2 1028 45 46 46 page 24 of 98. --A E QWH R ZWAOP ZRAOP Q-K R Q-HR --BWK R ZUH R Z-H R. (cont.).

(26) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample. 791. 792. naphtalene (µg/kg) (cont.) RIZA-IMLO (20) EXACT (28) ANATEK (29) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) ATM (54) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) CHE (887) TAMPERE (911) SHI (912) WANDSCH (958) PA2010LAB (1058). 159 120 263 200 170 303 286 118 140 230 100 120 140 109 100 250 221 210 59 182 109 161 181 130 147 314 165 107 87 103 183 122 30 97 104 38 158. 189 120 265 210 176 311 * 270 98 120 250 110 130 146 174 124 279 250 233 68 251 112 201 231 151 138 333 * 180 62 120 147 163 135 44 89 115 44 222. NDA mean NDA st dev N Median MAD phenanthrene (µg/kg) ZINDZIWE (1) BOANALHOAG (2) MLABTW (4) AL-West (5) Alconheinr (7) ANM (8) BLAUWHUIS (14) FRIDOLIN (15) HIDU (16) PAULINE (18) RIZA-IMLO (20) ANALGEO (21) EXACT (28) ANATEK (29). NDA mean NDA st dev N. *. * *. <. **. 784. 776. 676 390 810 650 443 803 1020 * 268 300 690 400 341 310 478 402 773 797 716 181 589 353 503 569 454 340 1052 * 551 235 314 270 502 423 169 250 323 155 670. 3479 2300 4405 3130 2321 3729 4180 1520 2120 3640 2000 1996 1844 3310 1263 3667 3899 3460 850 3642 1918 2532 3245 2223 2000 4994 * 2552 1590 1840 1463 2873 1985 624 1620 2280 1002 2553. MIC. D-AOP Q-K R Q-H R QZH R BRHR FHAOP ZVAOP --F-A P Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R ZYHR Q-HR QAH R Q-JR ZWH R. ================= Statistical Results ================= 139.7 153.3 442.0 2382 56.2 66.0 217.2 1028 45 45 46 46 140.0 147.0 432.8 2299 37.0 42.3 146.3 694 ====================================================. 136 * 286 185 360 281 237 319 322 303 354 438 * 290 492 ** ================= 292.6 56.6 47. 185 ** 383 400 362 316 414 453 368 377 503 * 400 574 **. 2900 1392 ** 27465 ** 2700 2671 2351 2800 2984 3416 3290 2680 2900 3872 **. 24000 23010 2690 ** 26000 28170 22920 27000 24420 30330 28040 17600 * 25000 28990. Summary Statistics ================== 393.9 2804 24889 50.0 310 3280 46 47 47 page 25 of 98. --A E QWH R ZWAOP ZRAOP Q-K R Q-HR --BWK R ZUH R Z-H R D-AOP DNZ R Q-K R Q-H R. (cont.).

(27) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample. 791. 792. 784. 776. phenanthrene (µg/kg) (cont.) ELML (33) WELLAB (35) US (39) LAS (48) CHEMLABSIT (52) ATM (54) 32A (56) HILL (58) ARCHIMEDES (59) GGM (60) ULS (61) COMALAB (67) QSANAL (76) BOREALIS (78) TECHHK (79) EPILAB-1A (87) GAL (91) STCRSC (92) VERITAS (101) RECKENHOLZ (108) THO1808MAS (110) APVROPAVA (112) ORGDIMCH (120) HHAFU (134) CH-SAMEN (469) ECCM (841) LAB607 (862) CNRLBR (875) LABAMB (878) TAMPERE (911) SHI (912) WANDSCH (958) LUNLAB (1052) PA2010LAB (1058). 330 366 310 413 275 320 340 179 258 242 256 239 348 308 302 240 326 225 334 280 266 242 409 270 443 268 252 280 318 313 275 165 342 273. 400 480 390 483 351 410 420 260 374 334 401 353 453 433 404 415 441 367 415 393 367 338 539 367 348 416 354 376 442 243 360 221 431 423. 2800 2616 2830 3590 2640 3000 2960 2000 2548 2914 3100 3099 2775 3192 2990 2340 3349 2153 2754 3082 2480 2643 3359 2602 2584 3800 2602 2643 2809 2750 2810 2165 4298 2891. 27600 23140 32090 26700 22500 27940 26210 28000 24230 26500 24910 17610 22490 15020 25200 24500 28440 22500 23920 25550 22430 23810 23250 19990 22220 35000 15170 28700 26750 32400 22200 23260 20480 23990. NDA mean NDA st dev N. *. * *. *. *. *. ** **. *. *. *. **. * **. *. * **. ** *. *. QZH R BRHR FHAOP ZVAOP --F-A P Z-HS ZXHR Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R Q-HR QAH R Q-JR TWHR ZWH R. ================= Statistical Results ================= 292.6 393.9 2804 24889 56.6 50.0 310 3280 47 46 47 47 290.0 396.7 2809 24421 38.0 34.5 207 2199 ====================================================. NDA mean NDA st dev N Median MAD. pyrene (µg/kg) BOANALHOAG MLABTW Alconheinr ANM FRIDOLIN HIDU PAULINE RIZA-IMLO ANALGEO ANATEK ELML WELLAB US LAS CHEMLABSIT 32A HILL. *. MIC. (2) (4) (7) (8) (15) (16) (18) (20) (21) (29) (33) (35) (39) (48) (52) (56) (58). 203 402 500 541 525 496 10 526 598 699 490 503 520 553 405 540 250. *. < **. *. *. ================= 457.6 96.3 41. 530 ** 1076 1300 1490 1380 1472 1124 1075 1294 1666 * 1280 1249 1440 1350 982 1390 720 *. 2595 ** 5880 5100 5298 5309 4971 7191 * 5618 4640 8174 ** 6530 5091 5930 5920 5760 5760 6700. 4352 5130 5500 5886 6028 6386 6519 5983 4660 8629 ** 4970 5534 6060 6890 4590 6190 5700. Summary Statistics ================== 1179 5494 5624 187 702 816 42 43 43 page 26 of 98. QWH R ZWAOP Q-K R Q-HR BWK R ZUH R Z-H R D-AOP DNZ R Q-H R QZH R BRHR FHAOP ZVAOP --Z-HS ZXHR. (cont.).

(28) SETOC 2012.1 - Polycyclic aromatic hydrocarbons Sample pyrene (µg/kg) ARCHIMEDES GGM ULS COMALAB QSANAL BOREALIS TECHHK EPILAB-1A GAL STCRSC VERITAS RECKENHOLZ THO1808MAS APVROPAVA ORGDIMCH HHAFU CH-SAMEN ECCM LAB607 CNRLBR LABAMB TAMPERE SHI WANDSCH LUNLAB PA2010LAB. NDA mean NDA st dev N Median MAD. 791 (cont.) (59) (60) (61) (67) (76) (78) (79) (87) (91) (92) (101) (108) (110) (112) (120) (134) (469) (841) (862) (875) (878) (911) (912) (958) (1052) (1058). 421 332 374 413 583 310 378 420 303 478 388 485 392 534 472 521 399 412 427 436 1230 ** 578 402 433 472. 792. 1092 1177 1162 995 1835 ** 854 1150 1197 814 1101 1061 1425 971 1253 1157 1134 1180 1062 1033 1125 423 ** 1570 * 1265 1053 1261. 784. 5268 6226 5652 5861 4741 6082 5790 4940 6441 4480 5383 5354 5114 5021 6091 4818 6368 8140 ** 5398 4705 5493 6400 5100 4791 7348 * 5101. 776. 5001 6348 6730 5150 4718 7567 * 5170 5000 5189 4333 5067 5740 6040 5651 6244 4389 5937 6300 5347 5735 5903 6710 5870 5445 5813 4939. ================= Statistical Results ================= 457.6 1179 5494 5624 96.3 187 702 816 41 42 43 43 471.5 1160 5493 5735 66.5 124 472 565 ====================================================. page 27 of 98. MIC. Z-H R ZVZ R Q-H R BZHR Z-H R --Q-HR QWHJA A-H R J-J R JZK R BHK R ZRH R QWA P ZZZ R QRH R Q-HR JAHR B-HR ZUH R J-K R Q-HR QAH R Q-JR TWHR ZWH R.

(29) SETOC 2012.1 - Polychlorobiphenyls Sample PCB 028 (µg/kg) ZINDZIWE MLABTW AL-West Alconheinr ANM BLAUWHUIS FRIDOLIN HIDU PAULINE RIZA-IMLO ANALGEO EXACT ANATEK ELML WELLAB US JYUIER LAS HILL ARCHIMEDES GGM ULS QSANAL BOREALIS EPILAB-1A GAL STCRSC VERITAS RECKENHOLZ THO1808MAS ORGDIMCH HHAFU ECCM LAB607 CNRLBR LABAMB TLR TAMPERE WANDSCH PA2010LAB. (1) (4) (5) (7) (8) (14) (15) (16) (18) (20) (21) (28) (29) (33) (35) (39) (41) (48) (58) (59) (60) (61) (76) (78) (87) (91) (92) (101) (108) (110) (120) (134) (841) (862) (875) (878) (900) (911) (958) (1058). N Median MAD. 792. 784. 22.7 12.8 21.0 37.2 5.0 10.4 9.0 7.4 12.8 22.0 1.0 24.0 2.0 11.7 20.9 13.7 19.8 8.9 26.6 25.5 5.7 1.0 13.1 10.0 5.0 5.9 10.0 0.5 14.3 9.3 6.1 10.9 19.8 15.5 10.4 12.5 2.3 10.0 15.5. 8.43 5.90 0.50 0.80 3.68 2.00 1.00 2.67 2.50 1.00 13.03 2.00 4.68 7.94 2.50 6.34 2.80 10.50 7.78 8.01 12.00 6.68 5.00 5.00 1.73 10.00 0.50 4.10 3.75 1.00 2.67 14.49 3.33 6.12 3.24 7.10 10.00 5.12. 2.000 3.500 2.000 0.500 0.800 0.330 2.000 1.000 0.500 0.400 1.000 2.870 2.000 2.000 0.700 0.500 0.300 1.100 20.000 2.000 1.000 1.000 0.890 5.000 1.000 0.370 10.000 0.500 0.500 0.261 8.000 0.321 1.370 0.500 1.000 1.000 1.400 10.000 0.330. **. < <. < < < < <. <. < <. <. < * <. * <. < <. < *. <. 776. < < < < ** < < < ** < < < < < < < < < < < <. ** ** < < < ** <. 10.0 20.5 2.0 0.5 11.0 9.6 8.0 11.1 12.0 21.0 1.0 25.1 2.0 12.4 18.7 11.2 16.9 10.9 20.0 23.2 10.7 34.0 11.9 10.0 10.0 6.0 10.0 0.5 12.6 13.8 6.6 11.3 19.7 13.2 8.4 8.0 7.4 10.0 12.8. MIC. ** <* < **. ** < ** ** <* *. < ** **. --HCE ZZK R ZZH R Q-K R Q-HR --BWK R ZUH Q Z-H R DUI Q ZNH Q QRK R Q-H R QZH R BKZQ FHJ Q ZZI Q ZUH R ZXHR Z-H R ZVZ R JRH R ZWH R CYH Q. <. < < **. *. <. JXH Q JAH Q JZK R BRK R ZZJ Q ZZZ R QUH R BHHR BRHR ZUH R J-K R DRKR Q-HR ZUJQ BUH R. ================= Statistical Results ================= 13.40 5.065 0.4245 10.93 7.82 3.325 0.2703 3.11 31 28 16 30 12.78 5.060 0.5000 11.61 5.41 2.324 0.2000 2.10 ====================================================. NDA mean NDA st dev N Median MAD. PCB 031 (µg/kg) HILL ORGDIMCH LABAMB TLR. 791. (58) (120) (878) (900). 10.20 7.91 7.02 13.90. 5.80 491.00 3.40 3.20. 1.100 < 0.133 1.000 < 1.000 <. 10.10 7.10 5.85 7.90. ============= Statistical Results (no NDA) ============= 4 4 1 4 9.057 4.600 0.1330 7.502 1.590 1.300 1.025 ====================================================. page 28 of 98. ZXHR ZZZ R J-K R DRKR.

(30) SETOC 2012.1 - Polychlorobiphenyls Sample PCB 052 (µg/kg) ZINDZIWE MLABTW AL-West Alconheinr ANM BLAUWHUIS FRIDOLIN HIDU PAULINE RIZA-IMLO ANALGEO EXACT ANATEK ELML WELLAB US JYUIER LAS HILL ARCHIMEDES GGM ULS QSANAL BOREALIS EPILAB-1A GAL STCRSC VERITAS RECKENHOLZ THO1808MAS ORGDIMCH HHAFU ECCM LAB607 CNRLBR LABAMB TLR TAMPERE WANDSCH PA2010LAB. (1) (4) (5) (7) (8) (14) (15) (16) (18) (20) (21) (28) (29) (33) (35) (39) (41) (48) (58) (59) (60) (61) (76) (78) (87) (91) (92) (101) (108) (110) (120) (134) (841) (862) (875) (878) (900) (911) (958) (1058). N Median MAD. 792. 784. 9.73 11.47 14.00 25.10 6.08 9.19 7.00 7.82 11.12 17.00 9.50 19.03 10.40 8.44 10.18 11.35 10.50 8.10 17.37 8.40 4.42 15.00 11.50 10.00 5.00 2.84 10.00 10.31 10.60 8.45 3.90 8.81 11.30 10.30 8.34 8.72 2.20 10.00 6.99. 3.19 7.40 30.10 2.69 3.01 3.00 42.20 3.53 2.10 4.70 46.04 2.30 2.00 3.36 3.26 3.46 4.70 1.00 3.15 4.17 21.00 16.40 5.00 2.00 1.05 10.00 3.34 4.78 3.02 5.60 3.11 4.76 3.49 6.14 2.17 8.00 10.00 2.23. 2.000 3.500 2.000 7.340 0.800 0.400 1.000 1.000 0.898 0.500 1.400 14.130 7.400 2.000 0.700 0.500 0.270 1.100 20.000 2.000 2.000 6.000 5.950 5.000 1.000 0.300 10.000 0.610 1.400 0.319 13.200 0.423 1.260 0.590 1.140 1.000 1.500 10.000 0.200. **. ** **. ** * * < < * <. *. * <. * **. **. ** <. <. ** ** <. <. * <. < < < ** < < <. ** ** < < < < < < ** ** < < <. **. < <. 776. MIC. 12.0 19.1 19.0 50.2 14.2 17.3 15.0 14.8 20.9 30.0 19.0 50.7 35.0 14.0 16.8 17.5 20.5 18.7 20.0 17.1 16.3 28.0 21.4 10.6 15.0 6.0 10.0 20.0 15.2 18.1 13.2 17.4 19.3 18.2 17.8 11.6 17.9 10.0 12.2. --HCE ZZK R ZZH R Q-K R Q-HR. **. ** ** **. <. *. * <. <. BWK R ZUH Q Z-H R DUI Q ZNH Q QRK R Q-H R QZH R BKZQ FHJ Q ZZI Q ZUHR ZXHR Z-H R ZVZ R JRH R ZWH R CYH Q JXH Q JAH Q JZK R BRK R ZRH Q ZZZ R QUH R BHHR BRHR ZUH R J-K R Q-HR ZUJQ BUH R. ================= Statistical Results ================= 9.430 3.401 0.7229 16.91 2.413 1.685 0.7761 3.73 35 33 22 36 9.725 3.460 1.0190 17.64 1.625 1.240 0.6075 2.64 ====================================================. NDA mean NDA st dev N Median MAD. PCB 077 (µg/kg) ELML WELLAB HILL EPILAB-1A ORGDIMCH LABAMB PA2010LAB. 791. (33) (35) (58) (87) (120) (878) (1058). 2.000 2.000 1.000 0.810 1.000 1.000 0.860. < < <. <. 2.000 2.000 1.000 0.170 0.154 1.000 0.100. < < <. <. 2.0000 2.0000 1.1000 0.0370 0.0345 1.0000 0.5000. < < <. <. 2.90 2.00 < 2.50 2.10 2.32 3.11 2.53. ============= Statistical Results (no NDA) ============= 3 3 3 6 0.8600 0.1535 0.03700 2.515 0.0500 0.0165 0.00250 0.291 ====================================================. page 29 of 98. QZH R. ZZZ R J-K R BUH R.

(31) SETOC 2012.1 - Polychlorobiphenyls Sample PCB 081 (µg/kg) HILL EPILAB-1A ORGDIMCH LABAMB PA2010LAB. 791. (58) (87) (120) (878) (1058). NDA mean NDA st dev N Median MAD. 1.0000 < 0.0160 0.0090 1.0000 < 0.3000. 784. 1.00000 < 0.00400 0.00500 1.00000 < 0.17000. 776. 1.10000 < 0.00100 0.00100 1.00000 < 0.10000 <. MIC. 1.0000 < 0.0230 0.0470 1.0000 < 0.3000. ZZZ R J-K R BUH R. ============= Statistical Results (no NDA) ============= 3 3 2 3 0.01600 0.005000 0.001000 0.04700 0.00700 0.001000 0.02400 ====================================================. N Median MAD. PCB 101 (µg/kg) ZINDZIWE MLABTW AL-West Alconheinr ANM BLAUWHUIS FRIDOLIN HIDU PAULINE RIZA-IMLO ANALGEO EXACT ANATEK ELML WELLAB US JYUIER LAS HILL ARCHIMEDES GGM ULS QSANAL BOREALIS EPILAB-1A GAL STCRSC VERITAS RECKENHOLZ THO1808MAS ORGDIMCH HHAFU ECCM LAB607 CNRLBR LABAMB TLR TAMPERE WANDSCH PA2010LAB. 792. (1) (4) (5) (7) (8) (14) (15) (16) (18) (20) (21) (28) (29) (33) (35) (39) (41) (48) (58) (59) (60) (61) (76) (78) (87) (91) (92) (101) (108) (110) (120) (134) (841) (862) (875) (878) (900) (911) (958) (1058). 12.4 11.8 14.0 16.6 7.4 13.1 10.0 8.1 12.4 10.0 12.0 13.3 8.1 10.9 10.7 12.1 12.2 1.7 19.3 11.4 7.0 14.0 10.8 10.0 5.0 5.9 4.0 9.7 11.4 13.8 4.0 12.0 10.5 13.6 12.4 9.2 3.6 10.0 7.4. ** *. < <* *. *. * <. 4.17 4.80 5.63 3.53 4.31 4.00 62.20 4.42 4.00 5.00 3.30 2.80 4.08 4.93 4.15 4.56 1.00 7.20 3.94 6.07 7.00 4.17 5.00 3.00 1.19 4.00 4.04 4.84 4.93 2.90 5.02 6.51 4.70 6.76 3.42 7.80 10.00 3.05. **. < ** *. * < *. * * ** <. 2.00 3.50 2.00 3.70 1.24 1.59 1.00 1.56 1.89 1.40 6.40 1.87 2.00 2.00 2.28 1.20 1.24 1.10 20.00 2.00 2.00 4.00 1.36 5.00 1.00 1.28 10.00 1.55 1.60 1.71 13.10 1.77 1.00 1.79 1.81 1.40 2.40 10.00 0.53. < < < **. <. ** < <. < < < < ** < < <. ** <. * < *. 12.0 12.0 19.0 27.6 17.9 25.7 15.0 8.7 21.8 19.0 23.0 18.5 13.6 17.7 17.5 19.6 24.2 4.4 20.0 21.6 17.7 31.0 23.2 13.8 14.0 12.1 6.5 18.4 20.3 18.6 12.2 22.3 21.9 21.8 18.2 17.4 16.2 10.0 13.5. <. * <. *. *. <. ================= Statistical Results ================= 11.09 4.285 1.575 18.25 2.92 1.032 0.387 5.25 36 35 24 36 11.14 4.310 1.655 18.29 1.96 0.690 0.275 3.60 ====================================================. page 30 of 98. --HCE ZZK R ZZH R Q-K R Q-HR --- Z BWK R ZUH Q Z-H R DUI Q ZNH Q QRK R Q-H R QZH R BKZQ FHJ Q ZZI Q ZUH R ZXHR Z-H R ZVZ R JRH R ZWH R CYH Q JXH Q JAH Q JZK R BRK R QZJ Q ZZZ R QUH R BHHR BRHR ZUH R J-K R DRKR Q-HR ZUJQ BUH R.

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