CENTRO DE METROLOGIA QUIMICA
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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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CENTRO DE METROLOGIA QUIMICA

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Centro de metrologia quimica

CENTRO DE METROLOGIA QUIMICA


Calculation of uncertainties for the results reported in sim qm p2

CALCULATION OFUNCERTAINTIESFOR THE RESULTSREPORTED IN SIM.QM-P2


Analytical measurement

As, Cu, Fe, Mn, Ni, Pb, (Zn)

Perkin-Elmer AAnalyst700 Atomic Absorption Spectrophotometer equipped with a longitudinal graphite furnace

ANALYTICAL MEASUREMENT


Analytical measurement1

Cd

Flame Atomic Absorption Spectrophotometry

Perkin-Elmer AAnalyst100 and using high sensitivity nebulizer

ANALYTICAL MEASUREMENT


Analytical measurement2

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


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THE UNCERTAINTY ESTIMATION PROCESS

Specify associated model

Identify Uncertainty Sources

QuantifyUncertainty Sources

Convert to standarduncertainty

Calculate combinedstandarduncertainty

Reporting Uncertainty


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ASSOCIATED MODEL:

BRACKETING

AH

AS

AL

CL

CS

CH

Sample concentration is calculated through the equation


Identyfing uncertainty sources

IDENTYFING UNCERTAINTY SOURCES

AL, AH, As

d

repeatability

repeatability

calibration

temperature

Csample

F(dil)

U-SMR

repeatability

calibration

CL, CH

temperature


Quantifying uncertainty sources

QUANTIFYING UNCERTAINTY SOURCES

AL, AH, As

d

repeatability

repeatability

calibration

temperature

Csample

F(dil)

U-SMR

repeatability

calibration

CL, CH

temperature


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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


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QUANTIFYINGUNCERTAINTY SOURCES

AL, AH, As

d

repeatability

repeatability

calibration

temperature

Csample

F(dil)

U-SMR

repeatability

calibration

CL, CH

temperature


Centro de metrologia quimica

Csample

F(dil)

U-SMR

repeatability

calibration

temperature

CL, CH

Equation for concentration assessment

Equation for the uncertainty calculation


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Csample

F(dil)

U-SMR

repeatability

calibration

temperature

CL, CH


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PREPARATION OF STANDARDS

Values and uncertainties

CL = 9.827 mg/L

uC = 0.055 mg/L


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QUANTIFYINGUNCERTAINTY SOURCES

AL, AH, As

d

repeatability

repeatability

calibration

temperature

Csample

F(dil)

U-SMR

repeatability

calibration

CL, CH

temperature


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CALCULATING THE CONCENTRATION


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CALCULATING THE COMBINEDSTANDARDUNCERTAINTY


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KRAGTEN(*)

Finally

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


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CALCULATION OF COMBINEDSTANDARDUNCERTAINTY


Uncertainty contributions

UNCERTAINTY CONTRIBUTIONS


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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%)


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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


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RESULTS OF SIM.QM-P2


Centro de metrologia quimica

RESULTS OF SIM.QM-P2


Centro de metrologia quimica

CENTRO DE METROLOGIA QUIMICA


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