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CENTRO DE METROLOGIA QUIMICA

CENTRO DE METROLOGIA QUIMICA. CALCULATION OF UNCERTAINTIES FOR THE REPORT OF ANALYSES IN SIM.8.P1.2 (C HLORINATED P ESTICIDES IN H EXANE ). HEXACHLOROBENZENE gamma-HCH (g-BHC, LINDANE) HEPTACHLOR HEPTACHLOR EPOXIDE 2,4'-DDE CIS-CHLORDANE (ALPHA-CHLORDANE) TRANS-NONACHLOR DIELDRIN

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CENTRO DE METROLOGIA QUIMICA

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  1. CENTRO DE METROLOGIA QUIMICA

  2. CALCULATION OFUNCERTAINTIESFOR THE REPORT OF ANALYSESIN SIM.8.P1.2(CHLORINATED PESTICIDESIN HEXANE)

  3. HEXACHLOROBENZENE gamma-HCH (g-BHC, LINDANE) HEPTACHLOR HEPTACHLOR EPOXIDE 2,4'-DDE CIS-CHLORDANE (ALPHA-CHLORDANE) TRANS-NONACHLOR DIELDRIN 4,4'-DDE 2,4'-DDD 2,4'-DDT 4,4'-DDT MIREX Gas Chromatograph Perkin-Elmer Model 8000 series2with Electron Capture Detector and manual injector Column Phase, BP- 5 Col. Length, 50.00 m Col. i.d., 0.33 mm Col. film thickness, 0.50 µm ANALYTICAL MEASUREMENT

  4. NIST-SRM 2261 was used for the preparation of calibration standards. The quantification method used was bracketing using the method of internal standard. Sample of SIM.QM-P1 was selected as control ANALYTICAL MEASUREMENT

  5. ANALYTICAL MEASUREMENT GENERAL SCHEME OF ANALYTICAL MEASUREMENT • Gravimetric Preparation of standards, samples and controls • Gravimetric Preparation of dilution • Verification of the standards through the calibration curve • Determination by bracketing using the method of internal standard • Statistical evaluation of the results and uncertainty calculation

  6. GRAVIMETRIC PREPARATION OF STANDARDS

  7. BRACKETING SCHEME ng/g 120 58 40 20 8 4,4 ‘ -DDE HCB, g-HCH, HEPTACLOR EPOXI, MIREX, 2’4-DDT, 4’4-DDT DIELDRIN HEPTACLOR (s/d), cis-CLORDANO, trans-NONACLOR, 2’4-DDD, 2’4-DDE

  8. THE UNCERTAINTY ESTIMATION PROCESS

  9. BRACKETING AND INTERNAL STANDARD (AH/AIS) (AS/AIS) (AL/AIS) CS/CIS CH/CIS CL/CIS Sample concentration is calculated trough the equation:

  10. IDENTYFYING UNCERTAINTY SOURCES Csample

  11. QUANTIFYING UNCERTAINTY SOURCES Csample

  12. UNCERTAINTY OF THE STANDARDS

  13. UNCERTAINTY OF THE STANDARDS

  14. Ampoules SMR 2261 sol. INT 1 sol. INT 3 Standard Standard Brack low Brack high IS – sol. INT IS solid GRAVIMETRIC PREPARATION OF STANDARDS 0.5% 0.6% 0.6% 0.6% 0.6%

  15. IDENTYFYING UNCERTAINTY SOURCES Csample

  16. IDENTYFYING UNCERTAINTY SOURCES Csample

  17. PURITY OF THE INTERNAL STANDARD The purity of IS is quoted by the supplier as 99.0 % . The quoted uncertainty is taken as a rectangular distribution

  18. QUANTIFYING UNCERTAINTY SOURCES

  19. UNCERTAINTY STANDARD OF THE SIGNAL The uncertainties associated with the variability of the area were estimated by making replicate measurements of samples and bracketing standards. These uncertainties are estimated through the following equation:

  20. UNCERTAINTY STANDARD OF THE SIGNAL

  21. QUANTIFYING UNCERTAINTY SOURCES

  22. CALCULATING THE CONCENTRATION

  23. UNCERTAINTY CONTRIBUTIONS

  24. CONCENTRATION AND UNCERTAINTY VALUES FOR THE SAMPLE SIM.8.P1.2

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