REPORT 23/12/2011 N DRC B

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1 REPORT 23/12/2011 N DRC B Analytical Proficiency Tests relating to measurements of hydrochloric acid, hydrofluoric acid, ammonia, sulphur dioxide, mercury, and metals (and metalloids) in samples coming from stationary source emissions. FINAL REPORT

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3 ANALYTICAL INTER-LABORATORY COMPARISONS ORGANIZED FOR THE LABORATORIES INVOLVED IN REGULATORY EMISSIONS CHECKS Campaign : HCl, HF, NH 3, SO 2, total Hg, Heavy metals FINAL REPORT D R C B D E C E M B E R 23, Sylvain BAILLEUL Characterization of the Environment Department Chronic Risks Division List of persons having taken part in the study : S. BAILLEUL, H. BIAUDET, F. DEL-GRATTA, J. POULLEAU, L. MEUNIER, B. DEFRENNE DRC B Page 3 sur 171

4 FOREWORD This report was drawn up on the basis of the information provided to INERIS and the objective (scientific or technical) data available and applicable regulations. INERIS cannot be held liable if the information received was incomplete or erroneous. Any findings, recommendations, suggestions or equivalent that are recorded by INERIS as part of the services it is contracted to perform may assist with decision making. Given the tasks entrusted to INERIS on the basis of the decree founding the organization, INERIS cannot be involved in the decision making process itself. INERIS cannot therefore take responsibility in lieu and place of the decision maker. The addressee shall use the results comprised in this report in whole or at least in an objective manner. Using this information in the form of excerpts or summary memos may take place only under the full and complete responsibility of the addressee. The same applies to any modification made to this report. INERIS declines any liability for any use of this report outside of the scope of the service provided. Drafting Checking Approval Name Sylvain BAILLEUL Florence DEL-GRATTA Nicolas ALSAC Quality Coordinator of the Proficiency Test «Analytical resources unit» Chronic Risks Division Coordinator of the Proficiency Test «Sources and Emissions unit» Chronic Risks Division Head of Characterization of the Environment Department Chronic Risks Division Signature DRC B Page 4 sur 171

5 TABLE OF CONTENTS 1 GLOSSARY DEFINITIONS REFERENCE DOCUMENTS CLIENTS ORGANIZATION OF THE INTER-LABORATORY COMPARISONS PRESENTATION OF THE REPORT INTRODUCTION ILT PROGRAM TEST PARTICIPANTS DESCRIPTION OF THE TEST MATERIALS DESCRIPTION AND INSTRUCTIONS Total mercury in permanganate medium Total mercury in dichromate medium Hydrochloric acid Fluorhydric acid Metals (and metalloids) Sulfur dioxide Ammonia SHIPPING HOMOGENEITY AND STABILITY OF THE SAMPLES HOMOGENEITY OF THE MATERIALS STABILITY OF THE TEST MATERIALS RESULTS OF THE INTER-LABORATORY COMPARISON EXPLOITATION OF THE DATA FROM THE TEST MATERIALS General information Presentation of the results Test material "11/119507_Hg_KMnO 4" Test material "11/119507_Hg_K 2Cr 2O 7" Test material "11_119507_HCl" Test material "11_119507_HF_Solution" Test material "11_119507_HF_Poussière" Test material "11/119507_Metaux_solution" Test material "11/119507_Metaux_Poussiére" free protocol Test material "11/119507_Métaux_Poussiére" imposed protocol Test material "11_119507_SO 2" Test material "11_119507_NH 3" LIST OF ANNEXES ANNEX 1 GENERAL ORGANIZATION, DESCRIPTION OF TESTS AND ALGORITHMS General organization of the test Prior checking of the data before launching statistical calculations Materials prepared by the INERIS : Statistical performance tests ANNEX 2 DATA RECEIVED, AVERAGES AND REPEATABILITY STANDARD DEVIATIONS FOR THE LABORATORIES AND VALUES DISMISSED BY EXPERT OPINION Table HCl Water Hydrochloric acid Raw data in mg/liter Table HF Sodium hydroxide (NaOH) Fluorhydric Acid - Raw data in mg/liter Table HF Dust Fluorhydric Acid Raw data in mg/g Table NH3 Sulfuric acid - Ammonia Raw data in mg/liter Table SO2 Hydroperoxide Sulfur dioxide Raw data in mg/liter Table Hg_ K2Cr2O7 Nitric acid - Dichromate (HNO3-K2Cr2O7) - Mercury Raw data in µg/liter Table Hg_KMnO4 Sulfuric acid - Permanganate (H2SO4-KMnO4) - Mercury Raw Data in µg/liter.. 88 Tables 8 to Metals_solution Raw data in µg/liter DRC B Page 5 sur 171

6 Tables 19 to Metals Dust Free protocol Raw Data in µg/g Table 30 à Metals Dust Imposed protocol- Raw Data in µg/g ANNEX 3 STATISTICAL DISTRIBUTION CURVES HF Acide Fluorhydrique HF Poussière - Acide Fluorhydrique NH3 Ammoniac SO2 Dioxyde de soufre Hg K2Cr2O7 - Mercure Hg_KMnO4 - Mercure Métaux_solution (11 figures) Métaux Poussière Protocole libre (11 figures) Métaux Poussière Protocole imposé (11 figures) ANNEX 4 GENERAL ORGANIZATION, DESCRIPTION OF TESTS AND ALGORITHMS Figure 1 : 11/119507_Métaux solution (part 1 to 3) Figure 2: 11/119507_Métaux poussière Free Protocol (part 1 to 3) Figure 3: 11/119507_Métaux poussière Imposed Protocole (part 1 to 2) DRC B Page 6 sur 171

7 1 GLOSSARY ILC ILT Extract QL Test material Matrix CRM ILCA Spiking solution Assigned value An Inter-Laboratory Comparison is defined and implemented to allow the laboratories to assess and demonstrate their performance in particular test, calibration or measuring sectors, An Inter-Laboratory Test is a technical operation that consists of determining the concentration of a sample, according to a specific operating mode, using comparisons between different laboratories; it makes it possible to assess laboratories performance, NOTE: Three terms may be used: inter-laboratory tests or inter-comparison tests or aptitude tests, Obtained either from extracted water, or from a solvent spiked by all of the sought substances, Quantification limit, Matrix of interest containing the element subject to the interlaboratory comparison, potentially added using a spiking solution. The test matrices are also called, in the referential, LAB-CIL REF 02, comparison substrate, Natural element, physical element as well as all of its components other than the species to be analyzed in which the substance subject to the inter-laboratory test is placed, Certified reference material, Inter-laboratory comparison analyzer, Concentration solution with known substance(s) dissolved in a solvent, Value assigned to a particular and recognized size, sometimes by convention, as having a suitable uncertainty at a given usage (ISO 13528). DRC B Page 7 sur 171

8 2 DEFINITIONS CV r CV R CV rep Standard deviation Population standard deviation IC R IC r Average Population average Number of decimals : standard deviation of the x measurements divided by the average of those x measurements by % [(Standard deviation / average) by %], : reproducibility variation coefficient equal to the standard deviation of the averages of the measurements divided by the average of the averages of the measurements by %, : mean repeatability variation coefficient, average of the CV 4 of the participants, : standard deviation of x measurements, : standard deviation of the measurement averages, : reproducibility confidence interval, : repeatability confidence interval, : average of x measurements, : average of the measurement averages, : number imposed in the instruction formula, σ : robust standard deviation for assessing the aptitude (stipulated, perceived or s*: robust standard deviation for evaluating the aptitude obtained using the algorithm A), z score : performance criteria provided to each participant making it possible to measure its deviation relative to the assigned value. The assigned value is the robust average, s* : robust standard deviation for assessing the aptitude obtained using the algorithm A, S L : inter-laboratory standard deviation, S R : reproducibility standard deviation, S r : repeatability standard deviation, u x* : standard uncertainty u x, U XMRC : standard uncertainty resulting from the certificate for the certified test material, w* : robust standard deviation obtained using algorithm S, x* : robust average obtained using algorithm A, X MRC : reference value resulting from the certificate for the certified reference material. DRC B Page 8 sur 171

9 3 REFERENCE DOCUMENTS Decree of March 11, 2010 : Decree pertaining to approval terms for laboratories or entities for certain types of samples and analyses upon the emission of substances into the atmosphere (NOR: DEVE A) LAB-CIL REF 02 : COFRAC (French organism of accreditation) reference document relative to the organizers of inter-laboratory comparisons Accreditation requirements Revision 03 March 2011, LAB REF 22 : COFRAC reference document relative to specific requirements Air quality Emissions from fixed sources Revision 00 June 2009, EN ISO/CEI : general requirements concerning aptitude tests April 2010, ISO : applications of the statistics Accuracy (correctness and faithfulness) of the results and measurement methods Part 1: general principles and definitions December 1994, ISO : application of the statistics Accuracy (correctness and faithfulness) of the measurement results Part 2: basic method for determining the repeatability and reproducibility of a standardized measurement method December 1994, ISO : application of the statistics Accuracy (correctness and faithfulness) of the measurement results Part 5: alternative methods for determining the faithfulness of a standardized measurement method December 1998, ISO : statistical methods used in aptitude tests by inter-laboratory comparisons December 2005, ISO : vocabulary and symbols Part 2: Applied statistics December 2006, NF X : application of the statistics Study of the normality of a distribution December DRC B Page 9 sur 171

10 4 CLIENTS Laboratories having participated in the inter-laboratory comparison. 5 ORGANIZATION OF THE INTER-LABORATORY COMPARISONS The inter-laboratory comparisons (ILC) were organized and implemented by the authorized personnel cited in table 1 below: Organization of the "Air" inter-laboratory comparisons INERIS Parc Technologique Alata VERNEUIL- EN-HALATTE First and Last Names Eva LEOZ Sylvain BAILLEUL Sylvain BAILLEUL José GUARNERI ILCA Function ILT Steering ILT coordinator Test material preparer Website management Design of the statistical processing tool 6 PRESENTATION OF THE REPORT This report cancels and replaces the initial provisional report referenced DRC A distributed on 07/11/2011. It is accessible on the site 7 INTRODUCTION These tests were organized by the INERIS according to a program developed in agreement with the Steering Committee for the tests bringing together three experts designated by the MEDDTL (Ministry of Ecology, Sustainable Development, Transportation and Housing), members of the Laboratory or Entity Approval Committee for the performance of certain types of sampling and analyses upon emission of substances into the atmosphere. One of the purposes of these tests is to determine the analytical repeatability and reproducibility standard deviations obtained in the implementation of the reference methods defined by the aforementioned decree and detecting any bias or factors influencing the measuring quality. Participation in these inter-laboratory tests was mandatory for the approved laboratories. Outside this regulatory context, participation in inter-laboratory tests is an essential tool in monitoring the mastery of the implementation of chemical analysis methods. To that end, it is subject to a COFRAC requirement in the context of accreditation according to referential EN ISO/CEI and leads to verification of the proper execution of this requirement during evaluations. DRC B Page 10 sur 171

11 Until now, participation in these inter-laboratory tests has been dedicated to companies/laboratories carrying out emission controls on stacks in France for regulatory purposes, for which an agrément from the ministry in charge of environment is necessary. This year, INERIS has decided to extend the participation to any European laboratory willing to take part. 8 ILT PROGRAM In 2011, the analytical inter-laboratory comparisons in the air field pertained to the analyses of parameters relative to approvals 3b, 4b, 5b, 6b, 10b and 16b of the decree dated March 11, 2010 by the Ministry of Ecology, Energy, Sustainable Development and the Sea pertaining to approval terms for laboratories or entities to perform certain types of samples and analyses upon the emission of substances into the atmosphere. The concerned substances were : mercury (Hg) gas, hydrochloric acid (HCl) gas, fluorhydric acid (HF) gas and particles, metals gases and particles: arsenic (As), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), manganese (Mn), nickel (Ni), lead (Pb), antimony (Sb), thallium (Tl), vanadium (V), sulfur dioxide (SO 2 ), ammonia (NH 3 ). The annual program for these analytical inter-laboratory comparisons (M1540AB_11_119507») was developed in cooperation with the advisory group. This group is made up at least of technical experts competent on the matrix, the analysis methods, and an expert of recognized skill in statistical data processing. The general organization of the inter-laboratory comparison and the different statistical processing procedures are presented in annex 1 of this report. 9 TEST PARTICIPANTS Twenty-nine laboratories, consisting of analysis laboratories and sampling entities having an in-house analysis laboratory, participated in this test. This population is broken down by programs as indicated below: 11 participants for measuring mercury in a permanganate medium, 15 participants for measuring mercury in a dichromate medium, 19 participates for measuring mercury in hydrochloric acid, 17 participates for measuring fluorinated compounds, 14 participants for measuring metals, 18 participants for measuring sulfur dioxide, 21 participants for measuring ammonia. DRC B Page 11 sur 171

12 The equipment used by the participants as well as the methodologies applied and the results relative to the tests are presented in this report anonymously, using the confidential codes assigned to the participants when they registered for the tests. 10 DESCRIPTION OF THE TEST MATERIALS 10.1 DESCRIPTION AND INSTRUCTIONS The same operator or team should perform all of the analyses for a given parameter, in a short time interval, specified for each compound below. These analyses should be considered independent tests: all of the operations were to be repeated, from sampling in the bottles to expression of the final result Total mercury in permanganate medium An absorption solution was prepared according to the stipulations of standard EN 13211, then was used as flushing solution on the INERIS test block where combustion gases were generated, in order to create a matrix as close as possible (presence of interferents) to samples usually analyzed. This absorption solution, made up of 2% of KMnO 4 and 10% of H 2 SO 4 was analyzed, then spiked to make up the test material referenced 11/119507_Hg _KMnO 4. Two samples (X and Y) were taken out to be sent to each participant in order to determine the so-called Hg gas content. The analysis of these two samples was to follow the stipulations of standard EN Two measurements were requested per bottle provided, or a total of 4 measurements expressed in µg Hg/L with zero decimals. It was strongly recommended to analyze these solutions within a maximum of 15 days (Cf EN 13211), the stability not being verified beyond that period Total mercury in dichromate medium An absorption solution was prepared according to the stipulations of standard EN 13211, then was used as flushing solution on the INERIS test block where combustion gases were generated, in order to create a matrix as close as possible (presence of interferents) to samples usually analyzed. This absorption solution made up of 4 % of K 2 Cr 2 O 7 and 20% of HNO 3 was analyzed, then spiked to make up the test material referenced 11/119507_Hg _ K 2 Cr 2 O 7. Two samples (X and Y) were taken out to be sent to each participant in order to determine the so-called Hg gas content. The analysis of these two samples was to follow the stipulations of standard EN Two measurements were requested per bottle provided, or a total of 4 measurements expressed in µg Hg/L with zero decimals. It was strongly recommended to analyze these solutions within a maximum of 15 days (Cf EN 13211), the stability not being verified beyond that period. DRC B Page 12 sur 171

13 Hydrochloric acid An absorption solution was prepared according to the stipulations of standard EN 1911, then was used as flushing solution on the INERIS test block where combustion gases were generated, in order to create a matrix as close as possible (presence of interferents) to samples usually analyzed. This absorption solution made up H 2 O was analyzed, then spiked to make up the test material referenced 11/119507_HCl. Two samples (X and Y) were taken out to be sent to each participant in order to determine the so-called HCl gas content. The analysis of these two samples was to follow the stipulations of standard EN Two measurements were requested per bottle provided, or a total of 4 measurements expressed in mg HCl/L with one decimal Fluorhydric acid Solution An absorption solution was prepared according to the stipulations of standard NF X , then was used as flushing solution on the INERIS test block where combustion gases were generated, in order to create a matrix as close as possible (presence of interferents) to samples usually analyzed. This absorption solution made up NaOH 0.1 N was analyzed, then spiked to make up the test material referenced 11/119507_HF solution. Two samples (X and Y) were taken out to be sent to each participant in order to determine the so-called HF gas content. The measurements have been done using standard laboratory methods. Two measurements were requested per bottle provided, or a total of 4 measurements expressed in mg HF/L with one decimal Dusts Dusts coming from a household waste incineration unit, previously analyzed, were dried and shredded to be spiked with fluorinated salts (NaF, CaF and K 2 SiF 6 ), also dried and shredded. The whole was homogenized in order to make up the final test material referenced 11/119507_HF Poussiére. Two samples (X and Y) were taken out to be sent to each participant in order to determine the fluorinated compound content level. The s have been done using standard laboratory methods. Two measurements were requested per bottle provided, or a total of 4 measurements expressed in mg HF/g with two decimals. It was recommended to carry out an extractive phase and the fusion phase for each test, the final result corresponding to the sum of the results of the two phases. DRC B Page 13 sur 171

14 Metals (and metalloids) Solution An absorption solution was prepared according to the stipulations of standard EN 14385, then was used as flushing solution on the INERIS test block where combustion gases were generated, in order to create a matrix as close as possible (presence of interferents) to samples usually analyzed. This absorption solution made up 3% of HNO 3 and 1.5% of H 2 O 2 was analyzed, then spiked to make up the test material referenced 11/119507_Metaux solution. Two samples (X and Y) were taken out to be sent to each participant in order to determine the content level in As, Cd, Cr, Co, Cu, Mn, Ni, Pb, Sb, Tl and V. The analysis of these two samples was to follow the stipulations of standard EN Two measurements were requested per bottle provided, or a total of 4 measurements expressed in µg/l with zero decimals Dusts Dusts coming from a glassworks manufacturing plant, previously analyzed, were dried and shredded to be spiked with oxides, also dried and shredded. The whole was homogenized in order to make up the final test material referenced 11/119507_Metaux Poussières. Two samples (X and Y) were taken out to be sent to each participant in order to determine the content level in As, Cd, Cr, Co, Cu, Mn, Ni, Pb, Sb, Tl and V expressed in µg /g with one decimal. The laboratories were asked to respect the following two protocols: free protocol: Usual practice of the laboratory in measuring particulate metals (EN 14385), imposed protocol: Free protocol with the requirement of not filtering the mineral residues before analysis Sulfur dioxide An absorption solution was prepared according to the stipulations of standard EN 14791, then was used as flushing solution on the INERIS test block where combustion gases were generated, in order to create a matrix as close as possible (presence of interferents) to samples usually analyzed. This absorption solution made up of 3% of H 2 O 2 was analyzed, then spiked to make up the test material referenced 11/119507_SO2. Two samples (X and Y) were taken out to be sent to each participant in order to determine the SO 2 content level. The analysis of these two samples was to follow the stipulations of standard EN Two measurements were requested per bottle provided, or a total of 4 measurements expressed in mg SO 2 /L with one decimal. DRC B Page 14 sur 171

15 Ammonia An absorption solution was prepared according to the stipulations of standard NF X , then was used as flushing solution on the INERIS test block where combustion gases were generated. This absorption solution made up of H 2 SO N was analyzed, then spiked to make up the test material referenced 11/119507_NH3. Two samples (X and Y) were taken out to be sent to each participant in order to determine the NH 3 content level. The s have been done using standard laboratory methods. Two measurements were requested per bottle provided, or a total of 4 measurements expressed in mg NH 3 /L with one decimal. Note: The participants were also alerted to the presence, in standard NF X , of errors in the description of the colorimetric method using indophenol blue and that it was preferable to refer to other standards (For example: NF T and EN ISO 11732). 11 SHIPPING A first shipment was done on May 17, For reasons inherent to our service provider, this first shipment was cancelled, requiring the production of new lots of test materials for the sensitive parameters (Hg). A second shipment was done on May 24, HOMOGENEITY AND STABILITY OF THE SAMPLES 12.1 HOMOGENEITY OF THE MATERIALS The homogeneity of the materials was verified at the time of their distribution, according to the methodology explained in annex 1. DRC B Page 15 sur 171

16 Test materials Homogeneity of the test materials Homogeneity according to ISO Comments 11/119507_Hg_K 2 Cr 2 O 7 Compliant - 11/119507_Hg_KMnO 4 Non-compliant Taking inhomogeneity into account in calculating the z score 11/119507_HCl Compliant - 11/119507_HF_Solution Compliant - 11/119507_HF_Poussiére Compliant - 11/119507_Metaux_solution 11/119507_Metaux_Poussiére Compliant for 9 of the 11 elements to be assayed Compliant for 10 of the 11 elements to be assayed Co, Pb: Taking inhomogeneity into account in calculating the z score As: Taking inhomogeneity into account in calculating the z score 11/119507_NH 3 Compliant - 11/119507_SO 2 Compliant STABILITY OF THE TEST MATERIALS For each lot of test materials, 9 samples were randomly taken so as to establish the stability of the materials at the time of their distribution and during the analysis period by the participants. Three samples were analyzed once per week for three weeks in double determination. The stability of the materials was verified according to the methodology presented in annex 1. Note: Because of internal analytical problem, the stability study of HCl has not been validated. Nevertheless, the study of the distribution of laboratory measures by time showed no significant trend due to a time effect. DRC B Page 16 sur 171

17 The following observations were made: past the 12 th day, a variation in the ammonia content in the vicinity of 3 % was shown.: no laboratory was affected, past the 6 th day, a variation in the sulfur dioxid content in the vicinity of 5 % was shown.: no laboratory was affected, solution: a variation in the Cd content in the vicinity of 11 % on the 6 th day to reach 15 % on the 29 th day was shown: no laboratory was affected, dusts: - a variation of the As content level was showed past the 17 th day: no laboratory was affected, - a variation of the Co content level in the vicinity of 10% was shown past the 17 th day: no laboratory was affected, - a variation of the Cu content level in the vicinity of 9% was shown past the 17 th day: no laboratory was affected. 13 RESULTS OF THE INTER-LABORATORY COMPARISON 13.1 EXPLOITATION OF THE DATA FROM THE TEST MATERIALS General information The details of the statistical processing are recalled in annex 1. In the context of this test, the assigned values were defined as follows: the value assigned to the average is taken to be equal to the robust average of the results provided by the participants in the inter-laboratory comparison, the reference value of the standard deviation for assessing the aptitude is taken to be equal to the robust standard deviation. The statistical processing applied to the data made it possible to determine: - the reference value (or assigned value) of each parameter for each test and its associated uncertainty, - each participant s performance relative to the reference values via the z score indicator, - suspicious or absurd results, - the repeatability and reproducibility confidence intervals for each compound and each test material Presentation of the results In this section, the results obtained before and after statistical processing, averages, repeatability standard deviations and performance of each laboratory (z score) are presented for each test material. A distribution diagram of the z scores making it possible to situate each laboratory globally relative to the other laboratories is also provided. DRC B Page 17 sur 171

18 The legend below is used : Legend 1,4 Z i < 2: satisfactory score 2,3 Laboratory having a 2 Z i 3: debatable score requiring monitoring or preventive action 3,56 Laboratory having a Z i 3 : unsatisfactory score requiring corrective action (the analysis results are not acceptable) The other results relative to each test material are grouped together in : annex 2: raw data for each participant: average, repeatability standard deviation, repeatability variability coefficient, and the values dismissed by expert opinion. annex 3: statistical distribution curves: Sort by Averages: Values comprised between (x * - 3s * ) and (x * + 3s * ). annex 4: histogram of the z scores obtained by each laboratory for all analytes of a test (Available for materials 11/119507_Metals_ solution and 11/119507_Metals_dust). DRC B Page 18 sur 171

19 Test material "11/119507_Hg_KMnO 4 " Values observed before application of statistical algorithms Parameter (µg/liter) Value targeted by spiking Population Average Population Standard Deviation CV R (%) CV rep (%) Mercury % 5.74% Population 10 S L 3.9 S R 4.0 S r 1.0 Values observed after application of statistical algorithms Parameters (µg/liter) Value targeted by spiking Mercury 12 x* 11.5 s* 1.7 u X* 0.7 w* 1.0 S L 1.6 S R 1.9 S r 1.0 Relative IC R (%) 39.0% Relative IC r (%) 21.1% DRC B Page 19 sur 171

20 Averages, standard deviations and z scores for the laboratories Laboratory Identification x µg/l s r µg/l Mercury s r % Z scores % Not analyzed % Not analyzed Not analyzed % % Not analyzed % < % (-5.22)* Not analyzed < % (-3.24)* % % % Not analyzed Not analyzed Not analyzed ()*: Z score calculated relative to the threshold value rendered. NB: the absolute value is bounded from below. Remarks and comments : Laboratories and delivered results in the form of measurement thresholds respectively of < 1 and < 5 µg/l. They were excluded from the robust statistical processing by expert opinion. DRC B Page 20 sur 171

21 Laboratory was marked as abnormal by the Mandel k test due to its intralaboratory dispersion Test material "11/119507_Hg_K 2 Cr 2 O 7 " Values observed before application of statistical algorithms Parameters (µg/liter) Value targeted by spiking Mercury 12 Population Average 11.3 Population Standard Deviation CV R (%) CV rep (%) % 3.25% Population 14 S L 1.75 S R 1.82 S r 0.51 Values observed after application of statistical algorithms Parameters (µg/liter) Value targeted by spiking Mercury 12 x* 11.3 s* 1.7 u X* 0.6 w* 0.5 S L 1.7 S R 1.7 S r 0.5 Relative IC R (%) 33.6% Relative IC r (%) 10.0% DRC B Page 21 sur 171

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