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Specify
Specify measurand
measurand
Quantify
Quantify components
components for
for within
within lab
lab reproducibility
reproducibility
AA control
control samples
samples
BB possible
possible steps,
steps, not
not covered
covered by
by the
the control
control sample
sample
Quantify
Quantify bias
bias components
components
Convert
Convert components
components to
to standard
standard uncertainty
uncertainty
u1 + u2
u1
Calculate
Calculate combined
combined standard
standard uncertainty
uncertainty
u2
Calculate
Calculate expanded
expanded uncertainty
uncertainty U
U=
= 22 uucc
0
rel. Uncertainty
Comments
sRw
standard deviation
0.5 g/l
2.5 %
Control sample 2
x = 250.3 g/l
sRw
standard deviation
3.7 g/l
1.5 %
Other components
--1
u(x)
Comments
sRw
0.6 g/l
Absolute:
u(x)=(0.5 + 0.37)1/2
High level
(>15 g/l)
sRw
3.9 %
Relative:
u(x)=(1.5% + 3.6%)1/2
The laboratory does not have access to stable control samples (e.g.
measurement of dissolved oxygen)
u(x)
Comments
s = 0.024 mg/l
mean: 7.53 mg/l
0.32 %
from 50
measurements
s = 0.5 %
0.5 %
based on
experience
sr
with
RMSbias =
(bias )
s
ubias = (bias )2 + bias + u(Cref )2
n
5
100(0.26/11.5)=2.21%
s
ubias = (bias )2 + bias + u(Cref )2 =
n
2
2.2%
(3.48%)2 +
+ 2.21%2 = 4.2%
12
7
RMSbias =
(bias )
i
u(Cref ) =
sR
9%
=
= 2.6%
n
12
(bias )
10
1%
u(vol ) =
+ 0.5%2 = 0.76%
3
5 % 2 + 2% 2 + 3% 2 + 4 % 2 + 1% 2 + 4 % 2
= 3.44%
6
12
13
U = 2 uc
14
Reproducibility Standard
Deviation from a Standard
The laboratory must first prove that they are
able to perform in accordance with the
standard method
No unusual bias
Verification of the repeatability
U = 2 sR
16
drinking water
surface water
waste water
17
U = 2 sR
18
auerhalb oben
auerhalb [%]
auerhalb unten
52,25
40,07
39,06
31,65
25,40
39,10
30,78
24,65
30,25
29,16
28,46
22,29
-41,60 37 3 1
-33,46 39 3 1
-32,75 39 1 0
-27,36 41 2 2
-22,55 38 0 1
-32,78 40 1 0
-26,71 41 1 1
-21,96 38 5 1
-26,31 39 2 0
-25,48 40 1 3
-24,94 38 5 2
-20,06 40 2 2
Summe 470 26 14
10,8
10,3
2,6
9,8
2,6
2,5
4,9
15,8
5,1
10,0
18,4
10,0
8,5
Anzahl Werte
0,1334
0,2256
0,3502
0,4726
0,4550
0,7704
0,7712
0,7361
0,9177
0,9965
1,0672
0,9854
0,584
1,248
1,982
3,238
3,822
4,355
5,421
6,360
6,553
7,361
8,063
9,359
Vorgabe [g/l]
1
2
3
4
5
6
7
8
9
10
11
12
Niveau
uc = sR 20%
U 40%
19
10
Method b)
direct use of the reproducibility standard deviation from
standards or PTs as combined standard uncertainty
Expression of Uncertainty
The statement of uncertainty always has to
contain the level of confidence
If possible also state the estimation method
used
Example:
SO42- in waste water (ISO 10304-2): 100 8 mg/l*
* Measurement uncertainty was derived from results of interlaboratory
comparisons. It represents an expanded uncertainty with a coverage factor
k=2; this corresponds to a level of confidence of about 95%.
21
11
23
12
Decision Rules
The key to the assessment are the decision
rules
Based on
The measurement result,
Its uncertainty,
The specification limit
25
13
26
27
14
More Complicated
Decision Rules
Decision rules may include, for
example, that for cases (ii) and (iii) in
the figure, additional measurement(s)
should be made, or
That the manufactured product might be
compared with an alternative
specification to decide on possible sale
at a different price
29
15
high confidence of
correct rejection
(1st example)
b)
high confidence of
correct
acceptance
(2nd example)
31
16
32
17
Guidance Documents
18