presentation at the particulates meeting in brussels 27-28 jan 2003 anders christensen / roger...

Presentation at the Particulates Presentation at the Particulates meeting in Brussels 27-28 jan meeting in Brussels 27-28 jan

20032003

Anders Christensen / Roger WesterholmDepartment of Analytical chemistry

Anders Christensen and Roger WesterholmDept. of Analytical chemistry, Stockholm university

DeterminationDetermination of PAH of PAH

Ultrasonic extraction with acetoneUltrasonic extraction with acetone– 5 ml solvent for 10 min

Solvent evaporationSolvent evaporation– reducing solvent volume and change to

toluene Solid phase extraction, SPESolid phase extraction, SPE

– 100 mg Si– elution of a 2 ml fraction containing alifatics

and PAH Analysis on LC-GC-MSAnalysis on LC-GC-MS


LC-GC-MS systemLC-GC-MS system

PTV injector

MS

HPLC-pump UV-detector

HPLC autosampler

Waste

Backflush valve

LC-columnTransfer line

GC injection valve


SRM 1649a Urban dust SRM 1649a Urban dust (National Institute of Standards & Technology, NIST)(National Institute of Standards & Technology, NIST)

0

1

2

3

4

5

6

7

8

Phenan

thre

ne

Anthr

acen

e

Fluora

nthen

e

Pyren

e

Benzo

(a)a

nthra

cene

Chrys

ene/T

riphen

ylene

Benzo

(b)fl

uorant

hene

Benzo

(k)fl

uoranth

ene

Benzo

(e)p

yren

e

Benzo

(a)p

yren

e

Peryle

ne

Inden

o(1,2

,3-cd

)pyr

ene

Diben

z(a,h

)anth

race

ne

Benzo

(ghi)p

eryl

ene

ug

/g Cert

n=5


SRM 2975 Diesel Particulate Matter SRM 2975 Diesel Particulate Matter (National Institute of Standards & Technology, NIST)(National Institute of Standards & Technology, NIST)

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

Phenan

thre

ne

Fluora

nthen

e

Pyren

e

Benzo

(a)a

nthra

cene

Chrys

ene/

Triphen

ylen

e

Benzo

(k)fl

uoranth

ene

Benzo

(e)p

yren

e

Benzo

(a)p

yren

e

Benzo

(ghi)p

eryl

ene

ug

/g Cert

n=6

X 10X 10 X 10

X 10

X 10X 10


Multivariate analysis, Round Robin Multivariate analysis, Round Robin resultsresults

To try and see why there are differences in the results between the different labs, we have tryed to do a multivariate analysis, PCA of the data.

The results of this experiment are not conclusive since thereis not enough data, but there might be some indications that could be intresting to discuss.


Scores plot, UDC resultsScores plot, UDC results

-4

-3

-2

-1

0

1

2

3

-4 -3 -2 -1 0 1 2 3 4 RESULT15, X-expl: 30%,31%

1 2

4

5

6

7 8

9

10

11 12

16

17

18

19

20

21

PC1

PC2 Scores

UDC

LAT

MTC

EMPA

Shell

TUG

VTT


Loadings plot, UDC resultsLoadings plot, UDC results

-0.5

-0.4

-0.3

-0.2

-0.1

0

0.1

0.2

0.3

0.4

-0.4 -0.3 -0.2 -0.1 0 0.1 0.2 0.3 0.4 RESULT15, X-expl: 30%,31%

Sampling temper

Atm. Pressure

Rel. Humidity

Driving distanc

CVS volume

Sample volumeSample flow

PM

Particulate mas

Sum PAH 1Sum PAH 2

PC1

PC2 X-loadings


Scores plot, EUDC resultsScores plot, EUDC results

-3

-2

-1

0

1

2

3

4

-4 -3 -2 -1 0 1 2 3 RESULT17, X-expl: 34%,25%

22 23

25

26

27

28

29

30

31

32 33

37 38

39 40

41

42

PC1

PC2 Scores

EMPA

TUG

VTT

MTC

Shell

LAT


Loadings plot, EUDC resultsLoadings plot, EUDC results

-0.6

-0.4

-0.2

0

0.2

0.4

-0.5 -0.4 -0.3 -0.2 -0.1 0 0.1 0.2 0.3 0.4 RESULT17, X-expl: 34%,25%

Sampling temper

Atm. Pressure

Rel. Humidity

Driving distanc

CVS volume

Sample volumeSample flow

PM

Particulate mas

Sum PAH 1

Sum PAH 2

PC1

PC2 X-loadings


Particle mass VS humidityParticle mass VS humidity

0

0.5

1

1.5

0 20 40 60 80

Rel humidity (%)

Par

t mas

s (m

g)


WP 500 ActivitiesWP 500 Activities

Tasks - PAH analysis of samples from Tasks - PAH analysis of samples from – LDV tests– Alternative fuels– Advanced engines & aftertreatment– Oil consumption

We have received samples from AVL, Volvo and We have received samples from AVL, Volvo and EMPAEMPA

The analysis of samples will probably begin during The analysis of samples will probably begin during the following weeksthe following weeks

Tests at MTC will be performed in FebruaryTests at MTC will be performed in February We have to decide which samples that are most We have to decide which samples that are most

important to analyse important to analyse


presentation at the particulates meeting in brussels 27-28 jan 2003 anders christensen / roger...

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