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French Inter-laboratories campaigns Context and finality

French Inter-laboratories campaigns Context and finality. Context. Arrêté du 04 septembre 2000 (agrément des organismes de contrôle) “ agréments” are issued to laboratories performing sampling that have been accredited (programme n°97 COFRAC or equiv t )

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French Inter-laboratories campaigns Context and finality

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  1. French Inter-laboratories campaigns Context and finality

  2. Context • Arrêté du 04 septembre 2000 (agrément des organismes de contrôle) • “agréments” are issued to laboratories performing sampling that • have been accredited (programme n°97 COFRAC or equivt) • agree to participate to interlaboratory campaigns of 3 days organized at INERIS at least once every 3 years on the bench and every year for the analytical comparisons.

  3. Finality of the tests on the bench • To follow and improve the quality of implementation of SRM • through the evolution of Confidence intervals of reproducibility, compared to those required by EN standards, • information and training for new EN standards (comparisons of measuring devices, of results). • Judgment of the capacity of the laboratories • conformity of measuring devices and of the implementation through audits, • test of knowledge of standards, • comparison of results / Caverage... ==> - the results of these tests are evaluated by the commission in charge of delivering “agréments” to the laboratories. - the synthesis report which enlightens slips of each laboratory in implementation of the SRM may be audited by the accreditation body.

  4. The bench

  5. Specificity of the tests on the bench • The totality of the method is involved (sampling + analysis) • Generation of real flue gases in order to be under real conditions of • operation (matrix, temperature, moisture). • Means: generation of combustion gases, doped by additions of pollutants ignorance of the generated exact concentration • Advantages: • Possibility to simulate different types of gases (LCP, WI) • provide real data and uncertainties at different level of concentrations • Drawbacks: • true value unknown _ comparisons of the results with the average value given by the participants • limited number of participants ==> use of statistics limited

  6. Capacity criteria • Respect of QA/QC procedures and associated criteria • field blank • Leak test • absorption efficiency • Respect of standardised procedures • list of key points • check of provisions (written procedures, forms) • check of application

  7. Inter-laboratories tests • Approach in the field leads to determination of the fidelity of the method characterised by a standard deviation or a repeatability or reproducibility confidence interval ==> see ISO 5725-2 lab A Sampled gases Type uncertainty sr "repeatability" lab A lab A lab A Type uncertainty sR Sampled gases "reproducibility" lab B lab C

  8. Inter-laboratories tests lab A - 2 lab A - 1 Flue gases lab D - 1 lab B - 1 lab D - 2 lab B - 2 lab C - 2 lab C - 1

  9. Inter-laboratories tests • Results of the 26 first campaigns obtained with accredited laboratories • They relates to : • automatic analysis of O2 (5-13%), CO2, CO (10 à 500 mg/m3), NOx (75 à 1000 mg/m3), SO2 (40 à 1000 mg/m3) et COVT (0 à 50 mgC/m3) • and from the 7th campaign on manual methods for HCl, HF, Hg and at last on H2O. • From the 9th campaign participants are accredited and consequently EN standards should be applied.

  10. Inter-laboratories tests Maximum value of Target value for the confidence interval reproducibility confidence fixed by directives interval : t.s R O - ±6 % 2 CO ±10 % ±5 % SO ±20 % ±10 % * 2 NO ±20 % ±10 % x COVT ±30 % ±15 % HF and HCl ±40 % ±20 % Hg - 25% dust ±30 % ±15 % * impossible to reach due to the manual method

  11. s average % s % I % compound concentration r R CR 3 2,1 mg/m n HF 2,7 26,5 53,0 3 4,7 mg/m n 2,9 18,1 36,2 3 20,6 mg/m n HCl 1,1 6,5 13,0 3 102,3 mg/m n 0,9 4,3 8,6 3 75,7 mg/m n SO 1,1 14,1 28,2 2 3 214,7 mg/m n 1,0 3,5 7,0 3 43,3 µg/m Hg 4,8 13,8 27,6 3 130,0 µg/m 2,5 12,7 25,4 Analytical inter-laboratories tests s : repeatability standard deviation r s : reproducibility standard deviation R I CR : : reproducibility confidence interval

  12. Analytical inter-laboratories tests

  13. Analytical inter-laboratories tests

  14. Compounds Target value Average Recovery µg/g X rate (µg/g) % Arsenic 2346 77,7 3020 Cadmium 421 81,0 520 Cobalt 4065 90,7 4480 Chrome 410 15,2 2690 Copper 5573 88,3 6310 Manganese 4425 89,9 4920 Nickel 4688 87,0 5390 Lead 8543 84,2 10150 Antimony 8102 88,2 9190 Tin 103 1,4 7250 Thallium 451 65,4 690 Selenium 2082 29,7 7009 Tellurium 1082 27,4 6205 Zinc 25316 92,1 27478 Vanadium Analytical inter-laboratories tests 3623 89,5 4050 Table 4 : statistics values– digestion efficiency

  15. O2 and CO2 15 14 13 12 11 10 9 8 7 6 5 4 3 2 1 2 0 Ic reference Ic average Ic 2005 Ic avrIcref Ic2005/Icref O 0,9 4,2 1,7 5,0 2,0 2 CO 4,0 3,8 2 Target value for O2 and CO2 : 6% 2 Target reached in 2005 for 4 campaigns out of 4 for O2: : 2,75 / 0,45 / 1,9 / 1.7 improvement Target reached Target reached in 2005 for 4 campaigns out of 4 for CO2 : 3,7 / 5,05 / 4,4 / 2,2 Stability Target reached 2 Inter-laboratories tests O2 4-13% IC % CO2 4-10% 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 Number of campaigns

  16. NOx Inter-laboratories tests 50 45 40 35 30 Ic % NOx 80-1000mg/m3 25 20 15 10 5 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 Number of campaigns Ic Ic /Icref Ic reference Ic average Ic ave/Icref 2005 2005 3 80-1000mg/m NOx 2 11,1 11,9 5,5 6,0 : 10 % Target for NOx Light improvement Target reached at 50% Target reached in 2005 2 times : 10 / 11,2 / 19,3 / 7,2 Improvements to be brought : respect warm up time of the analysers Leak tests Contrôle of drifts contrôle of converter (efft > 95 %) Losses of NO 2

  17. CO and TOC Ic Ic /Icref Ic reference Ic average Ic av/Icref 2005 2005 3 30-500mg/m CO 3,1 15,1 5,2 5,0 1,7 3 10-30mg/m CO 2,4 50,9 43,5 21,2 18,1 3 5-40mgC/m TOC 36,2 36,8 Target for CO : 5% Improvement Target reached at 50% Target reached 2 timesout of 4 in 2005 : 7,9 / 5,7 / 4,3 / 2,7 Target for TOC : 15% Improvement Target not reached Target not reached in 2005 : 20,9 / 46,4 / 42,9 / 37 ) Inter-laboratories tests 200 180 CO 30-500mg/m3 160 140 120 TOC 5-40mgC/m3 % Ic 100 80 CO 10-30mg/m3 60 40 20 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 Number of campaigns

  18. Inter-laboratories tests H2O 50 45 40 35 30 Ic % 25 H2O % 20 2 15 10 5 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 Number of campaigns Ic Ic /Icref Ic reference Ic average Ic av/Icref 2005 2005 H O % 20 23,6 19,1 1,2 1,0 2 Target for H O : 20 % 2 Improvement Targetr reached at 25% Target reached in 2005 1 time out of 4 : 12 / 20,2 / 20,6 / 23,4 Improvements to be brought : Leak test Global weighing of the whole water capture system with a balance of 0,1g precision Heating of the sampling line

  19. , SO2 , HCl and HF Ic Ic /Icref Ic reference Ic average Ic moy/Icref 2005 2005 3 70-300mg/m SO 10 41,5 32,1 4,1 3,2 2 3 5mg/m HF 30 75,4 29,9 2,5 1,0 3 40mg/m HCl 5 43,1 34,2 8,6 6,8 3 Target for SO : 20 % 2 Improvement Target not reached Target not reached in 2005 : 43,5 / 39,8 / 21,4 / 23,8 3 3 Ic analytique 2002 : 29,8 % at 76 mg/m and11 % at 212 mg/m Target for HCl : 20 % Light improvement Target not reached Target not reached in 2005 : 25 / 40 / 50 / 30 3 Ic analytique 2002 at 20 mg/m : 13 % 3 Target for HF pour 5 mg/m : 20 % Improvement Target not reached Target not reached in 2005 : 25 / nd / 52 / 29 4 2 Inter-laboratories tests 110 100 HF 1-20mg/m3 90 80 HCl 40mg/m3 70 60 SO2 70-300mg/m3 Ic % 50 40 30 20 10 0 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 Number of campaigns

  20. Inter-laboratories tests Hg 100 Ic 90 in % 80 70 60 50 Hg 40-100µg/m3 40 30 20 10 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 Number of campaigns Ic Ic / Icref Ic reference Ic average Ic ave/ Icref 2005 2005 3 40-100µg/m Hg 25 63,0 94,2 2,5 3,2 Target for Hg : 20 % No improvement Target not reached in 2005 : 90 / 52,6 / 140 / nd Ic analytique 2002 : 27,6 to 29,4%

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