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Repeatability and Repeatability and Reproducibility Analysis Reproducibility Analysis of the Round Robin of the Round Robin Results Results

Repeatability and Reproducibility Analysis of the Round Robin Results

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Repeatability and Reproducibility Analysis of the Round Robin Results. The familiarization of the participating laboratories within the project with the specific sampling system use (“particulates” system) - PowerPoint PPT Presentation

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Page 1: Repeatability and  Reproducibility Analysis of the Round Robin Results

Repeatability and Repeatability and Reproducibility Analysis Reproducibility Analysis

of the Round Robin of the Round Robin ResultsResults

Page 2: Repeatability and  Reproducibility Analysis of the Round Robin Results

Round Robin Objectives

The familiarization of the participating laboratories within the project with the specific sampling system use (“particulates” system)

The examination of the consistency of the results obtained when applying this methodology in different physical environments

Page 3: Repeatability and  Reproducibility Analysis of the Round Robin Results

Participating Laboratories

VTT Energy (VTT) – Finland MTC – Sweden IFP – France EMPA – Switzerland Technical University Graz (TUG) –

Austria AEA Technology (AEAT) – UK SHELL – UK Lab of Applied Thermodynamics

(LAT) - Greece

Page 4: Repeatability and  Reproducibility Analysis of the Round Robin Results

Round robin execution table

Laboratory Arrival DayDeparture

Day

VTT 11/09/2001 24/09/2001

MTC 28/09/2001 05/10/2001

IFP 12/10/2001 22/10/2001

EMPA 02/11/2001 09/11/2001

TUG 09/11/2001 20/11/2001

AEAT 29/11/2001 07/12/2001

Shell 08/12/2001 15/12/2002

LAT 16/12/2002 29/01/2002

Page 5: Repeatability and  Reproducibility Analysis of the Round Robin Results

Test Vehicle

VW Golf TDI 1.9 l, M Y 1996 with the oxidation catalyst removed

Fuel: Fulfilling the specification EN590 (Year 2000 specs)

Lubricant: BP Vanellus C4 multi SAE 20W – 50 grade (pre aged for 874 km)

Page 6: Repeatability and  Reproducibility Analysis of the Round Robin Results

Instrumentation

Primary Porous Diluter TYLAN MFC 2920 dilution air mass

flow controller Ageing Chamber Thermodenuder Dekati’s Electrical Low Pressure

Impactor (ELPI) & ELPI Filter Stage Vacuum Pump 2 Ejector dilutors Dekati’s Diffusion Charger (DDC) TSI’s 3022 Condensation Particle

Counter (CPC) Dekati’s Gravimetric Cascade

Impactor (DGI)

Page 7: Repeatability and  Reproducibility Analysis of the Round Robin Results

Testing

Transient Cycles: NEDC Artemis Road

Steady State Modes: 50 km/h 120 km/h

• (road loads)

Page 8: Repeatability and  Reproducibility Analysis of the Round Robin Results

Properties measured in round robin

Particulates System Mass emission rate (mg/km) [DGI] Active surface (cm2/cm3) [DDC] Number Concentration (cm-3) [ELPI stages

1 to 8] Number Concentration (cm-3) [ELPI end

filter stage] Mean aerodynamic diameter (nm) Number concentration (cm-3) [CPC] Total number concentration (cm-3) – mean

& median mobility diameters [SMPS] Regulated emissions:

NOx

CO2

CO HC PM

Page 9: Repeatability and  Reproducibility Analysis of the Round Robin Results

Repeatability – Reproducibility

Analysis proposed in

ASTM E691-99 Standard

Inspection of the repeatability and reproducibility of the results obtained from each laboratory.

Derivation of a precision statement in terms of the total within laboratory and between laboratories variances.

Page 10: Repeatability and  Reproducibility Analysis of the Round Robin Results

Factors affecting the outcome of a test method

The equipment used

The calibration of the equipment

The operators using the equipment

The environmental conditions

Page 11: Repeatability and  Reproducibility Analysis of the Round Robin Results

Precision and Accuracy

Accurate but Accurate but imprecise imprecise

resultsresultsTrue True ValueValue

Precise but Precise but inaccurate inaccurate

resultsresults

Page 12: Repeatability and  Reproducibility Analysis of the Round Robin Results

Within Lab and between

laboratories variability

Within Laboratory Variability: (σ2).

Between Laboratories Variability (στ

2).

Within Laboratory – Between Laboratories Variances reflect: The precision of the test method Any vagueness in the protocol Departures from the protocol

Coefficient of Variance: σ/μ

Page 13: Repeatability and  Reproducibility Analysis of the Round Robin Results

Repeatable Results

Distribution expected due to w ithin lab variability Case 1 Case 2

AveragAverage valuee value

Page 14: Repeatability and  Reproducibility Analysis of the Round Robin Results

Reproducible Results

Lab 1 Lab 2 Lab 3 Lab 4

Overall Overall mean mean valuevalue

Page 15: Repeatability and  Reproducibility Analysis of the Round Robin Results

Repeatability – Reproducibility Statistics and their critical

values

Repeatability Index: k

x… laboratory

Reproducibility Index: h

Critical h* and k* values.

2σx

x

sk

x

22

...xx

n

yyh

Page 16: Repeatability and  Reproducibility Analysis of the Round Robin Results

h plots by laboratories

(reproducibility)

CO2

-2.5

-2

-1.5

-1

-0.5

0

0.5

1

1.5

2

2.5

120

km/h

50 k

m/h

Art

emis

Roa

dN

ED

C C

old

NE

DC

Hot

120

km/h

50 k

m/h

Art

emis

Roa

dN

ED

C C

old

NE

DC

Hot

120

km/h

50 k

m/h

Art

emis

Roa

dN

ED

C C

old

NE

DC

Hot

Art

emis

Roa

dN

ED

C C

old

NE

DC

Hot

120

km/h

50 k

m/h

Art

emis

Roa

dN

ED

C H

ot12

0 km

/h50

km

/hA

rtem

is R

oad

NE

DC

Col

dN

ED

C H

otN

ED

C H

ot12

0 km

/h50

km

/hA

rtem

is R

oad

NE

DC

Col

dN

ED

C H

ot

AEAT EMPA IFP LAT MTC Shell TUG VTT

h s

tati

stic

Page 17: Repeatability and  Reproducibility Analysis of the Round Robin Results

h plot by driving cycles

CO2

-2.5

-2

-1.5

-1

-0.5

0

0.5

1

1.5

2

2.5

AE

AT

EM

PA

IFP

MT

CS

hell

VT

TA

EA

TE

MP

AIF

PLA

TM

TC

She

llT

UG

VT

TA

EA

TE

MP

AIF

PLA

TM

TC

She

llV

TT

AE

AT

EM

PA

IFP

MT

CS

hell

VT

TA

EA

TE

MP

AIF

PLA

TS

hell

VT

T

50 km/h NEDC Hot Artemis Road 120 km/h NEDC Cold

h s

tati

stic

Page 18: Repeatability and  Reproducibility Analysis of the Round Robin Results

k plots by laboratories

(repeatability)

CPC

0

0.5

1

1.5

2

2.5

3

120

km/h

50 k

m/h

Art

emis

Roa

d

NE

DC

Col

d

NE

DC

Hot

120

km/h

50 k

m/h

Art

emis

Roa

d

NE

DC

Col

d

NE

DC

Hot

120

km/h

50 k

m/h

Art

emis

Roa

d

NE

DC

Hot

Art

emis

Roa

d

120

km/h

50 k

m/h

Art

emis

Roa

d

NE

DC

Hot

120

km/h

50 k

m/h

NE

DC

Col

d

50 k

m/h

NE

DC

Hot

Art

emis

Roa

d

NE

DC

Hot

AEAT EMPA IFP LAT MTC SHELL TUG VTT

k st

atis

tic

Page 19: Repeatability and  Reproducibility Analysis of the Round Robin Results

k plots by driving cycles

CPC

0

0.5

1

1.5

2

2.5

3

AE

AT

EM

PA

IFP

MT

C

SH

ELL

TU

G

AE

AT

EM

PA

IFP

MT

CT

UG

VT

T

AE

AT

EM

PA

SH

ELL

AE

AT

EM

PA

IFP

LAT

MT

C

VT

TA

EA

T

EM

PA

IFP

MT

C

SH

ELL

50 km/h NEDC Hot NEDCCold

Artemis Road 120 km/h

k st

atis

tic

Page 20: Repeatability and  Reproducibility Analysis of the Round Robin Results

Repeatability problems in regulated emission results

VTT IFP EMPA

CO2 NEDC cold

CO

HC NEDC cold 50 km/hArtemis & NEDC hot

NOx NEDC cold Artemis

PM Artemis & NEDC hot

Page 21: Repeatability and  Reproducibility Analysis of the Round Robin Results

Reproducibility problems in regulated emission results

EMPA

SHELL

VTT IFPAEA

T

CO2 50 km/h

All cycles

CO 50 km/h

HC NEDC hot

NEDC cold

NOx Artemis

NEDC cold

PM All cycles

Page 22: Repeatability and  Reproducibility Analysis of the Round Robin Results

Within Laboratories

Coefficients Of Variance for Regulated Emissions

Results

Within laboratories COV

0%

10%

20%

30%

40%

50%

60%

CO2 CO HC NOx PM

Emission

% C

OV

Within laboratories COV

0%

10%

20%

30%

40%

50%

60%

CO2 CO HC NOx PM

Emission

% C

OV

120 km/ h 50 km/ h Artemis RoadNEDC Cold NEDC Hot

Within laboratories COV

0%

5%

10%

15%

CO2 CO HC NOx PM

Emission

% C

OV

Page 23: Repeatability and  Reproducibility Analysis of the Round Robin Results

Between Laboratories

Coefficients Of Variance for Regulated Emissions Results

Between Laboratories COV

0%10%20%30%40%50%60%70%

CO2 CO HC NOx PM

Emission

% C

OV

Between Laboratories COV

0%10%20%30%40%50%60%70%

CO2 CO HC NOx PM

Emission

% C

OV

120 km/ h 50 km/ h Artemis RoadNEDC Cold NEDC Hot

Page 24: Repeatability and  Reproducibility Analysis of the Round Robin Results

Repeatability Problems in Particulates instruments

results

MTC IFP EMPA AEAT SHELL TUG LAT

CPC120 km/h

50 km/h

NEDC hot

DDCNEDC cold

50 & 120 km/h

ELPI 1-8

Artemis &

NEDC cold

50 & 120 km/h

NEDC cold

ELPI filter

Artemis &

NEDCELPI

mean dp

120 km/h

SMPS total conc.

120 km/h

50 & 120 km/h

Page 25: Repeatability and  Reproducibility Analysis of the Round Robin Results

Reproducibility Problems in Particulates instruments

results

MTC IFPEMP

AAEAT TUG SHELL

CPC120 km/h

50 km/h

NEDC hot

NEDC cold

DDCArtemis

NEDC

120 km/h

ELPI Filter

Artemis

NEDC

ELPI 1-8

Artemis

NEDC hot

& 120 km/h

NEDC cold

ELPI mean dp

50 km/h

NEDC

cold

DGI total mass

NEDC Hot

Artemis

Page 26: Repeatability and  Reproducibility Analysis of the Round Robin Results

Within laboratories

Coefficients Of Variance for

Particle properties

Within Laboratories COV

0%

50%

100%

150%

200%

% C

OV

Within Laboratories COV

0%

50%

100%

150%

200%

% C

OV

120 km/ h 50 km/ h Artemis RoadNEDC Cold NEDC Hot

Within Laboratories COV

0%

25%

50%

75%

% C

OV

Page 27: Repeatability and  Reproducibility Analysis of the Round Robin Results

Between Laboratories

Coefficients of Variance for

particle properties

Between Laboratories COV

0%

50%

100%

% C

OV

Between Laboratories COV

0%

50%

100%

% C

OV

120 km/ h 50 km/ h Artemis RoadNEDC Cold NEDC Hot

Page 28: Repeatability and  Reproducibility Analysis of the Round Robin Results

Comparison of the Within Laboratory

Coefficients of Variance of the

particulates instruments

results with the regulated PM

ones0123456789

10

CO

V/C

OV

PM

0123456789

10

CO

V/C

OV

PM

120 km/ h 50 km/ h Artemis RoadNEDC Cold NEDC Hot

Page 29: Repeatability and  Reproducibility Analysis of the Round Robin Results

Comparison of the Between Laboratory

Coefficients of Variance of the

particulates instruments

results with the regulated PM

ones0123456789

10

CO

VT/C

OV

T,P

M

0123456789

10

CO

VT/C

OV

T,P

M

120 km/ h 50 km/ h Artemis RoadNEDC Cold NEDC Hot

Page 30: Repeatability and  Reproducibility Analysis of the Round Robin Results

Conclusions - Recomendation

s

Great variability observed in ELPI results (possibly thermodenuder?).

DDC results were the most repeatable and reproducible.

Possible dilution ratio determination problems.

Indications that the method is robust.

Importance of conducting another round robin now that all laboratories are familiar with the protocol.