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7

5
3
10
8
2
9
11
13
1
4
6
14
12
15
average
stdev
RSD
Uncertainty (k=2)

Ringtest OCW

94

Cumulative Rest (%)

Lab

Particle Size
Result True value Bias
91.13
92.1
-0.97
91.43
92.1
-0.67
91.73
92.1
-0.37
91.73
92.1
-0.37
91.77
92.1
-0.33
92.17
92.1
0.07
92.17
92.1
0.07
92.25
92.1
0.15
92.27
92.1
0.17
92.33
92.1
0.23
92.33
92.1
0.23
92.4
92.1
0.30
92.47
92.1
0.37
92.67
92.1
0.57
92.7
92.1
0.60
92.103
0.4513 RMS
0.436
0.5% %RMS
0.5%
1.0%
U
0.9%
0.11651964

93

92

91

90
7

Bitumen
Lab
6
6.02
6.09
6.12
6.12
6.13
6.14
6.16
6.16
6.17

6.163333333
6.163333333
6.163333333
6.163333333
6.163333333
6.163333333
6.163333333
6.163333333
6.163333333
6.163333333

-0.16333333
-0.14333333
-0.07333333
-0.04333333
-0.04333333
-0.03333333
-0.02333333
-0.00333333
-0.00333333
0.006666667

6.6

6.4
Bitumen (%)

5
8
6
2
15
4
11
9
10
7

6.2

average
stdev
RSD
% Uncertainty (k=2)
Uncertainty (k=2)

6.22
6.25
6.27
6.27
6.33
6.16333333
0.09232448
1.5%
3.0%
0.18464896

6.163333333
6.163333333
6.163333333
6.163333333
6.163333333

0.056666667
0.086666667
0.106666667
0.106666667
0.166666667
0.089193921
1.4%
2.9%
0.178387842

Bitumen (%)

13
12
1
3
14

6.2

5.8
5

Ringtest OCW - Particle Size Distribution Sieving Method FME


54.07 0,063 mm

Assigned Value

10

11

13

14

12

15
Labnr.

Ringtest OCW % Bitumen FME 54.07

15

11

10

13

12

14
Labnr

Test 1
Test 2
Test 3
Test 4
Test 5
Test 6
Test 7
Test 8
Test 9
Test 10

PersonA

PersonB

29.89
29.93
29.72
29.98
30.02
29.98
29.80
29.95
29.97
29.91

30.02
29.99
30.11
29.97
30.01
29.99
30.00
29.98
30.04
30.07

ID Pipet
Volume pipet:

MICROPIP 32
100-1000 l

Date

9/4/2012
z (l/mg) =

1.0027

ml/g

Correction factor for T and pressure

Weighings
Measurements (mg)

1
2
3
4
5
6
7
8
9
10

Nominal

50%

Smallest

1000 L
987.7
992.0
993.3
991.1
986.3
987.4
991.2
991.1
989.0
989.8

500 L
498.7
498.4
496.3
496.2
497.1
496.3
496.6
495.3
496.3
497.1

100 L
99.2
99.1
99.7
99.0
100.1
99.6
100.0
99.9
98.3
99.5

Aluminium
Arsenic
Zinc

Our result
Result (ng/mL)
ue (ng/mL)
110.3
5.6
67.2
3.4
81.3
3.8

Values
Sorted
Min
Max
Range
Qexp
n=8

82.5
78.4
78.4
86.8
8.4
0.5

82.5
80.6

0.3

81.7
80.8

81.0
81.0

80.8
81.7

80.6
82.5

78.4
82.5

86.8
86.8

Validation Spreadsheet

CRM:
m CRM
U CRM:
Number
1
2
3
4
5
6
7
8
9
10

issued on: 12/03/2007


revised on: 13/04/2008

ERM-BD 273
425
29

Toasted Bread
ng/g
ng/g

Date (dd-mm-yy)
04-Jun-06
04-Jun-06
04-Jun-06
04-Jun-06
04-Jun-06
04-Jun-06
04-Jun-06
04-Jun-06
04-Jun-06
04-Jun-06

Results
427
413
447
427
449
409
451
423
439
442

Analytical Services Lab

s
mg/l
g/l
ng/l
%
C

FM-0243
Page 5/11

Validation Spreadsheet

Number
1
2
3
4
5
6
7
8
9
10
11
12
13

issued on: 12/03/2007


revised on: 13/04/2008

Date (dd-mm-yy)
11-Jun-06
18-Jun-06
25-Jun-06
02-Jul-06
09-Jul-06
16-Jul-06
23-Jul-06
30-Jul-06
06-Aug-06
13-Aug-06
20-Aug-06
27-Aug-06
03-Sep-06

Analytical Services Lab

Results
402
418
444
455
413
444
460
421
450
408
439
455
416

FM-0243
Page 5/11

Validation Spreadsheet

Number
1
2
3
4
5
6
7
8
9
10

issued on: 12/03/2007


revised on: 13/04/2008

Clow (ng/g)
0.3880
0.4380
0.3270
0.3130
0.3950
0.4040
0.3850
0.3930
0.3420
0.4120

Analytical Services Lab

FM-0243
Page 3/11

QC,0
1
2
3
4
5
6
7
8
9
10

Recovery
92
92
95
94
98
99
98
94
95
92

QC,0
11
12
13
14
15
16
17
18
19
20

Recovery
98
98
97
89
93
94
94
89
95
98

QC,0
21
22
23
24
25
26
27
28
29
30

Recovery
95
97
98
92
92
93
97
97
99
98

QC,1
31
32
33
34
35
36
37
38
39
40

Recovery
97
94
92
94
92
97
96
95
98
95

QC,1
41
42
43
44
45
46
47
48
49
50

Recovery
97
96
97
99
97
98
92
98
99
98

QC,1
51
52
53
54
55
56
57
58
59
60

Recovery
98
97
88
93
94
99
98
95
100
100

Determination of moisture content EEC 71/393


Uncertainty by participation in intercompa
Year
2003
2003
2003
2003
2003
2003
2003
2003
2004
2004
2004
2004
2004
2004
2004
2004

Unit
%
%
%
%
%
%
%
%
%
%
%
%
%
%
%
%
x

Youden
6.6
5.3
5.5
7.0
6.3
12.8
1.4
5.4
17.9
6.0
7.1
6.0
0.7
0.7
0.7
0.7

Ref
6.6
5.3
5.5
7.0
6.3
12.8
1.4
5.4
17.9
6.0
7.1
6.0
0.70
0.70
0.70
0.70

Lab
6.8
5.6
5.3
7.1
6.1
12.6
1.5
5.5
17.6
5.8
7.4
5.8
0.67
0.72
0.68
0.67

sPT (predef)
0.220
0.124
0.147
0.233
0.147
0.469
0.047
0.126
0.476
0.199
0.166
0.220
0.019
0.023
0.021
0.016

etermination of moisture content EEC 71/393 in feed stuff


Uncertainty by participation in intercomparisons
u, lab (k=1)
0.143
0.116
0.111
0.149
0.128
0.265
0.030
0.116
0.370
0.122
0.105
0.122
0.010
0.010
0.010
0.010

u, ref (k=1)
0.093
0.075
0.078
0.099
0.089
0.181
0.020
0.076
0.253
0.085
0.100
0.085
0.010
0.010
0.010
0.010
average
stdev

% Bias
3.0%
5.7%
-3.6%
1.4%
-3.2%
-1.6%
7.1%
1.9%
-1.7%
-3.3%
4.2%
-3.3%
-4.3%
2.9%
-2.9%
-4.3%
-0.1%
3.8%

z
0.9
2.4
-1.4
0.4
-1.4
-0.4
2.1
0.8
-0.6
-1.0
1.8
-0.9
-1.6
0.9
-1.0
-1.9
-0.05
1.39


1.2
2.2
-1.5
0.6
-1.3
-0.6
2.8
0.7
-0.7
-1.3
2.1
-1.3
-2.1
1.4
-1.4
-2.1
-0.09
1.63

Source of
Uncertainty

Symbol

Value

Probability
Distribution

Divisor

%
K

Calibration factor
2.5
at 18 GHz

normal

Drift since last


calibration

0.5

rectangular

1.732050808

Instrumentation
Uncertainty

0.5

normal

50 MHz Reference
1.2
spec.

rectangular

1.732050808

Mismatch loss uncertainties:


M1

Sensor to 50 MHz
0.2
Reference

U-shaped

1.414213562

M2

Sensor to 18 GHz
Generator

5.9

U-shaped

1.414213562

Type-A
Uncertainties

2.1

normal

uC

Combined
Standard
Uncertainty

normal

Expanded
Uncertainty

normal (k=2)

ui
Ci
%
1

1.25

0.29

0.25

0.69

0.14

4.17

1.05

4.55
9.10

Parameter

A
B
C
D

Result, y :
uy

Value

12
160
0.9998
0.45

4265.81

Standard
Absolute
Uncertainty
0.125
0.367
0.00001
0.003

Relative uncertainty
A
1.04%
0.23%
0.00%
0.67%

12.125
160
0.9998
0.45

1.26%
53.66

Varied
Residual
Uncertainty
Relative uncertainty
Relative contribution

12
160.367
0.9998
0.45

12
160
0.99981
0.45

12
160
0.9998
0.453

4310.25
-44.44
53.56
1.24%
68.8%

4275.60
-9.78

4265.86
-0.04

4237.56
28.25

3.3%

0.0%

27.8%

Parameter

A
B
C
D
E
F
G
H
I
J
K
L
M
N

Purity
1 Weighing
2 Weighing
Pipetting 1mL
Pip - Trueness
Pip Reproducibility
Stock Solution 25mL

Value

Standard
Absolute
Uncertainty

P
W (mg)
W (mg)
V1mL

0.999
1100.0
1000.0
1.000
1.000

V25mL

Vol flask - Trueness


Vol flask Repeatability
Vol flask - Volume effect
Intermediate solution 25mL
Vol flask - Trueness
Vol flask Repeatability
Vol flask - Volume effect
Result, y :
uy

25.00
25.00
25.00
V25mL

25.00
25.00
25.00
159.8

Relative uncertainty
A

Purity

1 Weighing 2 Weighing

0.00058
0.1155
0.1155

0.000577928
0.000104973
0.00011547

1.000
1100.00
1000.00

0.0029
0.0100

0.002857738
0.01

0.0163
0.010
0.0212
0.0163
0.010
0.0212
1.05%
1.69

0.999
1100.115
1000.000

0.999
1100.000
1000.115

1.00
1.00

1.000
1.000

1.000
1.000

0.000653197
0.0004
0.000848705

25.00
25.00
25.00

25.000
25.000
25.000

25.000
25.000
25.000

0.000653197
0.0004
0.000848705
Varied
Residual
Contribution
Uncertainty
Relative uncertainty

25.00
25.00
25.00

25.000
25.000
25.000

25.000
25.000
25.000

160.0

159.7

159.9
-0.09
0.3%
1.70
1.06%

-0.18
1.2%

0.18
1.2%

Vol flask - Volume effect


Vol flask Repeatability
Vol flask - Trueness

Vol flask - Volume effect


Vol flask Repeatability
Vol flask - Trueness

Pip Reproducibility

Pip - Trueness

2 Weighing
1 Weighing
Purity
0.0%

10.0%

20.0%

30.0%

40.0%

50.0%

Pip - Trueness
Pip Reproducibility Vol flask - Vol
Trueness
flask Repeatability
Vol flask - Volume effect
Vol flask - Vol
Trueness
flask Repeatability
0.999
0.999
1100.000 1100.000
1000.000 1000.000

0.999
0.999
0.999
1100.000 1100.000 1100.000
1000.000 1000.000 1000.000

0.999
0.999
1100.000 1100.000
1000.000 1000.000

1.003
1.000

1.000
1.010

1.000
1.000

1.000
1.000

1.000
1.000

1.000
1.000

1.000
1.000

25.000
25.000
25.000

25.000
25.000
25.000

25.016
25.000
25.000

25.000
25.01
25.000

25.000
25.000
25.021

25.000
25.000
25.000

25.000
25.000
25.000

25.000
25.000
25.000

25.000
25.000
25.000

25.000
25.000
25.000

25.000
25.000
25.000

25.000
25.000
25.000

25.016
25.000
25.000

25.000
25.01
25.021

160.3

161.4

159.7

159.8

159.7

159.7

159.8

-0.46
7.2%

-1.60
88.4%

0.10
0.4%

0.06
0.1%

0.14
0.6%

Series1

50.0%

60.0%

70.0%

80.0%

90.0%

0.10
0.4%

0.06
0.1%

Vol flask - Volume effect


0.999
1100.000
1000.000
1.000
1.000
25.000
25.000
25.000
25.000
25.000
25.021

159.7
0.14
0.6%

Step

Symbol/
unity

Step

Distribution

0.999
100.0

B -Rectangular
B -Rectangular

Purity
Weighing
Pipetting 1mL

Pip - Trueness
Pip Reproducibility
Stock Solution 25mL

V25mL

25.00

Vol flask - Trueness


Vol flask Repeatability
Vol flask - Volume effect
Intermediate solution 25mL

V25mL

Concentration

mg/L

Concentration

mg/L

25.00
159.8
k=2
159.8

1
2

P
W (mg)
V1mL

xi

1.000
B -Triangular
A - Normal
B -Rectangular
B -Triangular
A - Normal
B -Rectangular
Combined u
Expanded U
Expanded U

Vol flask - Volume effect


Vol flask Repeatability
Vol flask - Trueness
Stock Solution 25mL
Pip Reproducibility
Pip - Trueness
Pipetting 1mL
Weighing
Purity

0%

10%

20%

30%

40%

50%
Relative Contr.

u(x i )

u(x i )

u(x i )/x

Comment

Contribu
tion

0.00058
0.1633

0.06%
0.16%
1.04%

99,9% purity
0,2 mg limit

0.29%
2.34%

+/-0,007mL from specs


0,01 mL repeatability

7.18%
87.89%

+/-0,04mL from specs


0,01 mL repeatability
Volume coeff. Del. T = 14C

0.75%
0.28%
1.27%

uc (mg/L)
U (mg/L)
U (mg/L)

1.70
3.41
3.4

0.0104
0.0029
0.0100
0.0286

0.11%

0.0163
0.010
0.0212
0.0286
uc (%)
U (%)

60%
Relative Contr.

0.11%
1.07%
2.13%

70%

80%

90%

100%

Purity
Weighing
Pipetting 1mL
Pip - Trueness
Pip Reproducibility
Stock Solution 25mL
Vol flask - Trueness
Vol flask Repeatability
Vol flask - Volume effect

Kragten Calibration of instrument

Reading
Zero reading
Calibration factor 1
Calibration factor 2
Correction factor

Quantity
A
B
C
D
E

Value
0.1860
0.0171
0.9808
1.2500
0.0000

u
0.0003
0.0002
0.0012
0.0005
0.0004

Estimate

Unit of
Measure of
Value

0.6

0.5

Temperature difference between parts

Coefficient of thermal deviation expansion CTE and


temperature difference from 20 C

Source
Gauge block (ISO Gr. 2)
Instrument reading resolution
Instrument repeatability

Validation against the following simple example by Dr. J Decker of the INMS Dimensional Metrology Program.
Published at:
Procedure:
1) From simplified example published by J Decker; PUMA Procedure - One Single Iteration:

Distribution and
Evaluation Type

dof

Factor

Uncertainty
u(xi) (m)

Standard uncertainty
u (xi) (m)

Rectangular, B

1.732

0.60

0.346

Rectangular, B

3.464

1.00

0.289

normal, A

11

1.000

0.50

0.500

Rectangular, B

1.732

0.28

0.159

Rectangular, B

1.732

0.22

0.127

Combined Standard Uncertainty:


Expanded Uncertainty k=2:

Coefficient of thermal deviation


expansion CTE and temperature
Temperature difference between
parts
Instrument repeatability
Instrument reading resolution
Gauge block (ISO Gr. 2)

0.703
1.4

f the INMS Dimensional Metrology Program.

cedure - One Single Iteration:

0%

10% 20% 30% 40%

Contribution

24%
17%
51%
5%

3%
m

2) From CLAS uncertainty template, using inputs from the example by J Decker

Series1

40% 50% 60%

ng inputs from the example by J Decker.

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