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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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Presentation Transcript
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
slide6

THE UNCERTAINTY ESTIMATION PROCESS

Specify associated model

Identify Uncertainty Sources

QuantifyUncertainty Sources

Convert to standarduncertainty

Calculate combinedstandarduncertainty

Reporting Uncertainty

slide7

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

slide10
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

slide11

QUANTIFYINGUNCERTAINTY SOURCES

AL, AH, As

d

repeatability

repeatability

calibration

temperature

Csample

F(dil)

U-SMR

repeatability

calibration

CL, CH

temperature

slide12

Csample

F(dil)

U-SMR

repeatability

calibration

temperature

CL, CH

Equation for concentration assessment

Equation for the uncertainty calculation

slide13

Csample

F(dil)

U-SMR

repeatability

calibration

temperature

CL, CH

slide14

PREPARATION OF STANDARDS

Values and uncertainties

CL = 9.827 mg/L

uC = 0.055 mg/L

slide15

QUANTIFYINGUNCERTAINTY SOURCES

AL, AH, As

d

repeatability

repeatability

calibration

temperature

Csample

F(dil)

U-SMR

repeatability

calibration

CL, CH

temperature

slide18

KRAGTEN(*)

Finally

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

slide21

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%)

slide22

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