2005 aerosol sci. technol. zervas e. interlaboratory test of exhaust pm using elpi
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Interlaboratory Test of Exhaust PM Using ELPIE. Zervas
a, P. Dorlhne
a, L. Forti
b, C. Perrin
b, J. C. Momique
c, R. Monier
c, H. Ing
d
B. Lopezd
aRenault, 1, Alle Cornuel, Lardy, France
bInstitut Franais du Ptrole (IFP), Rueil-Malmaison, France
cPSA Peugeot Citren, La Garenne-Colombes, France
dUnion Technique de l'Automobile, du Motocycle et du Cycle (UTAC), Autodrome de Linas
Montlhry, Montlhry, France
Version of record first published: 23 Feb 2007
To cite this article: E. Zervas, P. Dorlhne, L. Forti, C. Perrin, J. C. Momique, R. Monier, H. Ing & B. Lopez (2005):Interlaboratory Test of Exhaust PM Using ELPI, Aerosol Science and Technology, 39:4, 333-346
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Aerosol Science and Technology, 39:333346, 2005
Copyright c American Association for Aerosol ResearchISSN: 0278-6826 print / 1521-7388 online
DOI: 10.1080/027868290930222
Interlaboratory Test of Exhaust PM Using ELPI
E. Zervas,1 P. Dorlhene,1 L. Forti,2 C. Perrin,2 J. C. Momique,3 R. Monier,3
H. Ing,4
and B. Lopez4
1Renault, 1, Allee Cornuel, Lardy, France2Institut Francais du P etrole (IFP), Rueil-Malmaison, France3PSA Peugeot Citr oen, La Garenne-Colombes, France4Union Technique de lAutomobile, du Motocycle et du Cycle (UTAC), Autodrome de Linas-Montlh ery,
Montlhery, France
The Particulate Measurement Programme (PMP) works on thedevelopment of an improved method for the exhaust particulate
matter (PM) measurement, which can include, if feasible and nec-essary, the measurement of particle number. The French PMPsubgroup, composed of IFP, PSA Peugeot-Citroen, Renault, andUTAC, has defined a measurement protocol based on electricallow-pressure impactor (ELPI) and conducted an interlaboratorytest to evaluate its performances. The technical programwas basedon tests carried out on three Euro3 passenger cars(one gasoline op-erating under stoichiometric conditions, one Diesel, and one Dieselequipped with a diesel particulate filter (DPF)) that were testedon the New European Driving Cycle (NEDC). The regulated pollu-tants are also measured, as indicators of test repeatability and goodworking conditions. The interlaboratory reproducibility value ofthetunnel background tests is quite high (337%)due to lowparticlenumbers. Therepeatabilityvalues increase at lowparticle numbersindependently of the vehicle used. On the NEDC, the reproducibil-ity of total particle number is 59, 47, and 131% for the gasoline,
Diesel, and DPF-equipped Diesel vehicles, respectively (compare to67, 29, and 164% for PM collected on filters). These results showthat the protocol used in this study allows a reliable measurementof exhaust particle number in the case of vehicles emitting at leasttwo orders of magnitude more than the tunnel background. In theother cases, the measurement variability is too high, especially forregulatory purposes, without taking into account other metrologi-cal aspects, such as calibration.
INTRODUCTION
Current European regulations are basedon a gravimetricmea-
surement of exhaust particles emitted from Diesel passenger
cars. However, as health concerns and instrument capabilitiesincrease, more research is focused on number and size of emit-
ted particles. The Particle Measurement Programme (PMP) of
theWorkingPartyon Pollutionand Energy (GRPE)of theUnited
Received 1 July 2004; accepted 31 January 2005.Address correspondence to Efthimios Zervas, Renault,1 Allee Cor-
nuel, 91510 Lardy, France. E-mail: [email protected]
Nations at Geneva is mandated to work on the development of an
improved method for the particulate matter (PM) measurement,
which can include, if feasible and necessary, the measurement
of the particle number of the exhaust particles (UNECE 2001).Currently there are many methods for the particle number
and size determination. The method most commonly used in the
case of vehicle exhaust gas are the electrical low-pressure im-
pactor (ELPI; Keskinen et al. 1992; Ahlvik et al. 1998; Pattas
et al. 1998; Khalek 2000; Maricq et al. 2000; Witze et al. 2004),
scanning mobility particle sizer (SMPS; Wang and Flagan 1990)
andparticle counters (Willeke andBaron 1993; Hinds 1999), but
many others are also presented in literature. Burtscher (2001)
and Mohr and Lehmann (2003) give a detailed description of
several analytical methods. Because SMPS has an insufficient
resolution time (some minutes) it cannot be used for the analy-
sis of particle distribution on the New European Driving Cycle
(NEDC).Particles are composed of solid carbonaceous matter, other
solids such as metals, and adsorbed components such as water,
sulphates,and volatile organic compounds (Degobert 1992). The
very fine particles are not always solids but can be condensate
aerosol (Lunders et al. 1998; Matter et al. 1999). Several of the
methods used for the measurement of the particle number can-
not distinguish the solid particles from the volatiles (Burtscher
2001). Forthis reason, several methods, such as thermodenuders
or thermodiluters have been developed to eliminate the volatiles
before measurements (Wehner et al. 2002), but as sampling con-
ditions play a very important role on the particle size measure-
ments (Lunders et al. 1998; Khalek et al. 1999; Maricq et al.
1999; Ntziachristos and Samaras 2000) a standard procedure is
not well established yet.
Several authors evaluate the performances of ELPI.
Marjamaki et al. (2000) evaluate the collection efficiency of
the impactor and the performances of the charger. Maricq et al.
(2000) and Van Gulijk et al. (2003, 2004) perform a comparison
between ELPI and SMPS, while Witze et al. (2004) compares
ELPI with LII and TEOM.
333
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334 E. ZERVAS ET AL.
One specific point before the validation of an analytical
methodis the determinationof its repeatabilityand reproducibil-
ity. Round robin test is themost adequate methodfor thispurpose
(Hoekman et al. 1995; Lanning et al. 1997; Tejada et al. 1997).
However, no interlaboratory comparison on ELPI performances
has yet been presented.
This article presents the results of the French PMP subgroup,
composed by IFP, PSA Peugeot-Citroen, Renault, and UTAC, of
an interlaboratory comparison of particle number measurement
using ELPI. An interlaboratory comparison of particle counters
will be presented in a future article. Three Euro3 passenger cars
(PC) are used in this study: a gasoline vehicle operating un-
der stoichiometric conditions and two Diesel PC, one with and
one without diesel particulate filter (DPF). A pragmatic pro-
tocol based on the European regulatory conditions (tests on the
NEDC)is used. The intralaboratoryvariability, repeatability, and
reproducibility values are presented in the case of the three vehi-
cles. The CO2, fuel consumption (FC), and regulated pollutants
are also measured, and their repeatability and reproducibility
are compared with these of the particle number. Other particu-
lar measurement aspects that can influence the obtained results
and are not very well established today (Choi et al. 2003), such
as accurate day-to-day calibration of the analytical instruments,
are not treated here.
TECHNICAL BACKGROUND OF ELPI
Keskinen et al. (1992) present the operation principles of
ELPI (charger, impactor cut diameters, and electrometer) and
compare it with SMPS. An atomizer was used to generate an
aerosol, which is measured by SMPS and ELPI. This work con-
cludes that both instruments measure the same particle distri-
bution. Marjamaki et al. (2000) evaluates the performances ofELPI at a nominal flow rate of 10 l/min. The impactor, charger,
and their calibration using two differentaerosol-generation tech-
niques are presented. This article presents the impactor collec-
tion efficiency and charger performance (both are estimated sat-
isfactory) and the comparison of the size distribution obtained
by ELPI and SMPS using a di-octyl-sebacate (DOS) aerosol.
Both techniques give similar particle distribution.
ELPI is used for the measurement of exhaust gasparticle
number and distribution, but it is also used to estimate the parti-
cle mass. Ahlvik et al. (1998) uses ELPI to measure the particle
number distribution of a passenger car (model year 1993) and
a heavy-duty engine on two driving cycles (European Driving
Cycle (EDC) and Federal Test Procedure (FTP) for the pas-senger car, and US transient cycle and European Steady-state
Cycle (ESC) for the heavy-duty engine). A differential mobil-
ity analyzer (DMA) is also used for these measurements. The
effective particle density is estimated from the DMA and used
to estimate the particle mass from ELPI distribution; however,
the authors do not examine this method deeply. The effect of
dilution ratio and driving cycle on particle distribution is also
presented. Pattas et al. (1998) examine the effect of DPF on par-
ticle size distribution using ELPI. The influence of sulphur and
Ce content in the fuel on particle distribution is presented on the
NEDC. It is shown that DPF decreases the particle number, but
no information about repeatability is given. Shi et al. (1999) use
ELPI to study the number and distribution of particles emitted
from a Diesel engine tested on an 11-mode steady-state cycle.
A comparison of particle emissions at different engine load and
speeds is performed using ELPI and SMPS, where both tech-
niquesgive similar results. Theauthors present that theestimated
particle mass is 1.31.6 times higher than the mass collected on
filters.
Maricq et al. (2000) presents a comparison of particle distri-
bution of three diesel and three gasoline vehicles (model years
19951997) operating in steady states and on the FTP and mea-
sured by SMPS and ELPI. The effective density of particles
is also estimated and used to calculate the particle mass, but no
comparison with the mass collected on filters is given.
Tsukamoto et al. (2000) uses ELPI to measure the particle num-
ber distribution of a heavy-duty engine. The emitted particle
mass is estimated from ELPI measurements and compared with
the mass collected on filters. Generally, the estimated mass is
1.52 times higher than the mass collected on filters. Khalek
(2000) analyzes the particle number distribution of a heavy-duty
engine on FTP. Similar to Tsukamoto et al. (2000), he concludes
that ELPI overestimates total mass emissions comparing to filter
mass measurements. Andrews et al. (2001) estimate the particle
effective density as a function of size to 1.50.2 g/cm3. Thiswork
concludes that the estimated mass can be very different from the
mass collected on filters. This difference can be very important
for particles bigger than 1 m. One reason is that ELPI overes-
timates the particle number by up to two orders of magnitude
at this particle size. Virtanen et al. (2002) estimate the particleeffective density to 1.11.2 g/cm3 as a function of their size.
This work suggests that dilution has a strong effect on density
values. Ristimaki et al. (2002) use ELPI and SMPS to estimate
the effective density of different aerosols but not of exhaust gas
particles. Choi et al. (2003) use ELPI to study the emissions
of nanoparticles of a HSDI diesel engine and the effect of the
oxidation catalyst on mass and distribution of emitted particles.
Maricq and Xu (2004) use DMA and ELPI to determine the ef-
fective density and fractal dimension of particles emitted from
flames and motor vehicle exhaust gas. The effective densities of
particles emitted from two diesel engines and a direct-injection
SI engine are identical.
However, ELPI has some limitation for particle number mea-surements. Van Gulijk et al. (2001, 2003) presents a list of non-
ideal behavior of ELPI, as particle bounce, wall or interstage
loss, overloading or surface buildup, and losses due to electro-
static effects and to charger nonideal efficiency. Using a steady-
state speed, a continual decrease of small particles and a con-
tinual increase of bigger ones is observed. The authors explain
that this is due to impactor overloading. In our point of view,
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INTERLABORATORY TEST OF EXHAUST PM USING ELPI 335
TABLE 1
Main characteristics of the three passenger cars used
Vehicle 1 Vehicle 2 Vehicle 3
Type Renault Megane Peugeot 307 Peugeot 307
Fuel Gasoline Diesel Diesel
Inertia class (kg) 1130 1360 1360
Displacement (cm3) 1600 1997 1997
Number of cylinders 4 4 4
Valves per cylinder 4 2 4
Injection system MPI Common rail Common rail
Combustion system HDI HDI
Max. power (kW) 66 66 80
Emission limits Euro3 Euro3 Euro3
EGR type Electric closed loop Electric closed loop
After-treatment device TWC DOC DOC + DPF
even if a part of these changes is due to impactoroverloading, an
extremely constant source of particles and different analytical
methods must be combined to validate these conclusions.
Van Gulijk et al. (2004) present that ELPI underestimates the
apparent size of particles and, as a result, that their number is
overestimated.
Three other program must be mentioned. ACEA conducted
two important research programs studying the emissions of fine
particles (ACEA 1999, 2002). In the first study, 11 diesel and
5 gasoline vehicles were tested on NEDC and steady speeds by
two laboratories. The emissions of regulated pollutants and par-
ticle number (determined by SMPS) are presented in the final
report, but no repeatability or reproducibility values are given.
ELPI is not used in this work. Three diesel and four gasoline
passenger cars were tested in the second program. The stability
of ELPI is determined over 18 weeks (one test per week) us-
ing a reference vehicle at a steady speed of 100 km/h. Within
the same laboratory, the repeatability 1.96*RSD value (Relative
Standard Deviation, defined in the experimental section) is 31%
(data extracted from this report). With no apparent explanation,
the particle number decreases by about 35% between the begin-
ning and the end of this program. No other repeatability results
are presented. The third program is the Swiss contribution to
the GRPE particle measurement program (Mohr and Lehmann
2003b). In this study, 24 particle-measurement techniques were
tested using a heavy-duty engine and a combustion aerosol gen-
erator. As only one laboratory is involved, no reproducibility
values can be given. The repeatability values (1.96*RSD) ofELPI during the European Transient Cycle (ETC) are 20 and
57%, respectively, for a configuration without and with a par-
ticulate filter. The respective values are 16% and 39% for the
gravimetric method and 4% and 47% for the CPC. Other tests
on steady-state speeds are also performed. The 1.96*RSD of the
tunnel background measurements are 38% for ELPI, 55% for
the gravimetric method, and 95% for the CPC. The correlation
between particle number measured by ELPI or CPC and particle
mass is poor. The limits of detection (LOD) of ELPI are found
to be very close (90%) to the measured particle concentration
when a particulate filter is used.
EXPERIMENTAL SECTION
Three passenger cars were used in this study: a gasoline PC
operating under stoichiometric conditions (vehicle 1), a diesel
PC (vehicle 2) and a diesel PC equipped with a DPF (vehicle 3).
Table 1 provides their main characteristics. Twenty fiveparts per
million of commercially used, Ce-based additive were added in
the fuel in the case of the DPF-equipped vehicle to decrease the
necessary temperature for the DPF regeneration from about 650
to 550C. The addition of Ce-based additive does not change
the particle distribution.As fuel sulphur can influence the nanoparticle formation due
to sulphates emission, (Mohr2003a), fuels withless than 10 ppm
of sulphur were used for this study. The main characteristics
of these fuels are presented in Table 2. The same lubricant,
which contains less than 0.4% of sulphur, was used for all three
vehicles.
Three tests were performed on the NEDC (cold start)and reg-
ulated pollutants, CO2, and fuel consumption were measured ac-
cording to current European regulations (EU Directive 70/220).
Theexperimental procedureused is thefollowing: a cold NEDC,
24 h of conditioning at 20C, and three cold NEDCs with a con-ditioning of 24 h between each cycle. The results of the last
three NEDC are taken into consideration. In the case of theDPF-equipped diesel PC, a DPF regeneration is performed at
each laboratory before these cycles.
Number and size distribution measurements were performed
using a DEKATI ELPI, covering particle cut size from 8 to
10 m. Three laboratories used an ELPI sampling of 10 l/min,
while Lab 1 used an ELPI sampling of 20 l/min. As thermode-
nuders can induce high particle losses (OICA 2003; Zervas et al.
2004), a DEKATI ejector-type dilutor, heated at 130C with hot
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336 E. ZERVAS ET AL.
TABLE 2
Fuel characteristics
Characteristic Diesel Characteristic Gasoline
Density at 15C (kg/m3) 834 Density at 15C (kg/m3) 762Viscosity at 40C (cSt) 3.00 H/C ratio 1.82Cetane number 53.8 Octane number (MON/RON) 89.1/100.2
Flash Point (C) 82 Distillation (C)Distillation (C) Initial Boiling Point 34.9
Initial Boiling Point 197 10% 62.9
10% 222 20% 77.4
20% 235 50% 107.0
50% 278 90% 144.8
90% 331 95% 154.8
95% 347 Final Boiling Point 184.8
Final Boiling Point 359 E 70C (vol%) 15E 250C (vol%) 30.4 E 100C (vol%) 38.3E 300C (vol%) 69.6 E 150C (vol%) 92.5E 350C (vol%) 95.9 Composition
Composition Total paraffins (vol%) 59.4Sulphur (mg/kg) 8 Total olefins (vol %) 0
Polycyclic Hydrocarbons (wt%) 4.5 Total aromatics (vol%) 49.6
Ce (ppm, the DPF vehicle only) 25 Benzene (vol%) 1.73
Polyaromatics (wt%) 4.5
Total oxygenates (vol%)
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INTERLABORATORY TEST OF EXHAUST PM USING ELPI 337
FIG. 1. Experimental setup.
T4 =
i
n2i [7]
T5 =
i
(ni 1)RSD2i [8]
s L2 =
T2T3 T21T3(k
1)
T5
T3(k 1)T23
T4
[9]
Intralaboratory variability:
ILVi = 1.96 RSDi [10]
Repeatability = 1.96 100
T5/(T3 k)T1/T3
[11]
Reproducibility = 1.96 100
T5/(T3 k) + s L2T1/T3
[12]
where ni = the number of measurements ofi laboratory, mi,j =the value of j measurements ofi laboratory, and k= number oflaboratories.
RESULTS AND DISCUSSION
Emissions of Regulated Pollutants, CO2,and Fuel Consumption
Table 3 presents the emission of regulated pollutants, CO 2,
and FC of the three vehicles. In the case of CO, the mean
exhaust values are 0.7, 0.22, and 0.16 g/km for the gasoline,
diesel, and DPF-equipped diesel vehicle, respectively. The cor-
responding 1.96*RSD intralaboratory variability is within 215,
834%, and 1084%, respectively, for the three vehicles. The
corresponding reproducibility 1.96*RSD value is 13, 21, and
113%, respectively, while the corresponding repeatability value
is 11, 20, and 38%, respectively. The last reproducibility value
is due to the high CO mean value of Lab2 (more than double
that of the other three laboratories, probably due to the deac-
tivation of the oxidation catalyst). Nevertheless, this value is
not considered as an outlier and is not extracted form the cal-
culations. The 1.96*RSD values are more important at lower
emissions.
The 1.96*RSD of intralaboratory hydrocarbon (HC) vari-
ability is within 1116, 1021, and 1050% for the gasoline,
diesel, and DPF-equipped diesel vehicles, respectively. The re-
producibility 1.96*RSD value is 27, 22.5,and 67%, respectively,
for the three vehicles, while the corresponding repeatability
value is 14, 18, and 27.5%, respectively. Once more, the last
reproducibility value is due to the high HC emissions measured
by Lab 2 (probably due to the deactivation of the catalyst), but
this value is not considered as an outlier and is not extractedfrom the calculations. Like in the case of CO emissions, the
RSD values are more important at lower emissions.
The NOx 1.96*RSD intralaboratory variability values are
within 1467, 25.5, and 57% for the gasoline, diesel and
DPF-equipped diesel vehicles, respectively. The reproducibility
1.96*RSD value of these emissions is 47, 11, and 17%, respec-
tively, for the three vehicles, while the corresponding repeata-
bility value is 46, 4, and 6%. The gasoline vehicle has a higher
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TABLE3
Average,foreachlaboratory,emissionofregulatedpollutants,C
O2(ing/km)andfuelconsumption(in
L/100km),intralaboratoryvariability
(IVL),repeatability
(RPT),andreproducibility(RPD)1.96RSDvalues(%)forthe
threevehiclesused
CO
HC
NOx
PM
CO2
FC(inl/100km)
(g/km)
G
D
D+
DPF
G
D
D+
DPF
G
D
D+
DPF
G
D
D+
DPF
G
D
D+DPFG
D
D+
DPF
Lab1
0.67
0.2
0.12
0.116
0.034
0.033
0.045
0.333
0.254
0.0008
0.0233
0.0006
156.4137.1
136.5
6.645.2
5.14
Lab2
0.73
0.24
0.28
0.147
0.032
0.054
0.037
0.344
0.295
0.0275
0.0007
155.8137.9
135.9
6.595.23
5.09
Lab3
0.67
0.23
0.12
0.122
0.035
0.031
0.04
0.319
0.279
0.0011
0.0313
0.001
159.6136.1
135.9
6.75.23
5.18
Lab4
0.73
0.22
0.1
0.112
0.029
0.028
0.051
0.36
0.307
0.0313
0.001
161.7137.6
139.8
6.815.22
5.29
MEAN
0.7
0.22
0.16
0.124
0.032
0.036
0.043
0.339
0.284
0.001
0.0284
0.0008
158.4137.2
137
6.685.22
5.17
ILV(%)
Lab1
11
33.9
24.9
11.4
20.8
9.8
27.5
3.4
6
88.3
12.8
72
1.8
1.6
1.4
1.71.4
1.3
Lab2
2.6
10
10.3
15.8
13.2
13.8
14
2.4
7.4
0
5
169.7
0.8
0.9
0.3
0.71.1
0.4
Lab3
11.9
18.2
84.1
13.7
21.4
50.2
35.7
3.2
5.1
37.2
14.4
261.1
1.4
2.4
1.6
1.32.4
1.3
Lab4
15.2
8.1
41.1
14
10.4
34.9
67.3
5.5
6.5
0
13
122.2
0.7
0.9
1.3
0.80.9
1.3
RPT(%)11.2
20.4
37.6
14.2
18.3
27.5
45.9
4
6.4
60.4
12.9
191
1.2
1.6
1.2
1.21.6
1.2
RPD(%)13.1
21.3
113.1
27.2
22.6
67.2
47.2
10.9
16.7
67.8
29.3
163.9
3.6
1.7
2.9
2.91.4
3.3
G,gasolinevehicle;D,d
iese
lvehicle;D+
DPF,DPF-equippeddieselvehicle.
338
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INTERLABORATORY TEST OF EXHAUST PM USING ELPI 339
intralaboratory variability, repeatability, and reproducibility
(lower 1.96*RSD values) than the two diesel ones due to lower
emissions.
The PM emissions are less repeatable than the previous pol-
lutants in the case of the low-emitting vehicles. The 1.96*RSD
intralaboratory variability values are within 3788 (with the mea-
surements of only two laboratories), 514, and 72261% for the
gasoline, diesel, and DPF-equipped diesel vehicles,respectively.
The reproducibility 1.96*RSD value of these emissions is 67,
29, and 164%, respectively, for the three vehicles, while the
corresponding repeatability value is 60, 12.7, and 191%. The
gasoline vehicle and the DPF-equipped diesel vehicle have high
RSD values due to their very low emissions, which are similar
to the tunnel backgrounds.
The repeatability of CO2 and fuel consumption is better than
this of the regulated pollutants: the 1.96*RSD intralaboratory
variability values are less than 2.4%, with no significant dif-
ferences between CO2 and FC values. The reproducibility and
repeatability 1.96*RSD values of these emissions ranged from
1.2 to 3.6%.
The 1.96*RSD ILV values increase with the decrease of the
mean emitted value in the case of CO, HC, NOx, and PM emis-
FIG. 2. 1.96RSD intralaboratory variability values versus the mean value ofthe regulated pollutants (in g/km), CO2 (in g/km), and fuel consumption (in
l/100 km) of the three vehicles used (PM: particulate matter).
FIG. 3. Particle number of the tunnel background tests before and after each
NEDC for the four laboratories and the three vehicles used.
sions (Figure 2). This correlation seems independent of the ve-
hicle and technology used, even if more data are necessary tovalidate this statement. Within the observed range, this correla-
tion is not valid in the case of CO2 and FC.
Particle Number of the Tunnel Background Tests
Figure 3 presents the particle number of the tunnel back-
grounds, before and after the tests, for the four laboratories and
the three vehicles used. The particle number is quite similar be-
fore and after each NEDC, indicating that the tunnel is found
at its initial stage after each cycle. The difference of the tunnel
temperature before and after the tests is less than 5C; moreover,particle numbers after the tests arenot systematically higherthan
before the tests. These statements indicate that there is no par-
ticle desorption from the higher tunnel temperature after eachNEDC. The tunnel background values before tests are used in
the rest of this work.
Figure 4 presents the particle number of the tunnel back-
ground tests as a function of laboratory. This number depends
on the tunnel used at each laboratory, but it is generally around
1 1011 1/km. The particle number observed in the Lab 3 gaso-line tunnel is the lowest due to its cleanness. The higher num-
bers of the diesel tunnel are due to the particle deposit on the
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340 E. ZERVAS ET AL.
FIG. 4. Tunnel background tests. Lower bars: tunnel background particle
numbersmeasuredat eachlaboratory(mean of three tests); meanvalueof alltests
andELPI limits of detectionand quantification (LOD= 5.3 1010 1/km/LOQ=1.59 1011 1/km) for the three vehicles used. Upper bars: 1.96RSD of eachlaboratory ILV (left bars), and reproducibility and repeatability (right bars). Lab
3 has two tunnels, one for gasoline vehicles (3G) and one for diesel vehicles
(3D).
walls during the tests and the dropping during the measurements
(Andrews et al. 2000). All of these tests are not very repeatable
due to the low particle number; repeatability is also very depen-
dent on the tests performed previously due to the dropping of
the deposed particles (Andrews et al. 2000). For each labora-
tory, the 1.96*RSD intralaboratory variability values are within
43 and 153%. Mohr (2003b) presents an ILV of 38%, but for aheavy-duty engine. The reproducibility 1.96*RSD value of tun-
nel background tests is 200%, while repeatability 1.96*RSD is
163%. Figure 4 shows that the particle number of blank mea-
surements is very near or even below the ELPI LOD or limits
of quantification (LOQ = 3 LOD), which are 5.3 1010 and1.5 1011 1/km, respectively.
Particle Number on the NEDC
Figure 5 presents the particle number of the gasoline vehicle
emitted on the NEDC. The mean total particle numbermeasured
is1.3
10121/km, thesameorderof magnitudeas ACEA (2002).
The 1.96*RSD values are quite high due to low particle numbers(Zervas et al. 2004). The intralaboratory 1.96*RSD variability
values are 2469%, while the corresponding reproducibility and
repeatability values are 59 and 45%. These values are much
lower than those of the tunnel background tests of this vehicle,
which is 174%.
The mean total particle number of the diesel vehicle without
DPF is two orders of magnitude higher than the particle number
of the gasoline vehicle: 1.3 10141/km (Figure 6), as already
FIG. 5. Lower bars: particle number (in 1/km) of the gasoline vehicle mea-sured at each laboratory (mean of 3 tests), mean value of all tests and ELPI
limits of detection and of quantification (LOD = 5.3 1010 1/km/LOQ =1.59 1011 1/km). Blank= mean of all four laboratories blanks for this vehi-cle. Upper bars: blank reproducibility 1.96RSD values (left bars), 1.96RSDintralaboratory variability values (middle bars), and reproducibility and repeata-
bility 1.96RSD values (right bars).
FIG. 6. Lower bars: particle number (in 1/km) of the diesel vehicle measured
at each laboratory (mean of 3 tests), mean value of all tests and ELPI limits of
detection and of quantification (LOD = 5.3 1010 1/km/LOQ= 1.59 10111/km). Blank=mean of allfourlaboratories blanksfor this vehicle.Upperbars:blank reproducibility 1.96RSD values (left bars), 1.96RSD intralaboratoryvariability values (middle bars), and reproducibility and repeatability 1.96RSDvalues (right bars).
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INTERLABORATORY TEST OF EXHAUST PM USING ELPI 341
FIG. 7. Lower bars: particle number (in 1/km) of the DPF-equipped diesel
vehicle measured at each laboratory (mean of 3 tests), mean value (MV) of all
tests, and ELPI limits of detection and of quantification (LOD = 5.3 10101/km/LOQ = 1.59 1011 1/km). Blank= mean of all four laboratories blanksfor this vehicle. Upper bars: blank reproducibility 1.96RSD values (left bars),1.96RSD intralaboratory variability values (middle bars), and reproducibilityand repeatability 1.96RSD values (right bars).
presented (ACEA 2002; Zervas et al. 2004). The intralabora-
tory 1.96*RSD variability values are 1020%. These values are
lower than the corresponding values of the gasoline vehicle due
to higher particle number (Figure 5). The corresponding repro-
ducibility and repeatability 1.96*RSD values are 47 and 14%,
quite low compared to the values of this vehicle tunnel back-ground tests, which is 166%. It must be noted that this vehicle
is representative of the current European fleet (Euro3).
Figure 8 presents that the mean total particle number of the
DPF-equipped diesel vehicle is lower than the particle num-
ber of the two previous ones: 1.8 10111/km, as already pre-sented (ACEA 2002; Zervas et al. 2004). The intralaboratory
1.96*RSD variability values are within 18135%, while the cor-
responding reproducibility and repeatability values are 131 and
96%. These last values are quite close to the tunnel background
tests of this vehicle, which is 137%. The variability values are
higher than the values of the diesel vehicle due to the lower
particle numbers (Figure 3). It must be noted that the particu-
late emissions of this vehicle are representative of the emissionsof the future European passenger cars. The particle number of
this vehicle is very close or even lower than the ELPI limits of
detection or quantification, which induces high values of repro-
ducibility (as in the case of mass measurements). These high
values of reproducibility might not be adapted for regulatory
purposes.
There are some correlations between the 1.96*RSD values
and particle number. The lower curve of Figure 8 shows that the
FIG. 8. Lower curve: intralaboratory standard deviation (1.96SD) of particlenumber versus particle number on the NEDC. Upper curve: intralaboratory
1.96SD of particle number of each ELPI stage. All points for the three vehiclesused.
intralaboratory standard deviation (1.96*SD) of the measured
total particle number on the NEDC is linear with this number,
independent of the vehicle and technology used, indicating that
the error of this number determination using ELPI is quite con-
stant (Zervas et al. 2004). The same linear relation also exists in
the case of particle number 1.96*SD at each ELPI stage (upper
curves of Figure 8).
Figure 9 presents the ELPI 1.96*RSD ILV, reproducibility,and repeatability values as a function of particle number for the
threevehicles tested. Uppercurves show that reproducibility and
repeatability values increase at low particle numbers. The order
observedis tunnel backgrounds blanks>Diesel+DPF>Gaso-line > Diesel. The DPF-equipped diesel vehicle emits slightly
more particles that the blanks, but the 1.96*RSD reproducibil-
ity and repeatability values present a very important increase
between these two points. This statement indicates that ELPI
repeatability is critical for future vehicles. The lower curves
present the intralaboratory variability. The points are more scat-
tered, but three blocks of points are observed: one with low
1.96*RSD values due to high particle numbers (Diesel vehicle),
one with intermediary particle numbers and 1.96*RSD values(gasoline vehicle), and one with very disperse 1.96*RSD values
due to very low particle numbers. This last block corresponds to
DPF-equipped Diesel vehicle and blanks of the three vehicles.
This statement indicates that even within the same laboratory
the 1.96*RSD values are very dispersed in the case of future ve-
hicles. A probable correlation between repeatability of emitted
particle numbers andeach laboratory is searched but no tendency
is found.
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342 E. ZERVAS ET AL.
FIG. 9. Lower curves: ELPI 1.96RSD intralaboratory variability values as afunction of each laboratory average particle number, for the three vehicles used
and the tunnel background tests of each vehicle. Upper curves: ELPI 1.96RSDreproducibility and repeatability values as a function of the average particle
number, for the three vehicles used and the tunnel background tests.
Mean Particle Size Distribution
Figure 10 presents the mean particle size distribution of the
three vehicles. These distributions are quite similar for the four
laboratories. Furthermore, size distribution shows that there is
no nucleation during the measurements. The particle numbers
emitted from the gasoline vehicle (mean value of all tests) are
about one order of magnitude higher than particle numbers oftunnel blanks, up to about 300 nm (Figure 11, lower curves).
For bigger particles, the ratio between exhaust gas particles and
tunnel background ones drops to only two. The particle number
of the diesel vehicle is, on the entire distribution, 23.5 orders of
magnitude higher than the particle number of the tunnel blank
measurements, while the particle number of the DPF-equipped
diesel vehicle remains very close to the blank measurements
for the entire distribution, especially in the area of very fine
particles. For the three vehicles tested, the maximum of this
ratio is observed at the third ELPI stage (63109 nm). Upper
curves of Figure 11 present the ratio between the mean number
of emitted particles and ELPI LOD; the limits of quantification
are also presented. It is clearly shown that the particle numbersof tunnel blanks of the DPF-equipped diesel PC and of the upper
part of the gasoline PC distribution are very close or even lower
to the LOD and LOQ.
The repeatability 1.96*RSD values of each ELPI stage are
4182, 0.6188, and 18259%, respectively, for the gasoline,
diesel, and DPF-equipped diesel vehicles. These values remain
lowerthan 133, 35,and 211%, respectively, forthe three vehicles
at the four first stages of the ELPI, where the majority of the
FIG. 10. Mean particle size distribution of the tunnel background (average of
all tests), and of the gasoline PC (lower curves), diesel PC (middle curves), and
DPF-equipped diesel PC (upper curves) measured at each laboratory (mean of
3 tests).
particles are measured (99, 96, and 97%, respectively, for the
three vehicles). The corresponding reproducibility 1.96*RSD
values are 63178, 20161, and 129208%.
Comparison Between the Particle Number and Mass
ELPI gives the particle distribution, but some authors calcu-
late the particle mass from this distribution. To achieve it the
particle density must be first determined. Different particle den-
sities are used in literature: an average density of 1.0 g/cm3(Shi
et al. 1999; Tsukamotoet al. 2000), or 1.7 g/cm3(Ulfvarson et al.
1997), or 0.5 g/cm3(Witze et al. 2004). But particle density is a
function of size (Ulfvarson et al. 1997; Ahlvik 1998; Andrews
et al. 2001, Virtanen et al. 2002, Witze et al. 2004). The smallerparticles are spherical, and the effective diameter determines the
particle density. The larger the particles are the more primary
particles they contain, leading to much lower values of effective
density (Ahlvik et al. 1998). The values of 1 g/cm 3 at 50 nm
and 0.3 g/cm3 at 300 nm (Witze et al. 2004), or 1.50.2 g/cm3
(Andrews et al. 2001), or 1.20.3 g/cm3 (Maricq et al. 2004) or
1.60.2 g/cm3 (Ahlvik et al. 1998), or 1.11.2 g/cm3 (Virtanen
et al. 2002) are suggested.
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INTERLABORATORY TEST OF EXHAUST PM USING ELPI 343
FIG. 11. Lowercurves:ratio between the mean numbers of theparticles emit-ted from each vehicle and the number of the tunnel background tests. Upper
curves: ratio between the mean particle numbers and the ELPI LOD.
A correlation between the particle mass obtained from cal-
culations and the mass measured on filters is performed. The
conclusions of Tzsukamoto et al. (2000) are that an average
density cannot be assumed for all particle size and that ELPI,
due to the several assumptions used (same density of particles
FIG. 12. Comparison between particle mass collected on filters and estimated from ELPI using the lower, mean, and upper diameter for each stage. Lower
curves: all ELPI stages. Upper curves: six first ELPI stages.
of each size, each particle size of each stage, charge efficiency,
etc.), generally predicts 1.52 times more particle mass. Shiet al.
(1999) found that ELPI and SMPS predict 1.31.6 times more
mass than this collected on filters. Khalek (2000) also concludes
that ELPI overestimates the total mass emissions comparing to
filter mass measurements in the case of a heavy-duty engine.
Andrews et al. (2001) conclude that estimated mass can be very
different from the mass collected on filter. Witze et al. (2004)use
only the first 6 ELPI stages and an empirical method to adjust
particle density to the mass obtained on the filters.
The correlation between the particle mass estimated from
ELPI and the mass collected on filters is presented here. For the
estimation of particle mass from ELPI, the following procedure
is used: the particle mass is the sum of the particle mass of
each stage over the NEDC. The particle mass of each stage is
calculated as the product of particle numbers and the effective
density of each stage. The density values of Ahvil et al. (1998)
are used for these estimations. Two methods are applied: using
all or only the first six ELPI stages, as Witze et al. (2004).
These resultsare presented in Figure12. This figure is divided
in four parts. Lower part of this figure presents the particle mass
estimated from ELPI versus this collected on filters when all
ELPI stages are taken into consideration. The lower, upper, and
mean (defined as Di =mean upper) diameter of each ELPIstage is used for these calculations. The upper curves present the
same estimations using only the six first stages. As the emissions
of diesel vehicle are much higher comparing to the other two
vehicles, the right part of this figure presents the estimation of
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344 E. ZERVAS ET AL.
TABLE 4
The a, b, and r2 of the best-fit lines y = ax+ b of theestimated versus measured particle mass
a b r2
All ELPI stages
Upper diameter 15.60
0.016 0.90
Mean diameter 6.85 0.0066 0.92Lower diameter 0.917 0.0008 0.95
First six ELPI stages
Upper diameter 4.92 0.0048 0.96Mean diameter 2.61 0.0026 0.95Lower diameter 0.454 0.0005 0.93
thediesel vehicle,whilethe left onethe estimationof thegasoline
and diesel + DPF passenger cars.The best-fit linesy= ax+ b and the coefficient of determina-
tion (r2) of the estimated versus measured values are calculated
for each diameter. Table 4 presents the values of a, b, and r2
forthese configurations.
From a macroscopicpoint of view, the use of upper and mean
diameter gives much higherparticlemass than themeasuredone;
the use of lower diameter using only the six first ELPI stages
estimates very lower mass. The use of lower diameter using all
ELPI stages gives the quite good best-fit line: y = 0.917*x0.0008, with r2 = 0.95, and it could predict the measured mass.However, if each vehicle is examined in detail, the obtained
results are less good.
In the case of the diesel vehicle, Figure12 shows that globally
the estimated and measured mass points are found on a straight
line. However:
the use of upper diameter estimates higher mass thanthe measured one (in average 14 times more mass than
the measured one when all the ELPI stages are taken
into account, while the 6 first stages give, on average,
4.6 times more mass), the use of mean diameter also estimates higher mass
than the measured one (in average 6.3 times more mass
than the measured one when all the ELPI stages are
taken into account, while the 6 first stages give in av-
erage 2.4 times more mass), and the use of lower diameter estimates lower mass than the
measured one (in average 15% less than the measured
mass when all the ELPI stages are taken into account,while the 6 first stages give in average 68% less mass
than the measured one).
In the case of the low-emitting particles passenger cars,
Figure 12 shows that ELPI cannot estimate the measured mass.
The points are too dispersed. Moreover:
the use of upper diameter estimates higher mass thanthe measured one in the case of all ELPI stages (6.6
and 11 times more for the gasoline and Diesel+DPFvehiclesrespectively), while theuse of thefirst sixELPI
stages estimates lower mass (in average 47 and 78%
less mass than the measured one for the gasoline and
diesel + DPF vehicles respectively); the use of mean diameter gives similar results as the
upper one (2.6 and 4.3 times more mass for thegasoline
and Diesel+DPF vehicle, respectively, when all ELPIstages are taken into account; while the 6 first stages
give respectively 73% and 89% less mass); and the use of lower diameter estimates lower mass than
the measured one in all cases (all ELPI stages: 71 and
96% less mass than the measured one for the gasoline
and diesel + DPF vehicles, respectively; 6 first ELPIstages: 53 and 98%, respectively, less mass).
A coefficient can be applied to each stage density and adjust
the estimated values to the measured ones. This method can give
slightly better results, but only in the case of the diesel PC, while
the estimated emissions of gasoline and diesel
+DPF vehicle
are not improved. For all the above reasons, the use of ELPIresults is not recommended for the estimation of particle mass.
Comparison Between the Reproducibility andRepeatability of Regulated Pollutants and ParticleNumber Measurements Using ELPI
Figure 13 presents the reproducibility and repeatability of
regulated pollutants and particle numbers determined by ELPI.
The CO2 and FC corresponding values are very low and are not
FIG. 13. Reproducibility (R1) and repeatability (R2) of CO, HC, NOx, PM
(in g/km), and ELPI particle number of the tunnel background tests (Number
Blank) and on the NEDC (1/km, Number ELPI) for the three vehicles used. G,
gasoline; D, diesel; D + DPF, DPF-equipped diesel vehicle.
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INTERLABORATORY TEST OF EXHAUST PM USING ELPI 345
presented in this figure. The 1.96*RSD of particle emissions de-
termined by filters is, for each vehicle, higher than for the other
three regulated pollutants. This difference is not very important
in the case of the diesel vehicle: reproducibility of 14% and
repeatability of 30% against 1224% for the other pollutants.
As the other two vehicles emit very low particle mass, these
differences become quite important: 61 and 69% for the PM
emissions versus 1247% for the other three pollutants in the
case of the gasoline vehicle, and 165 and 190% against 6114%
for the DPF-equipped diesel passenger car. The ELPI repro-
ducibility over the entire NEDC is not very different from that
of PM emissions: 68, 29, and 164% for the PM determination
against 59, 47, and 131% for the ELPI, for the three vehicles,
respectively; the corresponding repeatability values are 61, 14
and 190% for the PM versus 45, 14, and 96% for ELPI.
CONCLUSIONS
The French subgroup of the Particulate Measurement Pro-
gramme, composed by IFP, PSA Peugeot-Citroen, Renault, and
UTAC, conducted an interlaboratory test on the determinationof exhaust particle number using ELPI. Three Euro3 passen-
ger carsone gasoline operating under stoichiometric condi-
tions, one diesel, and one DPF-equipped dieselare tested on
the NEDC. Only the metrological aspects related to repeatability
and detection limits are studied here, without touching on other
features not well established today, such as calibration of ana-
lytical instruments. The results of this study show the following:
The reproducibility 1.96*RSD values are 13, 21, and113%, respectively, for the three vehicles in the case of
CO; 27, 23, and 67% inthecase ofHC;47,11,and17%
in the caseof NOx; and 68, 29, and 164% in the caseof
particles collected on filters. For these pollutants, theintralaboratory variability 1.96*RSD values increase
quite regularly with the decrease of the mean emitted
values, independently of the vehicle and technology
used. The reproducibility 1.96*RSD values of CO2 emis-
sions and fuel consumption are always less than 3.6%
and much lower than the RSD values of the regulated
pollutants. There is very little difference between the
1.96*RSD values of CO2 and FC. There is no obvious
link between the 1.96*RSD values of CO2 emission
or fuel consumption and the vehicle used or the mean
value.
There is no effect of the ELPI sampling volume, be-tween 10 and 20 l/min, as the results of the Lab 1 are
similar to these of the other laboratories. The reproducibility 1.96*RSD of the tunnel background
tests is quite high (200%), due to low particle numbers,
very close to the ELPI detection limits. The 1.96*SD of the measured particle number (on the
NEDC or at each ELPI stage) is linear with this num-
ber, independently of the vehicle and technology used,
indicating that the error of this number determination
is quite constant. On theentire NEDC, thereproducibilityof total particle
number determined by ELPI is 59, 47, and 131% for
the gasoline, diesel, and DPF-equipped diesel vehicles,
respectively. These values are quite similar to those of
the mass particle determination. The particle number emitted from the DPF-equipped
diesel engine is very close or even lower to ELPI LOD
and LOQ. ELPI can be used, with some approximations, to esti-
mate the mass of emitted particles, but only for Euro3
Diesel passenger cars, and it fails to estimate the emit-
ted mass of the low-particle-emitting vehicles. Even if size distribution is given by ELPI with
insufficient reliability, it allows to check that there
is no nucleation mode due to inadequate dilution
parameters. These results show that the protocol used in this study
allows the reliable measurement of exhaust particle
number in the case of vehicles emitting at least two
orders of magnitude more than the tunnel background.
In the other cases, the measurement variability is too
high, especially for regulatory purposes.
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