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CENTRO DE METROLOGIA QUIMICA. CALCULATION OF UNCERTAINTIES FOR THE RESULTS REPORTED IN SIM.QM-P2.

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Presentation on theme: "CENTRO DE METROLOGIA QUIMICA. CALCULATION OF UNCERTAINTIES FOR THE RESULTS REPORTED IN SIM.QM-P2."— Presentation transcript:

1 CENTRO DE METROLOGIA QUIMICA

2 CALCULATION OF UNCERTAINTIES FOR THE RESULTS REPORTED IN SIM.QM-P2

3 ANALYTICAL MEASUREMENT As, Cu, Fe, Mn, Ni, Pb, (Zn) Perkin-Elmer AAnalyst700 Atomic Absorption Spectrophotometer equipped with a longitudinal graphite furnace

4 Cd Flame Atomic Absorption Spectrophotometry Perkin-Elmer AAnalyst100 and using high sensitivity nebulizer ANALYTICAL MEASUREMENT

5 NIST-SRMs were used for the preparation of calibration standards. The quantification method used was bracketing Four independent aliquots of the sample were analyzed, in all cases. NIST-SMR 1643d was used as control (except for Cd) ANALYTICAL MEASUREMENT

6 Identify Uncertainty Sources THE UNCERTAINTY ESTIMATION PROCESS Calculate combined standard uncertainty Specify associated model Quantify Uncertainty Sources Reporting Uncertainty Convert to standard uncertainty

7 ASSOCIATED MODEL: BRACKETING CLCL CHCH ALAL AHAH CSCS ASAS Sample concentration is calculated through the equation

8 IDENTYFING UNCERTAINTY SOURCES repeatability calibration temperature C sample d A L, A H, A s repeatability C L, C H calibration temperature F(dil) U-SMR

9 QUANTIFYING UNCERTAINTY SOURCES repeatability calibration temperature C sample d A L, A H, A s repeatability C L, C H calibration temperature F(dil) U-SMR

10 Repeatability of A (S,L,H) The uncertainty due to random variation of the EAA signal measurement of samples and bracketing standards was calculated as: QUANTIFYING UNCERTAINTY SOURCES Fe Determination

11 repeatability calibration temperature C sample d A L, A H, A s repeatability C L, C H calibration temperature F(dil) U-SMR QUANTIFYING UNCERTAINTY SOURCES

12 C sample repeatability C L, C H calibration temperature F(dil) Equation for concentration assessment Equation for the uncertainty calculation U-SMR

13 C sample repeatability C L, C H calibration temperature F(dil) U-SMR

14 C L = 9.827  g/Lu C = 0.055  g/L PREPARATION OF STANDARDS Values and uncertainties

15 repeatability calibration temperature C sample d A L, A H, A s repeatability C L, C H calibration temperature F(dil) QUANTIFYING UNCERTAINTY SOURCES U-SMR

16 CALCULATING THE CONCENTRATION

17 CALCULATING THE COMBINED STANDARD UNCERTAINTY

18 KRAGTEN (*) Finally (*) J. Kragten, Analyst, 119, 2161-2166 (1994)

19 CALCULATION OF COMBINED STANDARD UNCERTAINTY

20 UNCERTAINTY CONTRIBUTIONS

21 Finally, the concentration and uncertainty values for Fe in the sample SIM.QM-P2 are: Concentration C S = 93.19  g/L Combined uncertainty u com = 0.92  g/L Expanded uncertainty U = 1.84  g/L U=u*k, (k=2) (1.97%)

22 RESULTS OF Intec IN SIM.QM-P2 SUMMARY OF RESULTS OBTAINED ON SAMPLE SIM-P2 ElementAverage concentrationExpanded UncertaintyREU (  g/L)(  (%) Ni62,862,524,0 Fe93,191,842,0 Cu17,060,442,6 As50,941,022,0 Pb21,860,663,0 Mn39,441,584,0 Cd14442,8

23 RESULTS OF SIM.QM-P2

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25 CENTRO DE METROLOGIA QUIMICA

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