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CENTRO DE METROLOGIA QUIMICA. CALCULATION OF UNCERTAINTIES FOR THE RESULTS REPORTED IN SIM.QM-P2. As, Cu, Fe, Mn, Ni, Pb, (Zn) Perkin-Elmer AAnalyst700 Atomic Absorption Spectrophotometer equipped with a longitudinal graphite furnace. ANALYTICAL MEASUREMENT. Cd
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CALCULATION OFUNCERTAINTIESFOR THE RESULTSREPORTED IN SIM.QM-P2
As, Cu, Fe, Mn, Ni, Pb, (Zn) Perkin-Elmer AAnalyst700 Atomic Absorption Spectrophotometer equipped with a longitudinal graphite furnace ANALYTICAL MEASUREMENT
Cd Flame Atomic Absorption Spectrophotometry Perkin-Elmer AAnalyst100 and using high sensitivity nebulizer ANALYTICAL MEASUREMENT
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
THE UNCERTAINTY ESTIMATION PROCESS Specify associated model Identify Uncertainty Sources QuantifyUncertainty Sources Convert to standarduncertainty Calculate combinedstandarduncertainty Reporting Uncertainty
ASSOCIATED MODEL: BRACKETING AH AS AL CL CS CH Sample concentration is calculated through the equation
IDENTYFING UNCERTAINTY SOURCES AL, AH, As d repeatability repeatability calibration temperature Csample F(dil) U-SMR repeatability calibration CL, CH temperature
QUANTIFYING UNCERTAINTY SOURCES AL, AH, As d repeatability repeatability calibration temperature Csample F(dil) U-SMR repeatability calibration CL, CH temperature
Repeatability of A(S,L,H) QUANTIFYING UNCERTAINTY SOURCES The uncertainty due to random variation of the EAA signal measurement of samples and bracketing standards was calculated as: Fe Determination
QUANTIFYINGUNCERTAINTY SOURCES AL, AH, As d repeatability repeatability calibration temperature Csample F(dil) U-SMR repeatability calibration CL, CH temperature
Csample F(dil) U-SMR repeatability calibration temperature CL, CH Equation for concentration assessment Equation for the uncertainty calculation
Csample F(dil) U-SMR repeatability calibration temperature CL, CH
PREPARATION OF STANDARDS Values and uncertainties CL = 9.827 mg/L uC = 0.055 mg/L
QUANTIFYINGUNCERTAINTY SOURCES AL, AH, As d repeatability repeatability calibration temperature Csample F(dil) U-SMR repeatability calibration CL, CH temperature
KRAGTEN(*) Finally (*) J. Kragten, Analyst, 119, 2161-2166 (1994)
Finally, the concentration and uncertainty values for Fe in the sample SIM.QM-P2 are: Concentration CS = 93.19 mg/L Combined uncertainty ucom = 0.92 mg/L Expanded uncertainty U = 1.84 mg/L U=u*k, (k=2) (1.97%)
RESULTS OF Intec IN SIM.QM-P2 SUMMARY OF RESULTS OBTAINED ON SAMPLE SIM-P2 Element Average concentration Expanded Uncertainty REU (%) ( g/L) ( g/L) m m Ni 62,86 2,52 4,0 Fe 93,19 1,84 2,0 Cu 17,06 0,44 2,6 As 50,94 1,02 2,0 Pb 21,86 0,66 3,0 Mn 39,44 1,58 4,0 Cd 144 4 2,8