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Paper Number: 2005-01-2145

Development of an Improved Gravimetric Method for the MassMeasurement of Diesel Exhaust Gas Particles

Efthimios Zervas, Pascal DorlneRenault

Laurent Forti, Cyriaque PerrinIFP

Jean-Claude Momique, Richard MonierPSA

Didier Pingal, Batrice LopezUTAC

Copyright 2005 SAE International

ABSTRACT

The Particulate Measurement Programme (PMP) workson the identification of a method to replace or completethe existing particle mass (PM) measurement method.The French PMP subgroup, composed by IFP, PSAPeugeot-Citron, Renault and UTAC, proposes an

improved gravimetric method for the measurement ofemitted particles, and conducted an inter-laboratory testto evaluate its performances. The technical programmeis based on tests carried out on a Euro3 Dieselpassenger car (PC), tested on the New EuropeanDriving Cycle (NEDC). To achieve low particulate matter(PM) emissions, the EGR is disconnected and aparaffinic fuel is used. The regulated pollutants are alsomeasured. It is shown that the multiple filter weighingand a 0.1 g balance instead of a 1 g one are notnecessary, as the first weighing and the 1 g balanceperformances are satisfactory for type-approvalpurposes. The use of one filter for the entire NEDC and

the decrease of flow through the tunnel from 12 to 9m

3/min increases the collected PM mass, without

influencing the measurement of regulated pollutants.The collected PM mass is around 0.34-0.5 mg withsatisfactory levels of repeatability and reproducibility.These results show that the proposed gravimetricmethod can measure with good precision low PMemissions, at least as low as 8 mg/km, with no changeon the existing facilities and without supplementary cost,investment or staff training on new instruments.

INTRODUCTION

The current measurement of exhaust particles emittedby Diesel vehicles is operated in European Union by a

gravimetric method. But, as emission standards becomemore and more stringent, the current gravimetric methodreaches its limits. European regulations require that themass collected must be between 1 and 5 mg [1]. Theconditions typically used to achieve this target are a flowthrough tunnel of about 12 m

3/min and a flow through

filters of about 27 L/min. Four filters are used for a

particulate matter measurement on the New EuropeanDriving Cycle (NEDC): two (primary and backup) for theurban part of the cycle and two others (primary andbackup) for the extra-urban part. The current balanceshave a readability of 1 g, but a higher readability willprobably be necessary for future regulations.

The Particulate Measurement Programme (PMP) of theWorking Party on Pollution and Energy (GRPE) ofUnited Nations at Geneva, works on the identification ofa method to replace or complete the existing particlemass measurement method. [2]. The French PMPsubgroup, composed by IFP, PSA Peugeot-Citron,

Renault and UTAC, developed such a method andconducted an inter-laboratory procedure to determine itsrepeatability and reproducibility. The use of inter-laboratory tests is the most adequate method for thisdetermination in the case of exhaust gas [3-5].

A Diesel passenger car is used in this study. To obtainlow particulate mass emissions (around 8 mg/km), theexhaust gas re-circulation (EGR) is disconnected and aparaffinic fuel, which produces low PM emissions [6-9],is used. A pragmatic protocol, based on European type-approval Type I test on the NEDC is employed. CO, HC,NOx and CO2 emissions are also measured and theirrepeatability and reproducibility are compared with therepeatability of the PM emissions. The influence of the

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flow through the tunnel, of the multiple weighing and ofthe balance readability is examined. The intra-laboratoryvariability, reproducibility and repeatability on cold andhot cycles of these measurements are also determinedin this work.

EXPERIMENTAL SECTION

As the current gravimetric method is adapted to theEuro3 and Euro4 PM emissions level, a lower emissionvehicle is needed for this enhanced method. To achievelower emissions, a Euro3 Diesel vehicle is used withdisconnected EGR and fed with a paraffinic fuel. Table 1presents the main characteristics of this vehicle used.

Characteristic Value

Type Citron Xsara

Inertia class (kg) 1360

Displacement (cm3) 2000

Number of cylinders 4

Injection system Common rail

Combustion system HDI

Emission limits Euro3

EGR type Disconnected

After-treatment device Oxidation catalyst

Table 1. Main characteristics of the passenger car used.

As fuel composition can influence PM emissions [10-14],a paraffinic fuel, which produces lower PM emissionsthan conventional Diesel fuels [6-9], is used in this study.This fuel has been produced by blending severalparaffinic bases and is sulphur free. Its maincharacteristics are presented in table 2.

The tests are performed on the New European DrivingCycle and the regulated pollutants and CO2 aremeasured according to the current Europeanregulations. The flow through the tunnel is fixed to 9 and12 m

3/min. For each flow through the tunnel, two cold

and three hot cycles are performed. The absence of

water condensation is visually verified in the case of 9m

3/min. CO2concentration in bags is always below 3%.

For these four configurations (9 m3/min cold NEDC, 12

m3/min cold NEDC, 9 m

3/min hot NEDC and 12 m

3/min

hot NEDC), the flow through the filters is set between 35

and 40 L/min. The flow stability was 5%, conformed tothe current regulations.

The results between the four laboratories are regularlyverified and correlated using a reference passenger car.This comparison shows a good correlation: areproducibility and repeatability RSD value of 15% and7% respectively, for PM emissions of 0.028 g/km. As the

facilities of the four laboratories show a good correlation,Lab1 is chosen to work at a flow of 80 L/min to study the

flow influence. To increase the PM collected mass, onlyone filter is used on the entire NEDC. The backup filteris not used, because the filter efficiency is high enoughto collect the majority of particles [15]. Moreover, thecollected PM mass on the backup filter is extremely lowat this low PM emissions, inducing high dispersion. The

filter type is Pallflex TX40, diameter 47mm for the threelaboratories (Lab2, 3 and 4). However, to achieve ahigher flow, a filter type with lower pressure drop(Pallflex T60A20, diameter 47mm) is used in Lab1.Under the experimental conditions used, the filter mediaeffects are not decoupled from the filter flow effects. Thefilter holders are used at ambient temperature and arenot insulated or temperature controlled. Two types ofgrounded balance, with resolution of 0.1 and 1 g, areused. The influence of multiple weighing is also studiedin this work. Temperature in the weighing chambers is

212C, 211C, 255C and 222C respectively forthe four laboratories, while humidity is respectively

555% 505% 4510% 5010%.

Characteristic Value

Density at 15C (kg/m ) 772

Viscosity at 40C (mm2/s) 2.41

Distillation (C)

Initial Boiling Point 222

10% 238

50% 266

90% 287

Final Boiling Point 298

Cetane number >80

Sulphur content (ppm)

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Standard deviation of each laboratory:

)1(

)( 2,2

,

=

ii

jijii

inn

mmnSD (2)

Relative standard deviation of each laboratory:

i

i

imean

SDRSD *100= (3)

=i

jiimnT ,1 (4)

=i

jiimnT 2

,2 (5)

=i

inT3 (6)

=i

inT 2

4 (7)

=i

ii RSDnT 2

5 )1( (8)

=

4

2

3

35

3

2

1326

)1(

)1( TT

kTT

kT

TTTT (9)

Intra-laboratory variability, ii RSDILV *96.1= (10)

Repeatability

31

35 )(*100*96.1

TT

kTT = (11)

Reproducibility

31

635 )(*100*96.1

TT

TkTT +=

(12)

With, ni= number of measurements of laboratory i

mi,j= value of j measurements of laboratory i

k= number of laboratories

RESULTS AND DISCUSSION

AVERAGE EMISSIONS OF CO, HC, NOx, CO2ANDPM

CO emissions

The average CO emissions are 0.26 g/km and 0.28 g/kmin the case of cold NEDC and lower, 0.06 g/km and 0.08

g/km in the case of the hot cycle, respectively for the

flow of 9 and 12m3/min (figure 1). CO emissions are

lower on hot NEDC because the oxidation catalyst isalready activated and oxidizes CO in the beginning ofthe cycle.

1 2 3 4Laboratory

0.00

0.02

0.04

CO

(g/km)

Cold 9

Cold 12

Hot 9

Hot 12

0

40

80

120

1.96

*RSD(%)

Mean Value

Repeatability

Intra LabVariability

Reproducibility

0

20

40

60

AbsDifference(%)

Mean Difference

Cold

Hot

Figure 1. Lower bars: emission of CO (in g/km) for thefour laboratories using 9 and 12 m

3/min on cold and hot

NEDC, and mean values of all tests. Middle bars:1.96*RSD of each laboratory variability (left bars) andreproducibility and repeatability of the vehicle tested(right bars). Only one test is performed in the case ofLab1 for the cold 12m

3/min configuration. Upper bars:

absolute difference between 9 and 12m3/min, expressed

as ABS(100*(CO12-CO9)/CO12).

The 1.96*RSD intra-laboratory variability is within 2%and 68%. The reproducibility 1.96*RSD values are 86,99, 99 and 100% for the four configurations (cold 9m

3/min, cold 12 m

3/min, hot 9 m

3/min and hot 12

m3/min), while the corresponding repeatability values are

30, 23, 42 and 46%. The 1.96*RSD values of the hottests are higher than the cold ones because of the loweremissions [20], but there is no trend between 9 and 12m

3/min for the cold or hot tests.

The mean differences between 9 and 12m3/min are 9

and 28% for the cold and hot cycles. These values arewithin 1.96*RSD repeatability and reproducibility valuesindicating that, within the range tested, there is noinfluence of the flow through the tunnel on CO

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measurements.

HC emissions

The average HC emissions are 0.009 g/km and 0.009g/km (cold cycle) and 0.006 g/km and 0.007 g/km (hot

cycle) for 9 and 12m

3

/min respectively (figure 2). As inthe case of CO, HC emissions are lower on hot NEDCbecause the oxidation catalyst is already activated in thebeginning of the cycle, and thus more efficient for HCoxidation.

1 2 3 4

Laboratory

0.000

0.008

0.016

HC(g/km)

Cold 9

Cold 12

Hot 9

Hot 12

0

100

200

1.96*RSD(%)

Mean Value

Repeatability

Intra LabVariability

Reproducibility0

20

40

Ab

sDifference(%)

Mean Difference

Cold

Hot

Figure 2. Lower bars: emission of HC (in g/km) for thefour laboratories using 9 and 12 m

3/min on cold and hot

NEDC, and mean values of all tests. Middle bars:1.96*RSD of each laboratory variability (left bars) and

reproducibility and repeatability of the vehicle tested(right bars). Upper bars: absolute difference between 9and 12m

3/min, expressed as ABS(100*(HC12-

HC9)/HC12).

The 1.96*RSD intra-laboratory variability of HCemissions is within 5% and 111% for the fourconfigurations (cold 9 m

3/min, cold 12 m

3/min, hot 9

m3/min and hot 12 m

3/min). The reproducibility

1.96*RSD values are 127, 132, 121 and 176% for thefour configurations, while the corresponding repeatabilityvalues are 42, 12, 34 and 35%. The 1.96*RSD values ofthe hot tests are generally slightly higher than those of

the cold ones because of the lower emissions [20], butthere is no trend between the 9 and 12 m

3/min. Lab 1

presents quite high 1.96*RSD variability values becauseone measurement is very different to others. This valueis not eliminated as it is not found to be an outlieraccording to Cohran test [19].

The mean differences between 9 and 12 m3/min are 2

and 12% for the cold and hot cycles. These values arewithin the 1.96*RSD repeatability and reproducibilityvalues indicating that, within the range tested, there isno influence of the flow through the tunnel on HCmeasurements.

NOx emissions

The mean NOx emissions are very high due to EGRdisconnection; they reach 0.86 g/km and 0.87 g/km (coldcycle) and 0.91 g/km and 0.92 g/km (hot cycle) for 9 and12 m

3/min respectively (figure 3). NOx emissions are

similar for hot and cold cycles because there is no NOxafter-treatment.

1 2 3 4

Laboratory

0.0

0.5

1.0

NOx(g/km)

Cold 9

Cold 12

Hot 9

Hot 12

0

4

8

1.9

6*RSD(%)

Mean Value

Repeatability

Intra LabVariability

Reproducibility0

2

4

AbsDifference(%)

Mean Difference

Cold

Hot

Figure 3. Lower bars: emission of NOx (in g/km) for thefour laboratories using 9 and 12 m

3/min on cold and hot

NEDC, and mean values of all tests. Middle bars:1.96*RSD of each laboratory variability (left bars) andreproducibility and repeatability of the vehicle tested(right bars). Upper bars: absolute difference between 9and 12m

3/min, expressed as ABS(100*(NOx12-

NOx9)/NOx12).

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The NOx 1.96*RSD values are lower than the 1.96*RSDof other pollutants, because of the very high emissions.The intra-laboratory 1.96*RSD variability is within 0.3%and 5.1% for the four configurations. The reproducibility1.96*RSD values are 2.9, 7.0, 6.8 and 7.4% respectivelyfor the four configurations (cold 9 m

3/min, cold 12

m

3

/min, hot 9 m

3

/min and hot 12 m

3

/min), while thecorresponding repeatability values are 2.2, 2.0, 3.3 and3.0%. The 1.96*RSD values of the cold and hot tests arequite similar due to the similar NOx emissions.

The mean differences between 9 and 12 m3/min are very

low: 0.8 and 0.6% for the cold and hot cycles. Thesevalues are within the 1.96*RSD repeatability andreproducibility values indicating that, within the rangetested, there is no influence of the flow through thetunnel on NOx measurements.

CO2emissions

The mean CO2 emissions are 132.5 g/km and 133.3g/km (cold cycle) and 119.7 g/km and 119.6 g/km (hotNEDC) for 9 and 12 m

3/min respectively (figure 4). CO2

emissions are lower on hot NEDC because of the lowerfrictions due to the higher oil temperature than on a coldcycle.

1 2 3 4

Laboratory

100

120

140

CO2(g/km)

Cold 9

Cold 12

Hot 9

Hot 12

0

4

8

1.9

6*RSD(%)

Mean Value

Repeatability

Intra LabVariability

Reproducibility

0

1

2

AbsDi

fference(%)

Mean Difference

Cold

Hot

Figure 4. Lower bars: emission of CO2(in g/km) for the

four laboratories using 9 and 12 m3

/min on cold and hotNEDC, and mean values of all tests. Middle bars:

1.96*RSD of each laboratory variability (left bars) andreproducibility and repeatability of the vehicle tested(right bars). Upper bars: absolute difference between 9and 12m

3/min, expressed as ABS(100*(CO2 12-CO2

9)/CO2 12).

The repeatability values of CO2 are better than therepeatability values of CO and HC: the 1.96*RSD intra-laboratory variability values are less than 2.8%. Thereproducibility 1.96*RSD values are less than 6.7%,while the repeatability values are less than 2.0%. Themean differences between 9 and 12 m

3/min are less

than 0.6% for cold and hot cycles. These low valuesindicate that, within the range tested, there is noinfluence of the flow through the tunnel on CO2emissions.

PM emissions

The mean PM emissions are 0.0082 g/km and 0.0082g/km (cold NEDC) and 0.0074 g/km and 0.0072 g/km(hot cycle) for 9 and 12 m

3/min respectively (figure 5).

PM emissions are lower on hot NEDC because theoxidation catalyst is already activated in the beginning ofthe cycle and thus more efficient for SOF oxidation.

1 2 3 4

Laboratory

0

5

10

PM(mg/km)

Cold 9

Cold 12

Hot 9

Hot 12

0

15

30

45

RSD(%)

Mean Value

Repeatability

Intra LabVariability

Reproducibility

0

3

6

AbsDifference(%)

Mean Difference

Cold

Hot

Figure 5. Lower bars: emission of PM (in g/km) for thefour laboratories using 9 and 12 m

3/min on cold and hot

NEDC, and mean values of all tests. Middle

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bars:1.96*RSD of each laboratory variability (left bars)and reproducibility and repeatability of the vehicle tested(right bars). Upper bars: absolute difference between 9and 12m

3/min, expressed as ABS(100*(PM12-

PM9)/PM12).

The 1.96*RSD intra-laboratory variability of PMemissions is within 0.7% and 8.2% for the fourconfigurations tested (figure 5). Taking into account thefour laboratories, the reproducibility 1.96*RSD valuesare 34, 30, 33 and 29% for the four configurations (cold9 m

3/min, cold 12 m

3/min, hot 9 m

3/min and hot 12

m3/min), while the corresponding repeatability values are

2, 4, 8 and 6%. These values are very similar to thoseobtained when only the three laboratories using similarflow through the filters are taken into account(reproducibility 1.96*RSD values: 26, 30, 26 and 26%respectively; repeatability 1.96*RSD values: 2, 4, 8 and8% respectively), indicating that the flow of 35-40 L/minor 80 L/min does not influence the measured PMconcentration. The 1.96*RSD values of the hot tests aregenerally slightly higher than those of the cold onesbecause of the lower emissions [15], but there is notrend between 9 and 12 m

3/min for the cold or hot tests.

The mean differences between 9 and 12 m3/min are 0.2

and 2.2% for the cold and hot cycles (figure 5). Thesevalues are within the 1.96*RSD repeatability andreproducibility values indicating that, within the rangetested, there is no influence of the flow through thetunnel on PM concentration measurements.

Chase et al [15] presents a lower repeatability in filter

measurements and suggests that an important part ofPM mass corresponds to organic vapour which isadsorbed from particles. However, the conditionsbetween the two studies are not the same, as this latterstudy uses DPF equipped vehicles with lower PMemissions (about 4-6 mg/mi).

INFLUENCE OF MULTIPLE WEIGHING

Each loaded and unloaded filter is weighed five times oneach balance. The mean value of the five weighingvalues is compared with the first one (figure 6, only fortwo labs). In the case of the 1 g balance, the mean

difference of the PM mass is very low: only 1.4%. The0.1 g balance gives slightly better results, as the meandifference is 0.16%. Due to the more important mass offilters, these values are even lower in this case; themean differences are around 0.005-0.007% in the caseof unloaded and loaded filters for both balances. Nosignificant difference is observed between the twolaboratories.

The repeatability values of these measurements arevery good: the mean 1.96*RSD of the five weighingvalues is less than 7.0% for the PM mass using the 1 gbalance, while the 0.1 g balance gives 1.1%. The

1.96*RSD values of loaded or unloaded filters areextremely low, less than 0.04% in all cases. Generally,

the 1.96*RSD values are lower in the case of the 0.1 gbalance, while there is no trend between the unloadedand loaded filters.

The above very low differences between the first andfive weighing values suggest that the multiple weighing

is not necessary. Only the first weighing is taken intoaccount for the following tests.

0 5 10 15 20

Test Number

1E-4

1E-3

1E-2

1E-1

1E+0

AbsDifference(%) 1E-4

1E-3

1E-2

1E-1

1E+0

1E+1

1.9

6*RSD(%)

Lab1 Lab4

PM mass 0.1g

PM mass 1g

Unloaded 0.1g

Unloaded 1g

Loaded 0.1g

Loaded 1g1E+0

1E+1

1E+2

Mass(mg)

Figure 6. Bottom curves: mass of unloaded filters andcollected PM mass. Middle curves: absolute difference(%) between the first and the mean weighing values,expressed as Abs(100*(1

st-MV)/1

st). 1

st=first weighing,

MV= mean weighing value. Upper bars: 1.96*RSDvalues of each test multiple weighing. Values of twolaboratories: Lab1 and Lab4, using 0.1 and 1gbalances.

INFLUENCE OF BALANCE READABILITY (0.1 AND 1g)

Figure 7 presents the influence of balance readability(0.1 or 1 g) on filters weighing for Lab1 and Lab4. Themean difference between the two balances is 2.4% inthe case of PM mass. The mean difference between thevalues of unloaded and loaded filters using the two typesof balance is only 0.012% and 0.015%. These lowdifferences indicate that the obtained results arepractically equivalent and suggest that the performancesof the 1 g balance are satisfactory for type-approval

purposes at this PM emission level. Using higher

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balance readability does not improve accuracy of PMmass measurements at PM emission levels of about 8mg/km.

INFLUENCE OF FLOW THROUGH TUNNEL (9 AND 12m

3/min) ON THE COLLECTED MASS

The previous section presented that a balance of 1 g iswell adapted for the measurement of particulate mass atthe emission level of 8 mg/km. However, the tests wereinitially scheduled with a balance of 0.1 g, as webelieved that this balance would be better adapted; thusthe results of the 0.1 g balance are presented here.Figure 8 presents the collected mass on the filters forthe flows through the tunnel of 9 and 12 m

3/min. The

mean collected mass for the three laboratories using aflow through the filters of 35-40 L/min+TX40 filters is0.42 mg and 0.33 mg at 9 m

3/min for the cold and hot

tests respectively, against 0.39 mg and 0.29 mgrespectively at 12 m

3/min. The respective values of the

first laboratory are 0.68 mg, 0.56 mg, 0.59 mg and 0.50mg (figure 8, bottom bars).

0 5 10 15 20

Test Number

0.000

0.001

0.010

0.100

1.000

10.000

Absolute

difference(%)

Lab1

Lab4

Unloaded Filter

Loaded Filter

PM Mass

Figure 7. Influence of balance readability on the filterweighing. Absolute difference (expressed as

Abs(100*(b0.1-b1)/b0.1) between the mean weighing valueof unloaded and loaded filters of a balance of 1 g (b1)and 0.1 g (b0.1).

Middle bars of figure 8 present the normalized PM mass.This is the value of PM mass multiplied by the flowthrough the tunnel divided by the flow through the filters.The differences are now lower than the collected PMmass. The mean values are 0.093, 0.098, 0.085 and0.087 mg*m

3/L for the cold 9 m

3/min, cold 12 m

3/min, hot

9 m3/min and hot 12 m

3/min tests respectively.

Practically, there is no difference between the flows of 9and 12 m

3/min and hot and cold tests (however, cold

tests present slightly higher values than hot ones). Thevalues of the three last laboratories are very close and

the first laboratory is now closer to the other three ones,even if its results are lower. This is probably due to thehigh flow of 80L/min inducing lower collection efficiencyon filters.

The intra-laboratory 1.96*RSD variability values of the

normalized values are quite low: within 0.2-18.2%, 5.9-15.9%, 0.4-8.2% and 3.1-9.2% for the cold 9 m3/min,

cold 12 m3/min, hot 9 m

3/min and hot 12 m

3/min tests

respectively. The reproducibility 1.96*RSD values are27.3, 23.6, 31.1 and 18.9% for the four configurations,while the corresponding repeatability values are 7, 5.5,10.6 and 7.1% (figure 8, upper curves). The 1.96*RSDintra-laboratory variability, reproducibility andrepeatability values of the cold and hot tests are quitesimilar. These values indicate that the normalized PMmass measured from the four laboratories is similarsince it was found within the repeatability limits.

1 2 3 4

Laboratory

0.0

0.3

0.6

Mass(mg)

Cold 9Cold 12

Hot 9

Hot 12

Mean Value

0

20

40

1.96*RSD(%)

Intra Lab Variability

Repeatability

Reproductibility

0.00

0.08

0.16

Mass

*TunnelFlow/

FilterFlow

(mg*m3/L)

Figure 8. Lower bars: influence of flow through thetunnel on PM mass collected on filters. Each laboratorymean value for cold and hot tests, and mean value of alllaboratories. Middle curves: normalized valued PMmass: Mass*Flow through the tunnel/Flow through thefilters. Upper bars: Intra-laboratory variability,reproducibility and repeatability of the normalizedcollected PM mass.

CONCLUSIONS

A pragmatic protocol based on the New European

Driving Cycle is developed to measure PMconcentrations as low as 8 mg/km. This protocol is

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based on the decrease of the flow through the tunnelfrom 12 m

3/min usually employed to 9 m

3/min, and the

increase of the flow through filters from the usual valueof 27 L/min up to 35-40 L/min+TX40 filters or even 80L/min+T60 filters. Based on these experimentalconditions (Euro3 vehicle, 2.0 L engine displacement),

the main conclusions of this study are the following:

- There is no influence of the flow through the tunnelbetween 9 and 12 m

3/min on the measurements of

regulated pollutants and CO2.

- The multiple filter weighing does not improve themeasurements accuracy, as the mean value ispractically identical to the first one.

- The repeatability of the 0.1 and 1 g balances are verygood. The performance of the last one is satisfactory fortype-approval purposes.

- In the case of a flow through the filters of 35-40L/min+TX40 filters, the mean PM mass collected on thefilters is 0.33-0.42 mg with satisfactory levels ofreproducibility (1.96*RSD of 50-58%) and repeatability(1.96*RSD of 6-14%). If the flow through the filtersreaches 80 L/min+T60 filters, the collected mass is 0.56-0.68 mg. Under the conditions used, the collected massis sufficient for future type-approval purposes.

- The proposed gravimetric method can measureprecisely low PM concentrations, at least as low as 8mg/km, with no change on the existing facilities andwithout supplementary cost, investment or staff training

on new instruments.

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Test of Exhaust PM Using ELPI, Aerosol Sci. Technol., In press