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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 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


THE UNCERTAINTY ESTIMATION PROCESS standards.

Specify associated model

Identify Uncertainty Sources

QuantifyUncertainty Sources

Convert to standarduncertainty

Calculate combinedstandarduncertainty

Reporting Uncertainty


ASSOCIATED MODEL: standards.

BRACKETING

AH

AS

AL

CL

CS

CH

Sample concentration is calculated through the equation


Identyfing uncertainty sources
IDENTYFING UNCERTAINTY SOURCES standards.

AL, AH, As

d

repeatability

repeatability

calibration

temperature

Csample

F(dil)

U-SMR

repeatability

calibration

CL, CH

temperature


Quantifying uncertainty sources
QUANTIFYING standards. UNCERTAINTY SOURCES

AL, AH, As

d

repeatability

repeatability

calibration

temperature

Csample

F(dil)

U-SMR

repeatability

calibration

CL, CH

temperature


Repeatability of A standards.(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


QUANTIFYING standards.UNCERTAINTY SOURCES

AL, AH, As

d

repeatability

repeatability

calibration

temperature

Csample

F(dil)

U-SMR

repeatability

calibration

CL, CH

temperature


C standards.sample

F(dil)

U-SMR

repeatability

calibration

temperature

CL, CH

Equation for concentration assessment

Equation for the uncertainty calculation


C standards.sample

F(dil)

U-SMR

repeatability

calibration

temperature

CL, CH


PREPARATION OF STANDARDS standards.

Values and uncertainties

CL = 9.827 mg/L

uC = 0.055 mg/L


QUANTIFYING standards.UNCERTAINTY SOURCES

AL, AH, As

d

repeatability

repeatability

calibration

temperature

Csample

F(dil)

U-SMR

repeatability

calibration

CL, CH

temperature



CALCULATING THE COMBINED standards.STANDARDUNCERTAINTY


KRAGTEN standards.(*)

Finally

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


CALCULATION OF COMBINED standards.STANDARDUNCERTAINTY



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 the sample SIM.QM-P2 are:

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


RESULTS OF SIM.QM-P2 the sample SIM.QM-P2 are:


RESULTS OF SIM.QM-P2 the sample SIM.QM-P2 are:


CENTRO DE METROLOGIA QUIMICA the sample SIM.QM-P2 are:


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