exercises data

45
Particle Size Lab Result True value Bias 7 91.13 92.1 -0.97 5 91.43 92.1 -0.67 3 91.73 92.1 -0.37 10 91.73 92.1 -0.37 8 91.77 92.1 -0.33 2 92.17 92.1 0.07 9 92.17 92.1 0.07 11 92.25 92.1 0.15 13 92.27 92.1 0.17 1 92.33 92.1 0.23 4 92.33 92.1 0.23 6 92.4 92.1 0.30 14 92.47 92.1 0.37 12 92.67 92.1 0.57 15 92.7 92.1 0.60 average 92.1033 stdev 0.45128 RMS 0.43598 RSD 0.5% %RMS 0.5% Uncertainty (k=2) 1.0% U 0.9% Bitumen Lab 5 6 6.16333333333333 -0.163333333 8 6.02 6.16333333333333 -0.143333333 6 6.09 6.16333333333333 -0.073333333 2 6.12 6.16333333333333 -0.043333333 15 6.12 6.16333333333333 -0.043333333 4 6.13 6.16333333333333 -0.033333333 11 6.14 6.16333333333333 -0.023333333 9 6.16 6.16333333333333 -0.003333333 10 6.16 6.16333333333333 -0.003333333 7 6.17 6.16333333333333 0.0066666667

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Page 1: Exercises Data

Particle SizeLab Result True value Bias

7 91.13 92.1 -0.975 91.43 92.1 -0.673 91.73 92.1 -0.37

10 91.73 92.1 -0.378 91.77 92.1 -0.332 92.17 92.1 0.079 92.17 92.1 0.07

11 92.25 92.1 0.1513 92.27 92.1 0.17

1 92.33 92.1 0.234 92.33 92.1 0.236 92.4 92.1 0.30

14 92.47 92.1 0.3712 92.67 92.1 0.5715 92.7 92.1 0.60

average 92.1033stdev 0.45128 RMS 0.43598RSD 0.5% %RMS 0.5%Uncertainty (k=2) 1.0% U 0.9%0.11651964

BitumenLab

5 6 6.16333333333333 -0.163333338 6.02 6.16333333333333 -0.143333336 6.09 6.16333333333333 -0.073333332 6.12 6.16333333333333 -0.04333333

15 6.12 6.16333333333333 -0.043333334 6.13 6.16333333333333 -0.03333333

11 6.14 6.16333333333333 -0.023333339 6.16 6.16333333333333 -0.00333333

10 6.16 6.16333333333333 -0.003333337 6.17 6.16333333333333 0.006666667

13 6.22 6.16333333333333 0.05666666712 6.25 6.16333333333333 0.086666667

1 6.27 6.16333333333333 0.1066666673 6.27 6.16333333333333 0.106666667

7 5 3 10 8 2 9 11 13 1 4 6 14 12 1590

91

92

93

94

Ringtest OCW - Particle Size Distribution Sieving Method FME 54.07 0,063 mm

Labnr.

Cu

mu

lati

ve

Re

st

(%)

Assigned Value

5 8 6 2 15 4 11 9 10 7 13 12 1 3 145.8

6

6.2

6.4

6.6Ringtest OCW % Bitumen FME 54.07

Labnr

Bit

um

en (

%)

Page 2: Exercises Data

14 6.33 6.16333333333333 0.166666667average 6.16333333stdev 0.09232448 0.089193921RSD 1.5% 1.4%% Uncertainty (k=2) 3.0% 2.9%Uncertainty (k=2) 0.18464896 0.178387842

5 8 6 2 15 4 11 9 10 7 13 12 1 3 145.8

6

6.2

6.4

6.6Ringtest OCW % Bitumen FME 54.07

Labnr

Bit

um

en (

%)

Page 3: Exercises Data

7 5 3 10 8 2 9 11 13 1 4 6 14 12 1590

91

92

93

94

Ringtest OCW - Particle Size Distribution Sieving Method FME 54.07 0,063 mm

Labnr.

Cu

mu

lati

ve

Re

st

(%)

Assigned Value

5 8 6 2 15 4 11 9 10 7 13 12 1 3 145.8

6

6.2

6.4

6.6Ringtest OCW % Bitumen FME 54.07

Labnr

Bit

um

en (

%)

Page 4: Exercises Data

5 8 6 2 15 4 11 9 10 7 13 12 1 3 145.8

6

6.2

6.4

6.6Ringtest OCW % Bitumen FME 54.07

Labnr

Bit

um

en (

%)

Page 5: Exercises Data

PersonA PersonB

Test 1 29.89 30.02Test 2 29.93 29.99Test 3 29.72 30.11Test 4 29.98 29.97Test 5 30.02 30.01Test 6 29.98 29.99Test 7 29.80 30.00Test 8 29.95 29.98Test 9 29.97 30.04

Test 10 29.91 30.07

Page 6: Exercises Data

ID Pipet MICROPIP 32Volume pipet: 100-1000 µl

Date 4/7/2023

z (µl/mg) = 1.0027 ml/g Correction factor for T and pressure

Weighings

Measurements (mg) Nominal 50% Smallest

1000 µL 500 µL 100 µL1 987.7 498.7 99.22 992.0 498.4 99.13 993.3 496.3 99.74 991.1 496.2 99.05 986.3 497.1 100.16 987.4 496.3 99.67 991.2 496.6 100.08 991.1 495.3 99.99 989.0 496.3 98.3

10 989.8 497.1 99.5

Page 7: Exercises Data

a

Our result

Result (ng/mL) ue (ng/mL)Aluminium 110.3 5.6Arsenic 67.2 3.4Zinc 81.3 3.8

Page 8: Exercises Data
Page 9: Exercises Data

Values 82.5 82.5 81.7 81.0 80.8 80.6 78.4Sorted 78.4 80.6 80.8 81.0 81.7 82.5 82.5Min 78.4Max 86.8Range 8.4Qexp 0.5 0.3n=8

Page 10: Exercises Data

86.886.8

Page 11: Exercises Data
Page 12: Exercises Data

Validation Spreadsheet

issued on: 12/03/2007revised on: 13/04/2008

Analytical Services Lab FM-0243Page 5/11

sCRM: ERM-BD 273 Toasted Bread mg/l

m CRM 425 ng/g µg/lU CRM: 29 ng/g ng/l

Number Date (dd-mm-yy) Results %1 04-Jun-06 427 °C2 04-Jun-06 413 °3 04-Jun-06 4474 04-Jun-06 4275 04-Jun-06 4496 04-Jun-06 4097 04-Jun-06 4518 04-Jun-06 4239 04-Jun-06 439

10 04-Jun-06 442

Page 13: Exercises Data

Validation Spreadsheet

issued on: 12/03/2007revised on: 13/04/2008

Analytical Services Lab FM-0243Page 5/11

Number Date (dd-mm-yy) Results1 11-Jun-06 4022 18-Jun-06 4183 25-Jun-06 4444 02-Jul-06 4555 09-Jul-06 4136 16-Jul-06 4447 23-Jul-06 4608 30-Jul-06 4219 06-Aug-06 450

10 13-Aug-06 40811 20-Aug-06 43912 27-Aug-06 45513 03-Sep-06 416

Page 14: Exercises Data

Validation Spreadsheet

issued on: 12/03/2007revised on: 13/04/2008

Analytical Services Lab FM-0243Page 3/11

Number1 0.38802 0.43803 0.32704 0.31305 0.39506 0.40407 0.38508 0.39309 0.3420

10 0.4120

Clow (ng/g)

Page 15: Exercises Data

QC,0 Recovery QC,0 Recovery QC,0 Recovery QC,11 92 11 98 21 95 312 92 12 98 22 97 323 95 13 97 23 98 334 94 14 89 24 92 345 98 15 93 25 92 356 99 16 94 26 93 367 98 17 94 27 97 378 94 18 89 28 97 389 95 19 95 29 99 39

10 92 20 98 30 98 40

Page 16: Exercises Data

Recovery QC,1 Recovery QC,1 Recovery97 41 97 51 9894 42 96 52 9792 43 97 53 8894 44 99 54 9392 45 97 55 9497 46 98 56 9996 47 92 57 9895 48 98 58 9598 49 99 59 10095 50 98 60 100

Page 17: Exercises Data

Determination of moisture content EEC 71/393 in feed stuffUncertainty by participation in intercomparisons

Year Unit Youden Ref Lab2003 % 6.6 6.6 6.8 0.2202003 % 5.3 5.3 5.6 0.1242003 % 5.5 5.5 5.3 0.1472003 % 7.0 7.0 7.1 0.2332003 % 6.3 6.3 6.1 0.1472003 % 12.8 12.8 12.6 0.4692003 % 1.4 1.4 1.5 0.0472003 % 5.4 5.4 5.5 0.1262004 % 17.9 17.9 17.6 0.4762004 % 6.0 6.0 5.8 0.1992004 % 7.1 7.1 7.4 0.1662004 % 6.0 6.0 5.8 0.220

% 0.7 0.70 0.67 0.019% 0.7 0.70 0.72 0.023% 0.7 0.70 0.68 0.021% 0.7 0.70 0.67 0.016

sPT (predef)

Page 18: Exercises Data

Determination of moisture content EEC 71/393 in feed stuffUncertainty by participation in intercomparisons

u, lab (k=1) u, ref (k=1) % Bias z0.143 0.093 3.0% 0.90.116 0.075 5.7% 2.40.111 0.078 -3.6% -1.40.149 0.099 1.4% 0.40.128 0.089 -3.2% -1.40.265 0.181 -1.6% -0.40.030 0.020 7.1% 2.10.116 0.076 1.9% 0.80.370 0.253 -1.7% -0.60.122 0.085 -3.3% -1.00.105 0.100 4.2% 1.80.122 0.085 -3.3% -0.90.010 0.010 -4.3% -1.60.010 0.010 2.9% 0.90.010 0.010 -2.9% -1.00.010 0.010 -4.3% -1.9

average -0.1% -0.05stdev 3.8% 1.39

Page 19: Exercises Data

Determination of moisture content EEC 71/393 in feed stuffUncertainty by participation in intercomparisons

ζ1.22.2-1.50.6-1.3-0.62.80.7-0.7-1.32.1-1.3-2.11.4-1.4-2.1

-0.091.63

Page 20: Exercises Data

Value

± %

K 2.5 normal 2

D 0.5 rectangular 1.7320508075689

I 0.5 normal 2

R 1.2 rectangular 1.7320508075689

Mismatch loss uncertainties:

0.2 U-shaped 1.4142135623731

5.9 U-shaped 1.4142135623731

A 2.1 normal 2

normal

U normal (k=2)

Symbol Source of Uncertainty

Probability Distribution Divisor

Calibration factor at 18 GHz

Drift since last calibration

Instrumentation Uncertainty

50 MHz Reference spec.

M1 Sensor to 50 MHz Reference

M2 Sensor to 18 GHz Generator

Type-A Uncertainties

uC Combined Standard Uncertainty

Expanded Uncertainty

Page 21: Exercises Data

1 1.25

1 0.29

1 0.25

1 0.69

Mismatch loss uncertainties:

1 0.14

1 4.17

1 1.05

4.55

9.10

Ci

ui

± %

Page 22: Exercises Data

Parameter Value Standard Relative uncertaintyAbsolute

Uncertainty A

A 12 0.125 1.04% 12.125B 160 0.367 0.23% 160C 0.9998 0.00001 0.00% 0.9998D 0.45 0.003 0.67% 0.45

Result, y : 4265.81 1.26% Varieduy 53.66 Residual

UncertaintyRelative uncertaintyRelative contribution

Page 23: Exercises Data

B C D

12 12 12160.367 160 1600.9998 0.99981 0.9998

0.45 0.45 0.453

4310.25 4275.60 4265.86 4237.56-44.44 -9.78 -0.04 28.2553.56

1.24%68.8% 3.3% 0.0% 27.8%

Page 24: Exercises Data

Parameter Value StandardAbsolute

Uncertainty

A Purity P 0.999B 1 Weighing W (mg) 1100.0C 2 Weighing W (mg) 1000.0

D Pipetting 1mL

E Pip - Trueness 1.000F Pip Reproducibility 1.000

G Stock Solution 25mL

H Vol flask - Trueness 25.00I Vol flask Repeatability 25.00J Vol flask - Volume effect 25.00K Intermediate solution 25mL

L Vol flask - Trueness 25.00M Vol flask Repeatability 25.00N Vol flask - Volume effect 25.00

Result, y : 159.8uy

V1mL

V25mL

V25mL

Page 25: Exercises Data

Relative uncertainty

A B C D

Purity 1 Weighing 2 Weighing0.00058 0.000577928197387013 1.000 0.999 0.999

0.1155 0.000104972776216296 1100.00 1100.115 1100.000

0.1155 0.000115470053837925 1000.00 1000.000 1000.115

0.0029 0.00285773803324704 1.00 1.000 1.000

0.0100 0.01 1.00 1.000 1.000

0.0163 0.000653197264742181 25.00 25.000 25.000

0.010 0.0004 25.00 25.000 25.000

0.0212 0.00084870489570875 25.00 25.000 25.000

0.0163 0.000653197264742181 25.00 25.000 25.000

0.010 0.0004 25.00 25.000 25.000

0.0212 0.00084870489570875 25.00 25.000 25.000

1.05% Varied 159.9 160.0 159.71.69 Residual -0.09 -0.18 0.18

Contribution 0.3% 1.2% 1.2%Uncertainty 1.70

Relative uncertainty 1.06%

Purity

1 Weighing

2 Weighing

Pip - Trueness

Pip Reproducibility

Vol flask - Trueness

Vol flask Repeatability

Vol flask - Volume effect

Vol flask - Trueness

Vol flask Repeatability

Vol flask - Volume effect

0.0% 10.0% 20.0% 30.0% 40.0% 50.0% 60.0% 70.0% 80.0% 90.0%

Row 22

Page 26: Exercises Data

E F G H I J K L M

Pip - Tru Pip Reproducibility Vol flask Vol flask Vol flask - Volume efVol flask Vol flask 0.999 0.999 0.999 0.999 0.999 0.999 0.999

1100.000 1100.000 1100.000 1100.000 1100.000 1100.000 1100.000

1000.000 1000.000 1000.000 1000.000 1000.000 1000.000 1000.000

1.003 1.000 1.000 1.000 1.000 1.000 1.000

1.000 1.010 1.000 1.000 1.000 1.000 1.000

25.000 25.000 25.016 25.000 25.000 25.000 25.000

25.000 25.000 25.000 25.01 25.000 25.000 25.000

25.000 25.000 25.000 25.000 25.021 25.000 25.000

25.000 25.000 25.000 25.000 25.000 25.016 25.000

25.000 25.000 25.000 25.000 25.000 25.000 25.01

25.000 25.000 25.000 25.000 25.000 25.000 25.021

160.3 161.4 159.7 159.8 159.7 159.7 159.8-0.46 -1.60 0.10 0.06 0.14 0.10 0.067.2% 88.4% 0.4% 0.1% 0.6% 0.4% 0.1%

Purity

1 Weighing

2 Weighing

Pip - Trueness

Pip Reproducibility

Vol flask - Trueness

Vol flask Repeatability

Vol flask - Volume effect

Vol flask - Trueness

Vol flask Repeatability

Vol flask - Volume effect

0.0% 10.0% 20.0% 30.0% 40.0% 50.0% 60.0% 70.0% 80.0% 90.0%

Row 22

Page 27: Exercises Data

N

Vol flask - Volume effect0.999

1100.000

1000.000

1.000

1.000

25.000

25.000

25.000

25.000

25.000

25.021

159.70.14

0.6%

Page 28: Exercises Data

Step Step Distribution

1 Purity P 0.999 B -Rectangular2 Weighing W (mg) 100.0 B -Rectangular

3 Pipetting 1mL 1.000Pip - Trueness B -TriangularPip Reproducibility A - Normal

4 Stock Solution 25mL 25.00 B -RectangularVol flask - Trueness B -TriangularVol flask Repeatability A - NormalVol flask - Volume effect B -Rectangular

5 Intermediate solution 25mL 25.00

Concentration mg/L 159.8 Combined u

k=2 Expanded U

Concentration mg/L 159.8 Expanded U

Symbol/ unity

xi

V1mL

V25mL

V25mL

Purity

Weighing

Pipetting 1mL

Pip - Trueness

Pip Reproducibility

Stock Solution 25mL

Vol flask - Trueness

Vol flask Repeatability

Vol flask - Volume effect

0% 10% 20% 30% 40% 50% 60% 70% 80% 90% 100%

Relative Contr.

Page 29: Exercises Data

Comment

0.00058 0.06% 99,9% purity 0.29%0.1633 0.16% 0,2 mg limit 2.34%

0.0104 1.04%

0.0029 +/-0,007mL from specs 7.18%0.0100 0,01 mL repeatability 87.89%

0.0286 0.11%

0.0163 +/-0,04mL from specs 0.75%0.010 0,01 mL repeatability 0.28%0.0212 Volume coeff. Del. T = 14°C 1.27%

0.0286 0.11%

uc (%) 1.07% 1.70

U (%) 2.13% U (mg/L) 3.41

U (mg/L) 3.4

u(xi) u(xi) u(xi)/xContribu

tion

uc (mg/L)

Purity

Weighing

Pipetting 1mL

Pip - Trueness

Pip Reproducibility

Stock Solution 25mL

Vol flask - Trueness

Vol flask Repeatability

Vol flask - Volume effect

0% 10% 20% 30% 40% 50% 60% 70% 80% 90% 100%

Relative Contr.

Page 30: Exercises Data

Purity###

Weighing###

Pipetting 1mL###

Pip - Trueness###

Pip Reproducibility###

Stock Solution 25mL###

Vol flask - Trueness###

Vol flask Repeatability###

Vol flask - Volume effect###

Page 31: Exercises Data

Kragten Calibration of instrument

Quantity Value uReading A 0.1860 0.0003Zero reading B 0.0171 0.0002Calibration factor 1 C 0.9808 0.0012Calibration factor 2 D 1.2500 0.0005Correction factor E 0.0000 0.0004

Page 32: Exercises Data
Page 33: Exercises Data

Source

Estimate

Gauge block (ISO Gr. 2) 0.6 µm

Instrument reading resolution 1 µm

Instrument repeatability 0.5 µm

Temperature difference between parts 1 °C

8 °C

Unit of Measure of

Value

Coefficient of thermal deviation expansion CTE and temperature difference from 20 ºC

Page 34: Exercises Data

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:

Page 35: Exercises Data

dof Factor

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: 0.703

Expanded Uncertainty k=2: 1.4

Distribution and Evaluation Type

Uncertainty u(xi) (µm)

Standard uncertainty u (xi) (µm)

Gauge block (ISO Gr. 2)

Instrument reading resolution

Instrument repeatability

Temperature difference between parts

Coefficient of thermal deviation expansion CTE and temperature difference from 20 ºC

0% 10% 20% 30% 40% 50% 60%

Column I

Page 36: Exercises Data

Validation against the following simple example by Dr. J Decker of the INMS Dimensional Metrology Program.

1) From simplified example published by J Decker; PUMA Procedure - One Single Iteration:

Gauge block (ISO Gr. 2)

Instrument reading resolution

Instrument repeatability

Temperature difference between parts

Coefficient of thermal deviation expansion CTE and temperature difference from 20 ºC

0% 10% 20% 30% 40% 50% 60%

Column I

Page 37: Exercises Data

Contribution

24%

17%

51%

5%

3%

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

µm

Gauge block (ISO Gr. 2)

Instrument reading resolution

Instrument repeatability

Temperature difference between parts

Coefficient of thermal deviation expansion CTE and temperature difference from 20 ºC

0% 10% 20% 30% 40% 50% 60%

Column I

Page 38: Exercises Data

Gauge block (ISO Gr. 2)

Instrument reading resolution

Instrument repeatability

Temperature difference between parts

Coefficient of thermal deviation expansion CTE and temperature difference from 20 ºC

0% 10% 20% 30% 40% 50% 60%

Column I

Page 39: Exercises Data

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