Progress in Energy and Combustion Science 29 (2003) 635–672

www.elsevier.com/locate/pecs

Particulate matter mass measurements for low emitting diesel

powered vehicles: what’s next?
Elias Vouitsis, Leonidas Ntziachristos, Zissis Samaras*
Laboratory of Applied Thermodynamics, Department of Mechanical Engineering, Aristotle University,
P.O. Box 458, 54124 Thessaloniki, Greece
Received 20 November 2002; accepted 4 August 2003

Abstract
Legislation word-wide imposes stringent emission standards for particulate matter emitted by diesel engines, as an outcome
of evidence associating emitted particulate with a series of adverse health effects. Such emission standards call for significant
reductions in the particulate matter emission levels for small and large on-road diesel vehicles. In fact, emission levels adopted
for the near future are so low that the existing, regulated procedures might not be sensitive enough to accurately determine the
absolute level of emissions. In this regard, extensive research is conducted in the direction of both improving existing
procedures and developing alternative methods for more sensitive particulate matter measurements. This review paper
summarizes the developments in the area and provides an outlook to the future. At first, the character of diesel particulate matter
(DPM) is shortly discussed, mainly to show that the complex nature of emitted particulate is responsible for a series of
implications when its quantitative determination is considered. Secondly, the regulated procedure for sampling and
measurement of DPM is reviewed and its main qualities and shortcomings are presented. The recent technical advances aimed
at improving the characteristics of the reference procedure in the measurement of ultra-low emission levels are then presented.
Next the presentation of alternative methods follows which are gradually incorporated in regulations for particulate matter
sampling. The strength of these techniques is that only a small fraction of exhaust is sampled and conditioned before
measurement, hence significantly reducing the cost compared to the reference procedure. In addition to sampling, the
determination of the actual particulate mass emitted is an area which has attracted significant developments. The most relevant
instrumentation for DPM determination is also described and their potential for application in emissions certification is
examined based on published evidence. Finally, the cost of the different sampling and instrumentation techniques is compared
to demonstrate the cost-effectiveness of each option.
q 2003 Elsevier Ltd. All rights reserved.
Keywords: Emissions; Particle; Particulate; Sampling; Emission certification; Type approval; Real-time measurements

Contents
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 636
2. Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 638
2.1. DPM properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 638
2.2. Quality definitions for DPM characterization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 640
3. The reference method for DPM sampling: the full-flow sampling system . . . . . . . . . . . . . . . . . . . . . . 640
3.1. General description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 640
3.2. Quality of the full-flow dilution method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 641
3.3. Sources of variation for DPM determination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 642
3.4. Overview of the existing reference procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 644

* Corresponding author. Tel.: þ 30-2310-996014; fax: þ 30-2310-996019.

E-mail address: zisis@eng.auth.gr (Z. Samaras).

0360-1285/$ - see front matter q 2003 Elsevier Ltd. All rights reserved.
doi:10.1016/j.pecs.2003.08.002
636 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672

3.5. Provisions to the reference method introduced by new legislation. . . . . . . . . . . . . . . . . . . . . . . . 645

3.5.1. Dilution air pre-conditioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 645
3.5.2. PM sampling probe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 646
3.5.3. PM collection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 646
3.5.4. Sample filter conditioning and weighing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 648
4. Alternative sampling techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 649
4.1. Description of the partial flow sampling systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 649
4.2. Concepts for PFSSs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 649
4.2.1. Isokinetic systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 649
4.2.2. Flow controlled systems with concentration measurements . . . . . . . . . . . . . . . . . . . . . . . 650
4.2.3. Flow controlled systems with flowrate measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . 650
4.3. Characteristics and quality . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 650
4.4. Comparison to CVS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 651
4.4.1. PFSS optimization in comparison to CVS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 652
4.4.2. Comparison of absolute levels of PM emissions between CVS and PFSS . . . . . . . . . . . . 654
4.5. Summarizing table . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 655
5. Alternative DPM determination methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 655
5.1. Techniques based on filter heating and gas analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 658
5.2. Optical techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 658
5.2.1. Light-extinction methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 659
5.2.2. Light scattering photometry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 660
5.2.3. Laser induced incandescence (LII) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 660
5.2.4. Photoacoustic spectroscopy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 660
5.3. Fast-response flame ionization detection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 661
5.4. Tapered element oscillating microbalance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 662
5.5. Quartz crystal microbalance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 664
5.6. DMM-230 mass monitor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 664
5.7. Comparison of mass measurement techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 665
6. Cost of PM measurement facilities . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 666
7. Summary and concluding remarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 667
Acknowledgements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 668
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 668

1. Introduction health consequences. There is yet no firm opinion as to

Internal combustion engines used in motorized transport
are a major source of ambient particulate matter (PM).
Diesel engines in particular have been recognized as the
most significant source and have been subjected to
regulation. These engines are mainly applied to heavy-
duty powertrains because they are reliable, durable and have
high fuel efficiency. In addition, they begin to make major
inroad in passenger car market, particularly in Europe and in
parts in Southeast Asia [1,2]. In contrast, diesel passenger
cars comprise a small share of the United States (US) fleet,
making up just 0.1% of sales while diesel light trucks have
captured roughly 4% of the market [3,4].
Diesel particulate matter (DPM) is a complex mixture of
solid material (soot) produced during combustion and
volatile organic and inorganic material added as the exhaust
gases cool down. Due to the complexity in DPM nature, it is
rather impossible to provide a deterministic definition
according to its chemical or physical properties. Lack of a
definition complicates the study of its environmental and
which DPM components are responsible for detrimental
health effects [5], despite the large-scale relevant studies.
Lloyd and Cackette [6] have extensively reviewed
epidemiological studies associating DPM with specific
health related indices. Their review concluded that DPM
is responsible for both carcinogenic (esp. lung) and non-
carcinogenic (pulmonary and cardiovascular) effects. How-
ever, this work has been criticized [7] in that it draws
explicit conclusions neglecting the uncertainty associated
with some of its main hypotheses. But even the US
Environmental Protection Agency (EPA), in their long
expected report [8], have characterized diesel exhaust as
likely to be carcinogenic to humans and reported acute non-
carcinogenic effects to susceptible groups of people
(asthmatics, elderly, etc.).
Based on such evidence, legislation has imposed
stringent PM emission limits for the near future, pushing
both the engine and oil industries to improve the quality of
their products. Future steps in the heavy duty vehicles
(HDVs) emission regulation have been decided in
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672 637

Nomenclature HDV heavy duty vehicle

HE heat exchanger
AE specific optical extinction in Beer – Lambert
HEPA high efficiency particulate air filter
law (Eq. (3))
ICE internal combustion engine
F frequency of oscillation of TEOM element. F0
IF inorganic fraction
is the initial frequency and Ft is the frequency
IR infrared range or radiation
at moment t (Eq. (4))
ISP isokinetic sampling probe
G mass flowrate (Eqs. (1) and (2)) of exhaust gas
LDV light duty vehicle
(exh), intake air to the engine (air), fuel
LII laser-induced incandescence
consumed (fuel), total diluted sample in a
NDIR non-dispersive infrared analyzer or technique
PFSS (tot), dilution air consumed (dl)
PB pressure blower
HC hydrocarbon mass concentration in raw exhaust
PFSS partial flow sampling system
(Eq. (5))
PM particulate matter
I light beam intensity (Eq. (3)). I0 is the incident
PDP positive displacement pump
light and IT is the transmitted light
PSP particulate sampling probe
K0 calibration constant for the tapered element
QCM quartz crystal microbalance
(Eq. (4))
SB suction blower
L optical path length through the smoke plume
SDA secondary dilution air
(Eq. (3))
SOF soluble organic fraction
M particle mass concentration (Eq. (3))
SP sampling probe
n refractive index
TDAC transient dilution air controller
r sam split ratio for PFSSs
TEM transmission electron microscopy
R2 correlation coefficient
TEOM tapered element oscillating microbalance
Dm particulate mass (Eq. (4))
TT transfer tube
u opacity (Eq. (3))
UV ultraviolet radiation or range
VF volatile fraction
Abbreviations WHSC worldwide heavy steady cycle
WHTC worldwide heavy transient cycle
CFV critical flow venturi ACEA Association des Constructeurs Européens
CVS Constant Volume Sampling d’ Automobiles
DAF dilution air filter CARB California Air Resources Board
DMM Dekati Mass Monitor EC European Commission
DT dilution tunnel ECE Economic Commission for Europe
DOP di-octylphthalate EMA Engine Manufacturers Association
DPF diesel particulate filter EMPA Swiss Federal Laboratory for Materials
DPM diesel particulate matter Research and Testing
DPT differential pressure transducer EPA Environmental Protection Agency
d50% diameter of particle retained with 50% effi- EU European Union
ciency by a classifier or separator GRPE Group of Rapporteurs on Pollution and Energy
DR dilution ratio ISO International Organization for Standardization
EGA exhaust gas analyser JARI Japan Automobile Research Institute
ELPI electrostatic low-pressure impactor OICA Organisation Internationale des Constructeurs
EP exhaust pipe d’Automobiles
ESC European steady-state cycle PMP Particle Measurement Programme
ETC European Transient Cycle RWTÜV Rheinisch-Westfälischer Technischer Überwa-
FC flow controller chungsVerein
FH filter holder SwRI Southwest Research Institute
FID flame ionization detector US United States
FM flowmeter WHDC Worldwide Heavy Duty Certification
FTP Federal transient procedure WHO World Health Organization
HDE heavy duty engine
638 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Fig. 1. Evolution of US and EU diesel particulate matter (DPM)
emission standards for heavy duty vehicles over ~20 years.
the European Union (EU) for 2005 and 2008 (Euro IV
and V emission standards), whereas in the US up to year
2007. Fig. 1 depicts the emission standards evolution for
HDVs. Current and proposed standards employ a mass
metric as emission quantification criterion. It should be
mentioned though, that alternative metrics related to the
number, size and surface area of emitted PM, are screened
by the scientific community. On one hand, these metrics
seem to better associate particle emissions and health effects
and, on the other, to provide a more sensitive measure of
particle emissions. However, the particular topic is very
complex and rather equivocal, and if there is a consensus,
then this is to continue to keep PM mass down to a minimum
and assume that everything else will come down with it.
Today’s DPM legislation is based on this premise. In case
that future legislation is based on a different metric, a variety
of alternative methods can be considered: currently, the
industry and research centers investigate different instru-
ments for the characterization of PM properties and
comprehensive instrumentation reviews are available
[9–12].
Reducing DPM emissions from future vehicles is a
challenging task. Similarly, given the low emission level,
exact determination of DPM emission rate is equally
challenging. In contrast to gaseous exhaust components,
DPM is extremely unstable due to a variety of processes
starting with PM formation till removal by atmospheric
processes. Such processes continuously alter the physico-
chemical character of particles. Hence, the outcome of any
PM determination method depends not only on how the
actual measurement was made but also when and where in
the formation and exhaust processes this has taken place.
Additionally, the low mass concentrations emitted are likely
to induce uncertainties due to the limited sensitivity of the
existing gravimetric procedure.
This paper deals with the determination of PM emissions
from diesel engines. The focus is on HDVs measurements
although conclusions may concern light-duty vehicles
(LDVs) as well. Although an older paper [13] comprehen-
sively reviews the state-of-the-art of measurement technol-
ogy, the present one attempts to complement it focusing on:
(1) the provisions brought to the established sampling and
measurement techniques to ensure reliable measurement for
near future engines, (2) the alternative techniques which
may be used for PM sampling and, (3) the possibilities for
more sensitive and/or time-resolved PM mass quantifi-
cation. The paper is organized as follows: In Section 2 some
fundamental issues concerning the DPM and the measure-
ment quality are outlined. Section 3 discusses the reference
measurement method and the provisions proposed to ensure
reliable measurement for near future engines. Section 4
deals with alternative sampling methods; in particular
partial flow dilution systems are compared to the reference
method. Section 5 presents possibilities for mass determi-
nation techniques, with main emphasis on real-time
instruments. Finally, Section 6 provides an overview of
the cost of PM measurement facilities.
2. Background
2.1. DPM properties
DPM characterization can be made either in the airborne
phase or after particles have been collected on a medium. In
the first case, a particle-laden sample is led to an instrument
where the property in consideration is determined without
contacting the particles. In the second case, a sample passes
through a collecting medium and the deposited material is
characterized by weighing and physicochemical analysis.
Customarily, the term particle has been proposed for the
matter being characterized in the airborne phase (suspended
matter) and the term particulate for the deposited matter [14].
Current legislation defines DPM on a particulate basis as
all material that is collected on a filter after exhaust sampling
and dilution at temperatures below 52 8C. At this state, the
collected material consists of agglomerated carbonaceous
particles (soot), ash and adsorbed organic and inorganic
material. Soot is produced during combustion, while volatile
species are adsorbed as exhaust gases cool down during
transfer and dilution. The amount of adsorbed matter strongly
depends on sampling conditions. Ash comes from lube oil
and fuel (additives, impurities), normal engine wear and from
corrosion of the exhaust system. The schematic commonly
used for the composition of DPM is the following:
DPM ¼ soot þ SOF þ IF
The term SOF (soluble organic fraction) refers to the
organic material that can be extracted using a Soxhlet
apparatus. IF (inorganic fraction) contains volatile and
semivolatile compounds like sulfates and nitrates, ash
and water. By convention, SOF is combined with sulfates
and nitrates to a single component termed as volatile
fraction (VF) which can be determined by heating particles
in an inert atmosphere. Fig. 2 provides a simplified
schematic and a typical chemical composition of DPM.
PM in the atmosphere is usually distinguished in
three different modes: the ultrafine mode ðDp , 0:1 mm),
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Fig. 2. Particle schematic and typical chemical composition of
DPM [15]. Exact chemical composition depends on the engine
considered and fuel used, together with sampling conditions.
the fine mode ðDp , 2:5 mm), and the coarse mode
(2.5 mm , Dp , 10 mm). Although the above mentioned
size segregation can be applied also in the case of diesel PM,
two somewhat different size modes are more relevant for
vehicle exhaust aerosol [15]: the nuclei size range
(Dp , 0:05 mm), consisting mainly of volatile particles,
and the accumulation range ð0:05 mm , Dp ,, 1:0 mm),
consisting mainly of agglomerated soot particles with
adsorbed volatile material.
Although of limited importance to total PM mass due to
their small size, nuclei particles are currently the focus of a
scientific debate because a separate and distinct mode to the
accumulation one may be formed in this size range, mainly
when sampling conditions allow excessive condensation of
volatile material. Such particles disappear downstream of
thermodenuders [16] and recent findings [17,18] demon-
strate that there is not a significant number of nuclei
particles when using sulfur-free fuel. However, there is
evidence which suggests that nuclei particles may be formed
during atmospheric aging of exhaust aerosol [19] bringing
significant implications to the study of particle health
effects. A discussion on the nucleation mode particles
debate and the implications of such particles on human
health and measurement procedures is much beyond the
scope of this review. However, the reader can refer to the
work of large-scale projects which address these issues
[19 – 22]. In contrast to the uncertainties related with the
nuclei mode characterization, the concentration of the
mostly solid accumulation mode particles has been found
to significantly decrease with engine technology improve-
ment and use of aftertreatment devices [17,23].
Bérubé et al. [24] offer an instructive description of
individual particle morphology (Fig. 3). The authors
distinguish four basic structures of particles using trans-
mission electron microscopy (TEM) and studying particles
produced by a diesel tractor engine at idle. ‘Spherulites’ (1)
are the smaller individual solid particles generated by
combustion, which then agglomerate to formulate ‘chains’
(2) or ‘clusters’ (3). Also large ‘spherules’ (4) were
identified, which most probably constitute re-entrained
material from transport and sampling line hang-ups. Finally,
639
Fig. 3. TEM photo-micrographs of particles collected in the exhaust
of a tractor diesel engine [24]. Left photograph shows a collection of
typical shapes for particles sampled: A spherulite (1) is a primary
particle which agglomerates with other primary particles to form
chains (2) and clusters (3). A spherule (4) is a particle which usually
forms by re-entrained material from sampling system hang-ups and
is generally not considered as a primary combustion particle. Right
picture shows less frequently observed electron-dense flake-like
bodies, which may be formed from chain and cluster restructuring
during adsorption/desorption of volatile material from the particle
surface during sampling.
electron-dense ‘flake-like bodies’ were observed. It has been
proposed [25] that adsorption and subsequent desorption of
volatile material on the particle surface may lead to more
dense particle structures which may explain such flake-like
bodies. With regard to the contribution of such particles to
total mass emissions, studies using gravimetric impactors to
classify particles have shown that more than 80% of the
total mass resides in the size range between 0.05 and 0.5 mm
[26,27 and references therein].
A mathematical surrogate for particle morphology can
be given by the fractal-like dimension, which is defined as
the exponent that particle mobility diameter is raised to
become proportional to particle mass [28]. Hence, a fractal-
like dimension of 3 corresponds to a dense sphere, while
dimensions of 2 and 1 should be expected for 2D (plane) and
1D (chain-like) particles, respectively. Measurements on a
small diesel electrical power generator [29], suggested
fractal-like dimensions between 2.1 and 2.9 for diesel
particles, depending on engine load (higher values for lower
loads). This indicated compact soot agglomerates for low
loads changing to more loose structures at higher loads.
More recently, Park et al. [30] measured particles generated
by a 4.5 L engine (John Deer 4045, 75 kW) and found
fractal-like values ranging from 2.33 (high engine load) to
2.41 (low engine load). These results also suggest more
compact particles at lower engine loads. Based on TEM
studies, Park et al. [30] explained this observation
hypothesizing vapor condensation which may be understood
as a restructuring process, similar to Weingartner et al. [25].
Virtanen et al. [31] measured particles form a light duty
vehicle at normal road loads and reported fractal-like values
ranging from 2.58 to 2.84 with decreasing particle size. All
these studies suggest that diesel particles are mainly
640 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
agglomerated structures of various degrees, according to
engine characteristics and load. It should be noted that
fractal-like determination method might also have an effect
on the values reported. When optical techniques are used to
estimate fractal-like dimension, only values below 2 can be
deduced, because 2D particle projections are usually
examined [32].
The complex character of exhaust aerosol complicates its
quantitative determination. Section 3 provides a description
of the methods that legislation has adopted to quantify and
regulate PM emissions from diesel engines.
2.2. Quality definitions for DPM characterization
The evaluation of any physical measurement method
implies different kinds of quality assessment. In the case of
DPM characterization, the quality of the measurement needs
to be assessed both with regard to the technical adequacy of
the measurement as such, and with regard to the similarity of
the procedure to real-world exhaust aging. In that respect, a
number of criteria need to be fulfilled when selecting a
method for DPM characterization,1 which can be summar-
ized as follows:
1. Representativeness. The degree to which the method
accurately and precisely represents real world aging
conditions.
2. Accuracy. The closeness of an individual measurement
or the average of a number of measurements to an
accepted reference value. Departures from an accurate
measurement include a random error (precision) and a
systematic error (bias), due to sampling and analytical
procedures.
3. Repeatability. A measure of how consistently the method
determines exhaust DPM.
4. Reproducibility. A measure of how different persons or
facilities measure the same quantity.
5. Traceability. A measure of how an equipment relates to
international standards or basic physical constants or
properties.
6. Robustness. The degree to which the method con-
tinues to function despite the existence of faults in its
component subsystems or parts.
An additional, often deterministic, criterion for the
selection of any of the available techniques and instruments
is their cost-effectiveness, defined as the degree to which the
method gives optimum results for the expenditure. When
possible, methods and instruments presented in the follow-
ing sections will be evaluated on the basis of these criteria.
1
Many of these definitions are taken from EPA Guidance for
Quality Assurance Project Plans. EPA QA/G-5, EPA/600/R-98/018,
Washington DC, Office of Research and Development, 1998.
3. The reference method for DPM sampling: the full-flow
sampling system
3.1. General description
In US Federal, European and national test procedures,
the Constant Volume Sampling (CVS) technique (Fig. 4) is
prescribed as the DPM sampling method, applied both to
engine and vehicle emission certification. According to this
technique, all vehicle exhaust is mixed with filtered ambient
air in a dilution tunnel (DT) so that the total volumetric
flowrate is constant for all engine operating conditions. A
positive displacement pump (PDP) or a critical flow venturi
(CFV) at the DT outlet provides the constant flowrate.
By definition, the system operates on a variable dilution
ratio (DR) depending on the vehicle/engine operation mode.
DR may be defined as the ratio of the diluted exhaust flowrate
to that of raw exhaust, either in mass or in volumetric terms.
Experimentally, it can be determined as the ratio of the molar
concentration of a stable species (CO2 or NOx) in the raw
exhaust to its concentration in the diluted exhaust. Legis-
lation does not prescribe any DR range. It only sets a 52 8C
upper limit regulation to the diluted exhaust temperature at
DPM sampling location to avoid water condensation. Hence,
total flowrate and, therefore, DR range is adjusted in a way to
fulfill this limitation. At sampling location, a small sample
flow is drawn through a filter at a rate proportional to the main
flowrate. This technique is referred to as a ‘single dilution’
one if no further dilution occurs for the sample flow. If the
sample is once more diluted in a secondary (smaller) DT, the
method is referred to as a ‘double dilution’ one. Double
dilution may be useful if the filter temperature requirement
cannot be met with single dilution only but it may also result
in too little mass collected, in case of a low emitting engine.
DPM mass collected on the filter is determined by weighing it
in a chamber of controlled environmental conditions
(temperature, humidity) using a sensitive balance. The
mass collected is then referred to main flow conditions, by
means of flow proportionality, and a single DPM emission
value is deduced for the whole test in the form of mass per
power time (US, g/bhp h), (EU, g/kW h) for engine tests and
mass per distance (US, g/mile), (EU, g/km) for chassis tests.
The CVS technique has been developing since the late
1950s, initially applied in the characterization of lead and acid
aerosol found in engine exhausts [33,34]. Main target of the
technique is to allow sufficient mixing time for physical and
chemicalstabilization tooccur, before a representative sample
is extracted for analysis. However, this technique does not
completely simulate the actual processes occurring during
real world aging. In the real world, exhaust gas dilution
proceeds as a function of time (respectively, distance) from the
exhaust pipe (EP) outlet. In a DT, dilution stops progressing
with time after some point and obtains a constant value that
depends on the dilution air and exhaust gas flowrates.
Fig. 5 [35] shows this deviation by showing that while
dilution increases and temperature decreases continuously
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672 641

Fig. 4. The Constant Volume Sampling (CVS) technique, used as a reference for PM sampling and measurement. The CVS unit may either
consist of a CFV or a PDP. Option I corresponds to a single dilution system and option II to a double dilution one. The selection of each option
depends on the temperature and DPM concentration of the exhaust gas.

Fig. 5. Simplified schematic of the exhaust ageing process in the atmosphere and in the dilution tunnel of the CVS procedure. The CVS provides
much lower dilution ratios and cooling than aging in the atmosphere as a function of time [35].

in the atmosphere to reach ambient levels, CVS dilution
stops at an initial stage and further cooling occurs only
through convection to the surroundings. This can lead to
different particle characteristics obtained in the laboratory
versus ambient sampling and raises questions about the
representativeness of the method. In that respect, on-road
measurement techniques have been examined to obtain a
more representative sample [19,36] but such methods are far
from establishing a procedure suitable for type-approval
regulations. More detailed discussions on the CVS tech-
nique can be found in the literature [33 –35].
3.2. Quality of the full-flow dilution method
components (flowmeters, venturis, etc.) can be calibrated
according to prescribed standards. Round robin tests2 are the
only available tool to examine the overall reproducibility of
the method between different laboratories. Proper data
analysis following these tests provides summary statistics
concerning inter-laboratory precision and method bias [37].
Although results of such studies have only recently been
published for PM emissions [38] it is rather well perceived
that significant intra- and inter-laboratory variability
accompanies such measurements.
A typical inter-laboratory PM variability (tests con-
ducted with the same engine and fuel type and having the
exhaust gases measured with satisfactory agreement) and

It is difficult to put conditions about the traceability of 2

A method validation study involving a predetermined number of
the CVS method for PM sampling, since no reference laboratories, all conducting the same measurement following the
particle state exists [10]. Only individual laboratory same procedure.
642 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672

Fig. 6. Accuracy of the reference measurement method as function of the mass emission rate and corresponding emission standards for EU
legislation for heavy duty engines [41]. Two quality criteria are shown: repeatability corresponds to within (intra) laboratory variability and
reproducibility to between (inter) laboratory variability.

when good-practice rules are followed is estimated at
about 20% for a particulate emission rate of about
0.48 g/bhp h [39,40]. As pointed out by Kittelson and
Johnson [40], in order to achieve an inter-laboratory
variability of less than 20% for engines which meet the
1994 US Federal heavy duty standards (0.1 g/bhp h),
the absolute variability should decrease more rapidly
than the actual emission rate. At that time this seemed
unlikely. However, measurements for HDVs have shown
greater variability than those for LDVs [13], mainly due to
differences in the test cycles. The accuracy of the
reference method as a function of HDV DPM mass
emissions is given by ACEA [41] and is depicted in Fig. 6.
There are similar concerns [42] that as emission standards
decrease such problems may become significant for LDV
measurements as well (Fig. 7). Questions are also raised
with regard to the sensitivity of the procedure, especially
for future emission limits: the duration of the driving or
operating cycle may not suffice to collect enough
(detectable) amount of mass. However, this shortcoming
mainly relates to the test cycles chosen for emission
certification rather to the CVS technique as such.
3.3. Sources of variation for DPM determination
An understanding of the parameters influencing the
measurement is vital in order to give a better insight of
the processes occurring, to provide measures for

Fig. 7. Repeatability of regulated PM measurements for passenger cars of different engine concepts, tested over the cold start European Driving
Cycle [42]. Coefficient of variance is defined as the ratio of standard deviation over mean for the number of tests performed. Absolute particle
mass collected on the sampling filter is shown in the legend for each case.
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672 643

minimizing errors and to refine the interpretation of the results.
Considering the same engine tested on the same fuel, the most
significant sources of variability are thought to be [13,40]:
† The means of transporting the exhaust to the DT.
† The design of the tunnel.
† The design of the sampling probe.
† The tunnel operating conditions: collection temperature,
DR, dilution air specifications (temperature, humidity,
background PM concentration).
The phenomena occurring during the transport/sampling
processes are the ones taking place in every flowing aerosol
system [9]: wall-to-particle, particle-to-particle, and gas-to-
particle interactions. The first process includes particle
losses mechanisms (inertial impaction, thermo- and diffu-
sion-phoresis, sedimentation) and re-entrainment. The
second refers to coagulation and agglomeration of airborne
particles and the third concerns condensation/evaporation
and adsorption/desorption of volatile material to or from the
particle surface, respectively.
Particle deposition due to gravitational and electro-
static forces and temperature and concentration gradients
is important for estimating the systematic (deposition) and
random (re-entrainment) error introduced to the measure-
ment. Kittelson et al. [9,40] conducted preliminary studies
on deposition and summarized the impact of various
particle – wall interactions that affect particle measure-
ment, together with various recommendations to minimize
particle losses (Table 1). Although the need for further
investigations on the occurring processes has been
emphasized, little relevant work has been published. One
proposed deposition model [43] was not found accurate
enough when compared to experiments, mainly due to
difficulties with the computations of the temperature
profiles. However, due to the systematic character of the
error induced by deposition, some predictions are possible.
On the other hand, re-entrainment is in general
unpredictable because it refers to the momentarily release
of particle mass accumulated on the walls over many tests. It
mainly occurs in the transfer pipe from the engine to the DT
and in the transfer line from the DT to the secondary tunnel
(if any) [40]. Based on studies with electrostatic precipita-
tors, re-entrained particles are considered to be much larger
in size than primary diesel particles [44,45]. However, the
random motion of gas near the wall surface results in
hydrodynamic motions and moments that may cause the re-
suspension of smaller particles as well. Vortices and sloping
shear layer structures might add to the phenomenon [46].
Models of the process in the DPM measurement field are not
available but useful ideas can be obtained when combining
experiment and theory. Matsusaka et al. [47] observed that P
is re-entrained randomly from the surface layer of the
deposited matter in the form of aggregates, and then it
gradually progresses through the depth of the layer causing
re-suspension of smaller particles. Similarly, Ziskind et al.
[46] concluded that turbulent conditions may cause re-
suspension of smaller particles as well, by reviewing
different theoretical models of particle re-suspension.

Table 1
Particle-to-wall interactions responsible for variability on the PM determination when following the reference gravimetric procedure with CVS
[9,40]

Mechanism Impact Recommendations

Inertial Removes small number of the larger Avoid sharp changes in sample line
impaction particles (which however represent diameter or direction. Isokinetic
a larger fraction of the total particulate sampling not as important for submicron
mass). Introduces variability through particles
unpredictable re-entrainment of deposited
mass. Inertial and gravitational losses are
quite small for particles in 0.1 –1.0 mm range
Electrostatic Electric charge build-up on sample lines Use metal sample lines to avoid electrostatic
deposition attracts charged DPM, causing it to deposit build-up. Avoid Teflon sampling lines, prone
on the line walls to build-up of electrostatic charge.
Thermophoretic Large temperature differences between Insulate/heat sample lines to avoid large
deposition exhaust gas and sample lines produce differences in temperature between lines and
thermal driving force for particles deposition exhaust gas
on line walls. Most significant losses occur
during transient duty cycles.
Diffusional Diffusion for particles in the size range that Difficult to eliminate diffusional deposition. Use
deposition represents the majority of the mass (.0.1 mm) short sampling lines.
is negligible. Diffusion for particles in the size
range that represents the majority of number
(,0.03 mm) is also small, but should be con-
sidered for the smallest size ranges measured.
Gravitational Minimal impact on DPM losses. May Avoid unnecessary long horizontal sections of
deposition introduce variability through unpredictable re- sample lines where large particles settle.
entrainment of small deposited mass
644 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
These findings indicate the need for more focus on the
process in view of future measurement requirements.
Another important issue is the representativeness of the
extracted aerosol, compared to the free aerosol flow in the
tunnel. This issue is related to anisokinetic sampling
conditions. Isokinetic sampling is achieved when the
sampling probe is aligned parallel to the free gas stream
and the gas velocity entering the probe is equal to the free
gas stream velocity. Gas streamlines deform in anisokinetic
sampling and particles do not exactly follow the streamlines
due to their inertia. Hence, a preferential selection of
particles with respect to size occurs. If the velocity in the
sampling tube is less than the velocity in the DT then the
tube will become slightly pressurized and some particles
will miss entering the tube. Preferably, small particles will
be rejected due to their small inertia and, as a result, large
particles will be overpopulated. Opposite conditions prevail
in case of sampling at velocity larger than free flow velocity.
In either case, particle distribution will not be representative
of that in the DT. Very little attention is given to isokinetic
sampling by the relevant literature. This is due to the
generally accepted assumption that isokinetic sampling is
not a prerequisite to obtain representative DPM samples.
This assumption relies on experience and on the small
Stokes numbers usually established in the system. However,
Silvis et al. [48] have theoretically calculated that significant
sampling errors still arise for small Stokes numbers when
the velocity mismatch is large.
With regard to particle-to-particle interactions, coagu-
lation and agglomeration modify size distribution but
cause no change in the mass concentration and hence need
no consideration for mass measurement. On the other
hand, gas-to-particle conversions may result in a modifi-
cation of mass concentration. Processes such as con-
densation/evaporation and adsorption/desorption of
volatile compounds on soot particles can be strongly
influenced by the dilution process and the following
sampling procedure. The relevant parameters for such
mechanisms are the exhaust gas temperature, the dilution
air temperature, the DR, and the extent of thermal losses
of the CVS system. The significance of the DR and
mixture temperature on the final result is well documented
by several studies [35,40,49,50]. DPM mass concentration
increases with decreasing DR, mainly due to conden-
sation/adsorption of organic material. The latter has been
verified by thermogravimetric analyses of the samples.
Earlier theoretical calculations suggested adsorption as the
prevailing process when compared with experimental
trends [50– 52]. However, as pointed out by both Plee
and MacDonald [51] and Clerc and Johnson [52],
condensation can also contribute significantly to the
extractable material when operating conditions (such as
low load operation) yield low exhaust temperatures and
high hydrocarbon concentrations, but this finding has been
based on measurements of relatively older engines with
high volatile species emissions.
The actual influence of the above processes is, however,
poorly understood and extremely difficult to predetermine.
For example, the time constants for mass transfer of volatile
matter to and from the surface of soot particles immersed in
a flowing gas are unknown. This determines how easily
volatile material would be lost or gained by the surface of
particles, and it is in itself an important factor of the
sensitivity of VF to DR. The importance of these processes
grows as VF increases. Thus, a high sensitivity of DPM on
DR should be expected for low emitting engines because
lubrication oil related VF constitutes a major fraction of the
DPM emitted. Another important factor may be the
interaction of the volatile compounds with the surfaces of
the collection filters. Looking at engines equipped with
diesel particle filters (DPFs), where solid PM emission is
extremely low, condensation of volatile components on the
filter surface needs to be specifically addressed. In addition,
there is considerable disagreement depending on how much
the mixture temperature at the filter face varies during the
transient test. All these variability sources led investigators
in the field [48,53] to consider DT not just as measuring
equipment but rather as a complex physicochemical reactor.
Based on such an approach, an illustration of the dilution
and sampling parameters that may influence the measure-
ment is given in Fig. 8.
3.4. Overview of the existing reference procedure
Despite the difficulties and inherent shortcomings
mentioned in the previous paragraphs, the CVS method
has been recognized so far as the technically and practically
best choice for emissions certification and engine develop-
ment. However, it has been in question for some time since
it requires a bulk installation and large investments to
achieve adequate DRs for large heavy-duty engines testing.
Capacities of the order of 180 m3/min are typical for engines
up to 500 kW, in order to achieve appropriate mixing and
DRs in the order of 10:1 at the engine rated operation mode.
This question on the applicability of the CVS has been
recently revived concerning the low emitting engines of the
near future.
High capacities are associated with relatively large DRs
at partial loads, which for low emitting engines lead to
gaseous and particulate concentrations below detection.
These may severely affect the accuracy and repeatability of
the test results. On the other hand, the installation and
operating costs of these systems are very high, especially for
large engines. Costs further increase by the need for
thorough dilution air pre-conditioning, including dehumi-
dification, efficient filtration and scrubbing and/or catalytic
conditioning. Typical purchase cost of a CVS system of a
capacity of 180 m3/min is in the range of 600 ke, including
the flow regulator (PDP or CFV), the DT, the secondary
dilution and ancillaries.
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Fig. 8. Simplified schematic of the dilution and sampling parameters influencing the collected particulate mass collected on the gravimetric filter
in the CVS reference procedure.
3.5. Provisions to the reference method introduced by new
legislation
Both EU and US recently decided stricter emission
standards for all categories of motor vehicles, in order to
alleviate atmospheric pollution risks. As far as HDVs are
concerned, EU and US launched Directive 1999/96/EC [54]
and Federal Register 2007 [55] respectively. Both regu-
lations promulgate emission standards for the vehicle
categories covered and describe the necessary certification
procedures for new engine type approvals.
Furthermore, the new ISO 16183 standard [56]
specifies the measurement and evaluation methods for
gaseous and particulate exhaust emissions from HDVs
under transient conditions on a test bed. It focuses on the
introduction of partial flow sampling systems (PFSSs) and
the procedure defined can be applied to any transient test
cycle that does not require extreme system response
times. Such systems aim to be used as an option of
certification equipment on type approval tests. This
applies to steady state and transient tests such as the
European Transient Cycle (ETC) and the US Heavy Duty
Transient Cycle.
The sections below provide a summary of the most
relevant provisions brought by new regulations and
standards, aiming at the improvement of the DPM
measurement quality.
3.5.1. Dilution air pre-conditioning
Dilution air temperature is a significant parameter for the
dilution process of exhaust PM as it imposes an important
parameter for the behavior of volatile species in the DT.
Directive 1999/96/EC defines a lower (20 8C) and an upper
(30 8C) limit for the dilution air temperature. However,
preheating of the tunnel walls up to 52 8C is recommended if
645
the ambient temperature is below 20 8C. In contrast, neither
the ISO 161833 standard, nor the US regulation define any
upper limit for the dilution air temperature. Instead they
introduce a lower permissible dilution air temperature of
15 8C. Leaving the upper temperature limit to be defined by
the system manufacturer is well perceived. This may give an
additional degree of freedom for the achievement of the
lower temperature limit at the sample holder, when exhaust
gases are at a low temperature. In addition, a high dilution
air temperature helps to reliably prevent condensation on the
sample filter. On the other hand, a dilution air temperature
limit lower than 20 8C is needed to offer the possibility for
lower dilution factors (hence increase mass of PM collected
on the filter).
The relative humidity of the dilution air may also affect
the measurement result, since it adds water in the dilution
process and, more significantly, may react with sulfur
components to produce VF components. One would expect
therefore a more precise definition of this parameter by the
regulations (as is in the case of filter conditioning, for
example). In the EU Directive and the ISO standard the
dehumidification is simply permitted, while the US
regulation does not include any relevant recommendations.
Another issue that may become significant in view of the
very low particulate emission of future engines is the
particulate content of the dilution air. The EU Directive and
the ISO standard recommend either efficient filtration prior
to its introduction in the DT or sampling of dilution air
according to good engineering practice to determine the
background particulate levels. More clearly, the US
regulation specifies that primary dilution air shall be passed
3
ISO 16183 indirectly specifies a maximum dilution air
temperature of 52 8C at the position of the particulate sampling
probe (PSP).
646 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
through a filter having a minimum removal efficiency of
98% and that secondary dilution air shall be filtered using a
high efficiency (99.97%) particulate air filter (HEPA).
Background corrections or dilution air filtration may still
not be totally equivalent approaches because existing
particles may act as condensation sites for VF condensation
which does not occur in a filtered air stream. Hence,
correction of the background PM when the engine is off does
not correct for the VF condensed on pre-existing particles
when the engine operates and the actual DPM measurement
is conducted.
In summary, any future requirement relating to the
dilution air should include limits for: (a) the minimum
temperature, (b) the relative humidity and (c) the permiss-
ible particulate content and/or compulsory background
corrections for the PM collected on the filter.
3.5.2. PM sampling probe
PM samples in the CVS are drawn with a sampling probe
from the diluted exhaust stream to the gravimetric filter
(Fig. 4). The design of the sampling probe is closely related to
the condition of the diluted exhaust. US regulation accepts an
open tube facing upstream design in conjunction with a pre-
classifier to exclude coarse particles from entering the sample
flow (e.g. rust from the engine exhaust system or re-entrained
material sheared from the sampling system walls), while
allowing primary combustion-generated particles to pass in.
The pre-classifier may be either an inertial impactor or a
cyclonic separator with a d50% cutpoint between 2.5 and
10 mm at the volumetric flowrate selected for the sampling
flowrate. EU Directive does not precisely define the probe
design although the relevant pictures included therein imply
the open tube facing upstream. Pre-classifier is not prescribed
and this can be considered as a drawback.
In the same direction, the ISO standard foresees four
different possibilities:
(a) an open tube facing upstream,
(b) an open tube facing downstream,
(c) a multiple hole probe,
(d) or a ‘hatted’ probe facing upstream (known as a
‘Chinese-hat’ from the EU Directive on passenger
car emissions).
A pre-classifier is recommended only in conjunction
with a sampling probe of the open tube facing upstream
design, while the other three alternatives are believed to
prevent large particles from entering into the probe by their
design only. Although the above alternatives have been
discussed in the framework of ISO for samples taken
directly from the raw exhaust gases, their application can be
extended to CVS method. Thus, it is recommended that the
future European regulations have to specifically address the
sample probe issue and the diluted exhaust sample pre-
conditioning. However, it is noted that in ISO discussions,
the European and Japanese members are of the opinion that
the design required in the US (open probe) is not an
adequate technical solution, whereas the US delegation has
an opposite view [57]. Hence, all four alternatives are
included in the ISO standard and it is suggested to
experimentally check these alternatives against each other,
prior to any final decision.
3.5.3. PM collection
Filter material. All the procedures accept Teflon coated
glass fiber or membrane filters, a well known material for its
resistance to acids, alkalis and oxidizing agents. Directive
1999/96/EC prescribes a minimum clean filter collection
efficiency of 95% with 0.3 mm DOP (di-octylphthalate)
particles, while ISO and US regulations require an efficiency
of 99%.
Stain diameter. An advantage of Directive 1999/96/EC
and the US regulation over the ISO standard is the
determination of the stain diameter. This is defined as the
diameter of the filter surface area where PM is actually
collected. The lack of such a definition in ISO permits the
testing laboratory to measure with filters effectively much
smaller than the minimum prescribed (47 mm), while using
any acceptable size, by simply modifying the filter holder,
thus reducing the stain diameter. Comparing the EU
Directive and the US regulation it has to be mentioned
that the Directive’s approach is advantageous as the stain
diameter is prescribed as a function of the filter size, while in
the US regulation only one value is given, corresponding to
the permissible filter size.
Number of sample filters. The backup filter, required in
Directive 1999/96/EC, is of the same type as the primary
one and aims at collecting particle matter escaping the
primary filter. Losses from the primary filter though should
be assumed very low, especially in view of the low
backpressure increase permitted (see Section 3.5.4 on filter
load). The backup filter may only act as a condensation
surface, which by itself introduces additional inaccuracies.
Considering the very low particulate loading expected on
the secondary filter, the accuracy with which it is
determined (weight difference between loaded and unloaded
filters) is limited, especially in view of possible filter
material losses in the holder and humidity effects. It is
expected that the use of the backup filter has an overall
negative effect on the accuracy of the measurement.
Consequently, the use of a single filter as prescribed in
both ISO standard and US regulation, will most probably
increase, if not the accuracy, at least the repeatability of the
method.
Filter holder temperature. The US 2007 regulations
introduce a narrow temperature range (42 – 52 8C) at the PM
filter position through the test. The introduction of this
temperature range seems to be a significant step forward
because it attempts to deterministically regulate the VF of
the sampled DPM. This is especially valid in view of the
possibility that DPFs will be widely used for compliance
with future emission standards, where SOF will constitute
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
the dominant part of the overall low emitted DPM. This is
clearly illustrated by the measurements reported by Stein
[58,59] and Schweizer et al. [60,61] when a DPF is used.
Furthermore, a narrower filter temperature regulation is
supported by recent studies, where the impact of processes
such as condensation and adsorption are tested both
theoretically and experimentally [62]. The authors con-
cluded that the main mechanism influencing the formation
of DPM is the accumulation of hydrocarbons that leads to
gas phase saturation and later liquid adsorption on the
particles. Thus, specification of filter temperature as well as
of DR will be necessary to avoid variations in the amount of
DPM collected during the test.
The task to maintain the filter holder temperature at the
desired temperature range, is additionally restricted by the
need to keep the temperature at the primary DT below
191 8C, as required by the EU Directive. Obviously, this
needs to be achieved without modifying the primary DT
flowrate between full load and idle. In principle, there are
several possibilities to keep the filter holder within this
temperature window for the low loads:
† either heat up the filter holder and the sampling line (i.e.
put the whole system into an space of controlled
temperature),
† or heat-up the dilution air of the secondary tunnel to a
suitable temperature,
† or a combination of the two.
The ISO standard provides for a DT and sample line
heating up to a temperature of 52 8C. This option is also
included in the US regulation for the DT walls, as an
alternative to their heavy insulation, without specifying the
maximum permissible temperature. Still, it has to be
mentioned that the US regulation states that: “Measurement
procedure intent is to maintain sample temperature by
dilution and mixing with air rather than by transferring heat
to the surfaces of the sampling system”, and this
may be considered as contradictory to the possibility of
heating the sample. However, because of the different
equipment involved in the ISO standard and the
US regulation some difficulties concerning the heating of
the dilution air are introduced.4 Discussions with parties
involved in these developments [57,63,64] indicated that:
† The US EPA proposal for the narrow temperature range
has been well received because it should reduce
measurement uncertainty.
† The way this will be realized is still unclear, while US
EPA still awaits for comments and input for the technical
details of the regulation.
† The first priority will be to look at heating the sample
holder rather than the dilution air.
4
ISO 16183 deals only with partial flow sampling systems
discussed later in Section 4.
647
Nevertheless, it has to be emphasized that from a
measurement point of view, one should be very careful in
using filter holder and sample hose heating to keep the
sampling temperature at the desired range, in particular in
cases where there is a need to heat the diluted exhaust from
temperatures of around 15 to 42 8C. Thermal gradients
(associated with thermophoresis and other phenomena) may
affect the physical character of particulates at the sampling
point. It is unclear how significantly this process will affect
the DPM mass. However, other parameters may substan-
tially be affected (such as number and distribution of
particles), which must be carefully studied, in particular if
other particle metrics are envisaged for the near future. It is
certain that mass measurement systems as those discussed
for legislative purposes will also be used for the measure-
ment of other particle properties.
Fig. 9 shows the results of an exemplary calculation
(assuming adiabatic conditions) which illustrates how the
temperature window of 42 – 52 8C could be achieved with
hot dilution air (42 8C dilution air temperature) and double
dilution. In this example, a first dilution with a DR ¼ 8 at
the rated mode results in a diluted exhaust temperature of
about 100 8C. A second hot dilution with a DR ¼ 10 leads to
48 8C final dilution temperature. At idle, the first dilution
leads to temperatures below 52 8C for DR $ 6; while the
second dilution keeps the temperature at 42 8C. Fig. 9.
presents also a drawback of this approach: the power that is
required for heating up the dilution air from 20 to 42 8C is
substantial (of the order of 50 – 70 kW for primary DRs of
the order of 8 – 10). This is both technically difficult to
realize and expensive.
Sample filter loading. A difference between the EU
Directive and ISO is found in the definition of minimum
sample filter loading. In Directive 1999/96/EC, a minimum
loading is recommended in the range of 0.56 – 0.73%
of the weight of the unloaded filter; the exact value
depending on filter size. In order to increase the particulate
mass collected on the sample filter, a sufficient number of
test repetitions with the same sample filter is permitted, at
the manufacturer’s request.
Instead, in the ISO standard, the minimum required load
is prescribed in the order of 0.13% of the clean filter weight,
i.e. about 1/5 of that recommended in EU Directive.
Additionally, ISO makes a provision for multiple tests on
the same sample filter, in order to collect the minimum
required mass, provided that the parties involved (i.e. the
laboratory and the engine manufacturer) agree. Also in ISO,
filter loading lower than the minimum required is allowed,
provided that a higher resolution balance (0.1 mg) is used
and the parties involved agree to that.
The US regulation simply recommends a filter loading as
high as possible, without either giving any limit values or
implying anything for test repetition(s).
In view of the face velocity limit established in all cases
(80 cm/s: EC Directive, 100 cm/s: ISO and US regulation),
combined with the low emission rate of the engine and
648 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Fig. 9. Calculated temperature at filter holder assuming adiabatic mixing with dilution air heated at 42 8C. Assumed values for the calculations:
Texhaust ¼ 500 8C at rated power mode, Texhaust ¼ 100 8C at idle, secondary dilution ratio 10.
the (high) DR, the US regulation simple suggestion for
maximum possible filter loading is the most adequate, since
it may be impossible to achieve the minimum either
required or recommended loads with one test run (this
problem is highlighted by Schweizer et al. [60]).5 On the
other hand, allowing for test repetitions with the same filter
on the engine manufacturer’s request (EU Directive) or
agreement (ISO) is difficult to accept, since this decision
should be made only by the testing laboratory, which has the
responsibility of the test result accuracy. Moreover, recent
experimental findings [60] strongly question the accuracy
improvement by test repetitions on the same filter: the more
repetitions were made, the lower the specific emission got,
as shown in Table 2. The reasons of such a behavior are not
clear but one may suspect that decreasing condensation of
VF on the filter surface as this saturates in successive
repetitions is a possible explanatory mechanism.
3.5.4. Sample filter conditioning and weighing
Filter conditioning before and after the test at a specific
temperature (22 ^ 3 8C) and relative humidity ranges
(45 ^ 8% or the equivalent 9.5 ^ 3 8C dew point) is in all
three procedures. However, the US regulation specifies a
tighter humidity control, i.e. a dew point of 9.5 ^ 1 8C.
Evidently this is done to minimize the humidity effect on the
accuracy of the weighing, due to the possibility that the
particulate layer of the loaded filter absorbs ambient
moisture, especially in view of the very low mass collected.
In addition to the temperature and humidity requirements,
5 an analytical balance with 1 mg resolution. ISO, addition-
It is worth mentioning here that many laboratories may still
adjust the sample flowrate at low values and far from optimum for
new engines. This ‘habit’ is probably a leftover from the times when
the mass collected was not of significant concern. In such cases it is
expected that increasing the sample flowrate within the range
allowed by the legislation will significantly increase the sensitivity
of the method.
the US regulations specify that microbalance and filter
stabilization environments shall be free of ambient con-
taminants (such as dust or other aerosols) that could settle on
the particulate filters. Therefore, it is recommended that
these environments be built to conform to Class 1000
specification (or cleaner) as determined by Federal Standard
209D or 209E for clean room classification.6 An alternative
recommendation would be to equilibrate and/or weigh the
filters within a separate, smaller, particle-free, temperature
and humidity-controlled chamber (i.e. ‘glove box’ or small
environmental chamber such as the one described by Allen
et al. [65]). Such chambers can offer significant cost
reduction for maintaining the environmental quality during
conditioning and weighing. Overall, the US regulation
provisions for tighter humidity and dust control of the
conditioning and weighing room constitute a clear improve-
ment, even though they may increase both installation and
operation costs.
In addition to temperature and humidity control, the ISO
standard and the US regulation recommend the use of a
neutralizer (imperative in the US case, only for unstable
balance readings in the case of the ISO standard). Static
neutralizers, such as Polonium-210 sources, shall be used to
neutralize charge on a filter prior to each weighing. It is
considered that the overall weighing procedure benefits
from using the neutralizer. In the US regulation it is also
permitted to have multiple weighing runs and then use the
average result.
Directive 1999/96/EC and ISO 16183 specify the use of
ally, requires a resolution of 0.1 mg, in case the minimum
required sample filter loading is not achieved. The US
requirement is 0.1 mg, regardless of the mass accumulated
6
The Class 1000 chamber has a maximum concentration 1000
particles (5 mm maximum diameter) per cubic feet of air.
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Table 2
Filter loading and deduced emission rate of a Euro III HDE
depending on the number of runs repeated on the same filter pair [60]
Test cycle Test repetitions Loading (mg) Emission (g/kW h)
WHTC 1 0.139 0.0072
WHTC 3 0.252 0.0044
WHSC 1 0.125 0.0055
WHSC 3 0.265 0.0039
Measurements conducted over a transient (WHTC) and a Steady
State (WHSC) cycle. Specific emissions decrease as number of
repetitions increases.
on the sample filter. As already mentioned, the accuracy of
the sample filter loading determination is not a question of
only the balance resolution, since it is calculated as the
weight difference between loaded and clean filter. The
effects of minor filter material losses in the filter holder, as
well as of humidity absorbed on filter material and on the
accumulated particles, or even spill of some particles when
removing the filter from the holder can become very
significant and the increased resolution of the balance used
cannot compensate for them. The only way to overcome
such effects is to increase the filter loading.
With regard to the repeatability of reference filter
weighing, used as an indicator of the conditioning room
environment quality, the provisions of ISO and US
regulation (10 mg) are more stringent than those of
1999/96/EC (5% of recommended minimum filter load,
i.e. 25 mg for 47 mm diameter filters, increasing up to
180 mg for 110 mm case filter size). This constitutes an
improvement of the method, in view of the very low overall
sample filter loads expected.
4. Alternative sampling techniques
4.1. Description of the partial flow sampling systems
To overcome the cost and size problems of the full-flow
dilution method, microdilution systems have been tested for
the measurement of particulates. These systems were
developed in early 1980s and were applied both to heavy
engines and light duty vehicles [13]. In such systems, a
small—but proportional to the total flow—fraction of the
total exhaust is sampled and used for the determination of
the PM emission rate. Consequently, the typical term PFSS
is used to characterize such techniques. After sampling, the
proportional sample flowrate may be conditioned accord-
ingly, avoiding the limitation that imposes the high flowrate
of the total exhaust. In this respect, PFSSs reverse the
process of the CVS systems: exhaust gas is first sampled and
then conditioned at wish, while the whole exhaust is first
conditioned and then sampled for PM analysis in a CVS-
type system. Obviously, sampling of a proportional to
649
the total exhaust flowrate even at transients is critical for the
precision of the measurement. The proportionality ratio is
often called ‘split ratio’ ðrsam Þ and needs to be kept constant
throughout the measurement.
Depending on the method of controlling and determining
the split ratio, PFSSs are distinguished into three configur-
ations: (1) isokinetic systems, (2) flow controlled systems
with concentration measurements, and (3) flow controlled
systems with flowrate measurement. Furthermore, PFSSs
are distinguished according to the PM determination
concept: if the entire diluted sample is led through the PM
measurement system, then the method is referred to as ‘total
sampling’. If only a portion of the diluted sample is analyzed
with regard to PM, then the method is referred to as
‘fractional sampling’. The following sections provide a
description of the main concepts governing these systems.
4.2. Concepts for PFSSs
4.2.1. Isokinetic systems
Fig. 10 shows one type of isokinetic type fractional
sampling system with suction blower (SB) control.
These systems require that the velocity into the transfer
tube (TT) is equal to that in the EP. Engine’s exhaust is
transferred from the EP to the DT through the TT by the
isokinetic sampling probe (ISP). The differential pressure of
the exhaust gas between the EP and the inlet to the probe is
measured with the differential pressure transducer (DPT).
This signal serves as a feedback to the flow controller (FC)
that controls the SB to maintain a differential pressure of
zero at the tip of the probe. Under these conditions, exhaust
gas velocities in the EP and ISP are identical, and the flow
through ISP and TT is a constant fraction (split) of the
exhaust gas flow. The split ratio is determined from the
cross-sectional areas of EP and ISP. The dilution air flowrate
Fig. 10. Partial flow sampling system with isokinetic probe [54].
The particular system is of the ‘fractional sampling type’ (only part
of the diluted sample is led to the measurement filter). ISP:
isokinetic sampling probe, TT: transfer tube, DT: dilution tunnel,
DAF: dilution air filter, FM: flow meter, SB: suction blower, FH:
filter holder, EP: exhaust pipe, DPT: differential pressure transdu-
cer, FC: flow controller, PSP: particulate sampling probe.
650 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
is measured with the flow meter (FM). The DR is calculated
from the dilution air flowrate and the split ratio. Several such
isokinetic sampling systems, commonly known as ‘split
type systems’, have been developed mainly in Japan in the
early 1990s [66,67] but are of limited interest nowadays.
4.2.2. Flow controlled systems with concentration
measurements
Fig. 11 shows a PFSS with tracer gas concentration
measurement and fractional sampling. In these systems, the
sample is taken from the bulk exhaust stream by adjusting
the dilution air flowrate and the total diluted exhaust gas
flowrate. The DR is determined by measurement of tracer
gases (CO2 or NOx) concentrations in the raw and diluted
exhaust as well as in the dilution air with exhaust gas
analyzers (EGAs). If CO2 concentration measurement in the
raw exhaust is not possible, it can be determined from fuel
consumption and the carbon balance equation, if the fuel
composition is known. These signals are transmitted to the
FC that either regulates the pressure blower (PB) or the SB
to maintain the desired exhaust split and DR in the DT.
4.2.3. Flow controlled systems with flowrate measurement
Fig. 12 shows a PFSS of the total sampling type with
flowrate measurement control. In these systems, the sample
is taken from the bulk exhaust stream by setting the dilution
air flowrate and the total diluted exhaust flowrate. The
total flowrate through the tunnel is adjusted with FC2 and
the sampling pump P of the particulate sampling system.
Fig. 11. Partial flow sampling system with tracer gas concentration
measurement (fractional sampling type) [54]. DAF: dilution air
filter, PB: pressure blower, FC: flow controller, EGA: exhaust gas
analyzer, DT: dilution tunnel, SB: suction blower, FH: filter holder,
PSP: particulate sampling probe, EP: exhaust pipe, SP: sampling
probe.
Fig. 12. Partial flow sampling system with flow measurement and of
the total sampling type (all of the diluted exhaust is led through the
PM filter) [54]. DAF: dilution air filter, FC: flow controller, FM:
flow measurement, DT: dilution tunnel, FH: filter holder, EP:
exhaust pipe, SP: sampling probe, P: sampling pump, Gexh : exhaust
flowrate, Gair : intake air flowrate, Gfuel : fuel consumption.
The dilution air flowrate is controlled by the FC1, which
may use the exhaust flowrate, Gexh ; or intake air, Gair and
fuel consumption, Gfuel as command signals for the desired
exhaust split. The sample flowrate into the DT is the
difference of the total flowrate and the dilution air flowrate.
The latter is measured with the flow measurement device
FM1 and the total flowrate with FM2. The DR is calculated
from these two flowrates. Accurate calibration of the FMs
relative to one another is required to prevent errors, in
particular at higher DR (above 15). The extraction of a
sample proportional to Gexh is usually achieved by keeping
the diluted exhaust flowrate constant and varying accord-
ingly the dilution air flowrate.
4.3. Characteristics and quality
It is rather obvious that accurate control and determi-
nation of the sampled flowrate is a major requirement for
PFSSs. For isokinetic systems an undistributed and uniform
flow is required to manage this. Experience [53] has shown
that pressure fluctuations of less than 2 – 5 mbars and rather
high flow velocities should be maintained to ensure good
control and accurate determination of the sample flow.
Additionally, accuracy of the systems controlled by tracer
gas concentration measurements depends on the accuracy of
the concentration measurement. Because of the potentially
low CO2 concentration in the diluted gases, especially in
low-load engine conditions, NDIR analyzers with several
ranges are needed, and each of those needs calibration and
eventually linearization that is a tedious task.
Flow measurement systems on the other hand, which
either use thermal mass or critical orifice FMs, seem to be
the most practical choice. For such systems, the group of
equations relating the engine exhaust flowrate, Gexh ; the
sampled exhaust flowrate, Gsm ; the dilution air flowrate, Gdl ;
and the total diluted exhaust flowrate, Gtot ; are:
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Gexh
rsam ¼ ¼ const ð1Þ
Gsm
Gsm ¼ Gtot 2 Gdl ð2Þ
In order to maintain a constant split ratio, rsam it is
practical to keep the diluted exhaust flowrate, Gtot constant,
and to control the dilution air flowrate, Gdl using Gexh or the
intake air flowrate and fuel consumption as input signals.
The accuracy of the systems using mass FMs can be
substantially improved by the so-called ‘relative calibration’
method proposed by Engeljehringer and Schindler [53].
According to this method, a calibration curve for Gsm is
obtained as follows: the mass flow Gtot is set to the desired
constant value, while the controller for Gdl is stepwise set to
values corresponding to DRs ranging from a value of 4 to
the maximum value required by the test run. At each set
value of Gdl the value of Gsm is measured by traceable
laminar flow elements. Deviations of the measured Gsm
from the calculated ðGtot 2 Gdl Þ are recorded and a
correction table of calibration is set up. As mentioned by
the authors, the required accuracy can only be obtained if the
proper calibration procedure has been carried out.
The split ratio, rsam depends on the size of the unit used.
Larger units sample a larger fraction of raw exhaust and
fractional sampling provides sufficient PM quantities. On
the other hand, in smaller units total sampling split ratios can
be as low as 0.01% of the total exhaust flowrate [48]. The
latter have drawn the interest of industry since they are
smaller and easier to use. Several designs are commercially
available: AVL’s Smart Sampler SPC 472, Horiba’s MDLT
Partial-Flow Dilution tunnel, Control System’s PSS-20,
NOVA-Microtrol 4 Particulate Measurement, Sierra Instru-
ments BG-2. All these systems are flow controlled with
flowrate measurements.
Accurate sampling is even more difficult in transient
testing since exhaust flowrate changes rapidly. If the
sampled flow follows the exhaust flow with time delay,
the PM emissions will not be estimated correctly. Silvis et al.
[48], using opacimeter data as an estimation for the PM
concentration, showed that for systems utilizing mass FMs
such time delay may be significant (about 1.35 s). Both
experiments and calculations have shown that in order to
maintain an overall accuracy of ^5%, the sample flowrate
has to follow the exhaust flowrate within a time delay of
300 ms or less. This response is very difficult to achieve due
to inherent time delays of intake air FMs, fuel FMs, flow
control devices, data acquisition system, and pneumatic
delays in quickly changing flows of compressible fluid in
tubes and tunnels. More or less, the same time delays occur
in systems using venturi FMs.
To overcome such problems, manufacturers applied the
so-called look-ahead method [48,68]. Silvis et al. [48] used a
prerecorded exhaust flow signal, rather than the online
signal, to control the PFSS flowrates. Yamagishi [68]
reported an additional improvement to reduce the delay in
the DT flow control: dilution air flow control is made by
651
a piezo-electric valve with a venturi flowmeter and a critical
flow orifice. As reported, both delay and response times at
90% of indication are significantly reduced (0.2 s).
The sources of variability discussed in the full-flow CVS
systems may be even more important in PFSSs. The large
surface-to-volume ratio of the TT is considered as the most
critical element for such effects [69]. Some experience has
been gained from studies on the behavior of these systems,
especially in steady-state tests and recommendations for
proper layout are given in the literature [53,69]. Correlation
studies between full-flow and PFSS resulted in deviations of
the order of 5% [70,71]. Based on these studies, European
and Japanese legislation for HDV accepted PFSSs for
emissions certification over steady-state tests.
Considering the complexity of the procedure and the
additional demands of transient testing, fundamental studies
in both wall –particle and gas– particle processes may be
required to get optimum engineering solutions for the
measurement of future engines. It will be necessary to set up
one or more test cells that incorporate some or all of these
recommendations in order to confirm experimentally that
the recommendations deduced from the fundamental studies
will indeed make the desired improvements in repeatability,
and will not significantly change the absolute level of
measured PM emissions. Design of experimental studies
should be based on the fundamental studies’ key variables.
Additional investigations to assist in explaining the
difference between observed and predicted phenomena
might include size distribution analysis and chemical
analysis of the filter samples.
4.4. Comparison to CVS
PFSSs can be regarded as CVS systems with all flows
downsized by the factor, rsam : Hence, the discussion on the
measurement quality criteria for CVS is effective for PFSSs
as well. However, some equivalence issues are imposed by
the design of the two systems and should be evaluated in any
case (raw vs. diluted exhaust sampling). An advantageous
characteristic of PFSSs is that due to the small split ratios, a
high DR may be achieved even at moderate dilution air
flowrates. Accuracy and sensitivity issues though may limit
this advantage. But PFSSs seem to be inferior to CVS in
terms of robustness due to the more sophisticated control
system used for proportional sampling. However, they are
attractive due to their small size and cost and have recently
received much attention in conjunction with the new
transient engine test cycle being under consideration.
Furthermore, if hot dilution needed to achieve the
temperature range of 42 – 52 8C becomes a customary
reality, PFSSs may be successfully used without the
significant power penalty for air heating required in full-
flow CVS systems.
In that respect and in the framework of the United
Nations ECE (Economic Commission for Europe) GRPE
(Group of Rapporteurs on Pollution and Energy) activities,
652 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Fig. 13. Schematic of the measurement setup used in ISO studies to
test suitability of PFSSs for engine certification over transient test
emission standards [58].
a number of correlation studies were undertaken by the
Worldwide Heavy Duty Certification group (WHDC)
[58 – 60] to unravel the relationship between CVS and
PFSSs techniques. The essential objective was to conclude
about the suitability of PFSSs for engine certification to
transient test emission standards and to develop the
appropriate ISO standards. The tests were conducted in
parallel in a number of laboratories7 and arrived to an
encouraging conclusion. A general schematic of the
measurement set-up used in the above tests is given in
Fig. 13.
However, EPA questioned the above conclusion
especially for transient conditions. The doubt mainly
stemmed from preliminary findings suggesting a major
disagreement between PFSS and the CVS [72]. Thus, EPA
together with the Engine Manufacturers Association (EMA)
and California Air Resources Board (CARB) sponsored
additional testing of the PFSSs8 [73]. The study concluded
about the potential of reliable PFSS designs pinpointing
areas for further improvements. In the following sections,
the major findings of the comparative studies are discussed.
4.4.1. PFSS optimization in comparison to CVS
The efficiency of PFSSs in sampling a constant fraction
of total exhaust (constant split ratio) is essential, especially
during transient testing. Stein [58] reported good transient
control capability for some of the PFSSs tested at European
and Japanese laboratories. Regression analysis between
sample probe and free stream exhaust gas flowrates over the
Heavy Duty ETC showed a correlation coefficient ðR2 Þ of
0.94 –0.99 for the AVL system and of 0.97 for a Control
System’s unit. JARI reported a R2 value of over 0.99 for the
Horiba system tested. Data for the other systems tested were
not available. The application of a look-ahead function in
7
EMPA in Switzerland tested AVL, Control System, and
Pierburg units, RWTÜV in Germany tested NOVA and AVL
systems, JARI in Japan tested Horiba’s device and SwRIe in the
US tested Sierra Instrument’s system.
8
Units tested: AVL, Horiba and Sierra Instrument.
the AVL system tested in the EPA/EMA/CARB study [73]
gave a R2 of 0.95 – 0.99 between the exhaust and the sample
probe mass flowrate, depending on the engine mode. The
relevant correlation coefficient for the Horiba system was
not given whereas the look-ahead option was not available
at Sierras’s system. Instead, Sierra used a transient dilution
air controller (TDAC) designed to speed the response of the
dilution air flowrate. However, the system was on a pre-
production stage and further work will be needed when
production units with TDAC are made available.
Further to flowrate control, parameters of interest for PM
determination may be distinguished to those critical for both
full and partial sampling systems: DR, filter face velocity,
sample filter loading and the number of test repetitions; and
to those essential for partial systems only, such as sample
line temperature and geometry (length, diameter) and
sample probe design. Table 3 presents the summary results
of a parametric study conducted to identify the effect of such
variables on recorded PM concentration [61] (measurements
conducted at EMPA). The study showed that the effect of all
parameters depended on engine operation condition and
were not consistent. From all variables examined, filter face
velocity and filter loading exhibited only little influence to
the result. PM levels tended to be slightly higher at low filter
face velocity and low filter loading. This finding would
allow lower minimum filter loading in future emissions
regulations to account for the low PM levels of future
engines. DR seemed to have a significant effect on both CVS
and PFSSs tests but this was not consistent at low load/high
SOF modes and the authors did not come to a definitive
conclusion. With regard to parameters relevant to PFSSs
only, significant effects were only observed in a few cases
but they were not consistent. PM levels tended to be slightly
lower with longer sampling lines so sampling lines shorter
than 1.5 m were recommended.
Stein [58] also reports results on the influence of the
sampling probe design to the PM emission reported with
two PFSSs (actual measurements conducted at RWTÜV).
From the four designs explored, namely open probe
facing upstream or downstream, hated probe and multi-
hole probe, the open probe facing upstream resulted to
closest proximity to the reference method results. The
effects of DR and sample line temperatures as well as
the DR value on PFSS operation were also reported in
the same study. All effects were found negligible with the
exception of a minor dependence of PM collected on the
DR. Similar to Ref. [61], this was not consistent in all
engine modes and was not considered further.
The effect of sampling parameters (probe geometry and
location and DR) on CVS–PFSS comparability was also
studied in the work by EPA/EMA/CARB [73], examining
three partial sampling systems (AVL, Horiba, Sierra
Instruments). Also, an optimization of the PFSSs
response was attempted using look-ahead functions and
concentration-control rather that flowrate-control for the
DR. This study showed that depending on the particular
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672 653

Table 3
ANOVA (analysis of variance) results of the measurements conducted for identification of the effect of various parameters on PM concentration
measured by CVS and PFSSs [61]

Parameter Mode CVS AVL Control system Parameter Mode CVS AVL Control system

Dilution ratio A100 – – Tunnel heating A100 – –

C75 ** ** C75 – –
B100 ** ** B100 – –
B50 * * B50 – –
B25 * * B25 – –
B10 – – B10 – –
ESC ** ** ESC ** **
ETC * ** ETC – –
Filter face velocity A100 – – – Sample line length A100 – –
C75 – – * C75 * –
B100 – ** ** B100 ** –
B50 * * * B50 – –
B25 – – – B25 – –
B10 – – – B10 * –
ESC * – – ESC – –
ETC ** ** ** ETC – –
Filter loading A100 – * – Sample line diameter A100 ** **
C75 – – – C75 – –
B100 – ** ** B100 – –
B50 – – – B50 – –
B25 * * – B25 – –
B10 – – – B10 – –
ESC ** ** ** ESC – –
ETC – – – ETC – –
Sample line temperature A100 – –
C75 – –
B100 – –
B50 – –
B25 – –
B10 – –
ESC – –
ETC – –

Results obtained with a Euro III HDE tested over ETC: European Transient Cycle, ESC: European Steady Cycle, and various modes of the
ESC (A100, C75, etc.; the letter corresponds to engine speed and the number to percent load). ( –) non-significant; (*) significant; (**) highly
significant.

PFSS system, sampling parameters may have different
effects but identified that close proximity between CVS
and PFSS results (i.e. within 5%) is possible when good
engineering practice is applied and that such systems
develop and improve. In particular, small deviations of
PFSS sampling from isokinetic conditions is beneficial for
PM mass determination and this conclusion is similar to
the study of Stein [58].
However, this particular study came with an interesting
finding with regard to the DR calculation. The usual
method, namely the calculation of DR on the basis of
flowrates only, gave results poorly correlated with the
CVS. Use of a CO2-based DR improved the comparison
for AVL and Horiba units but not for Sierra Instrument
unit. The authors attributed the improvement for the AVL
unit to the fact that this system uses hot-wire mass flow
sensors for flow measurement and control. Since this
method is influenced by the specific heat of the flowing
mixture and the sensors are calibrated with dry air, an
appropriate correction might be required. Similar correc-
tions would in principle be needed both for the Sierra unit
and the Horiba one which use hot-wire and subsonic
venturi flow sensors, respectively. In the case of steady
state tests, a straightforward correction can be applied
based on chemical composition of exhaust gases and the
heat capacity of H2O, CO2 and N2. The chemical
composition of the exhaust gas can be deduced for a
known fuel by measuring the fuel and intake air flowrates
[48]. Possibly, extrapolation of such a correction would
also improve flowrate measurement during transient tests.
654 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672

Fig. 14. PM emission results for three different engines tested over the Worldwide Harmonized Test Cycles WHTC (transient) and WHSC
(steady-state) with CVS and PFSS. Engine 2 was equipped with a DPF [60].

4.4.2. Comparison of absolute levels of PM emissions
between CVS and PFSS
With regard to the absolute level of PM emissions,
there are a number of conclusions that can be drawn from
the results of correlation studies between PFSSs and CVS
[58,60,73]. These studies mainly point out that PFSSs
measured generally lower (2– 15% on average) DPM
concentrations than CVS systems on steady state and
transient cycles. However, there were individual differ-
ences between measuring laboratories and sampling
systems examined. In contrast to the above, additional
tests reported by Schweizer et al. [60] conducted on a
single PFSS system showed slightly higher values than the
CVS system (of about 10%).
The results were highly inconsistent between CVS and
PFSS for tests on engines equipped with DPF [58,60].
PFSSs tended to measure slightly higher DPM in this case
(Fig. 14) and with increased standard deviation (Fig. 15).
However, increase of the standard deviation when a DPF is
installed also occurs for the CVS measurements. There are
two main reasons for the variability increase when using a
DPF, which are depicted in Fig. 16. First, the absolute DPM
emission levels are very low and measurement sensitivity
issues increase uncertainty. Secondly, almost all of DPM
collected comes from sulfate and volatile organic material.
Emission of such species is highly variable due to storage
and release effects in the DPF and in the measurement
system. In that respect, Fig. 14 shows that the percentage
difference between PFSS and CVS was about 50% when a
DPF was used, which is much higher than the 10%
difference obtained from engines without DPF. However,
since the absolute difference was below 0.007 g/kW h for all
engines, the agreement between the two systems was
considered good, particularly if someone takes into account
the reproducibility of different CVS systems.
In the EPA/EMA/CARB study [73] emission results
obtained with an AVL unit in the baseline steady-state tests
were lower than the CVS, ranging from 10 to 20%. Sierra

Fig. 15. Coefficient of variance of PM measurements conducted in a CVS and using three different PFSSs. Tests conducted in a number of cycles
(ETC: European Transient Cycle, ESC: European Steady Cycle, FTP: US Federal Test Procedure, JAP: Japanese 13 mode cycle) on a heavy
duty engine tested with and without (w/o) a particle filter (DPF) installed [58].
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Fig. 16. Comparison of PM composition with and without DPF for the tests conducted in the framework of ISO 16183 development [58]. ETC:
European Transient Cycle, ESC: European Steady Cycle, FTP: US Federal Test Procedure, JAP: Japanese 13 mode cycle, DPF: diesel
particulate filter.
Instrument’s unit gave somewhat contradictory results
measuring higher than CVS value for some modes and
lower for another. Results for a Horiba unit were 20 – 40%
lower than the CVS. This large divergence was most
probably due to flowrate problems of the particular unit.
Results for the AVL unit were further improved after the
implementation of a CO2-based DR (as discussed above). As
far as the transient tests are concerned, PFSSs were generally
found to underestimate the PM emissions. However, the
implementation of a look-ahead function improved the
results in the range of 5 –10% with respect to CVS for both
AVL and Horiba units. Sierra Instrument’s device using a
pre-production TDAC instead of a look-ahead function gave
a range of 5 –14% deviation from the CVS.
4.5. Summarizing table
The discussion so far made clear that there are two
candidate sampling techniques for PM determination of
future vehicle and engines, namely the full-flow CVS
system and different variants of PFSSs. In both cases, a
range of parameters needs to be accurately controlled to
increase sensitivity, representativeness and robustness of
the method, especially in the light of the continuously
decreasing emission levels. In that direction, regulation
and standardization authorities have reacted by consider-
ing improvements in existing methods. This also initiated
independent studies, cross-examining existing techniques
with alternative ones. The major improvements brought by
these efforts are summarized in Table 4 which presents the
important provisions of the EU and US legislation
regarding the measurement of PM emitted from future
HDVs and of the procedures specified by the new ISO
standard for PFSSs.
655
5. Alternative DPM determination methods
PM content of filter samples from future engines will be
as low as 0.2 mg. With the given regulated cycles, it is
questionable if such an amount is reliably detectable by
weighing a filter paper of about 1000 times heavier than the
sample itself. Additionally, it has already been shown
(Fig. 16) that PM from vehicles and engines equipped with
DPFs in the future will mainly consist of volatile material
condensed on the filter. This further complicates filter
handling due to possible loss or gain of condensable
material during filter stabilization. In addition, it has already
been shown (Table 2) that cycle repetitions to collect more
particulate mass on the same filter might not be a viable
solution and the unstable character of the VF may be
responsible for such an effect. In general, the reduction of
the solid soot content of DPM as technology improves and
the increasing importance of the VF for DPF equipped
engines brings several implications to the established so far
filter weighing method. It is later shown that such
developments are also responsible for the inadequacy of
traditional smoke measurement methods to provide even a
rough control method for future vehicles.
Additionally, instantaneous emission data become
increasingly important for various purposes including
engine research and development, emission inventorying,
atmospheric modeling, health effects studies, etc., i.e.
activities that have an influence on legislation. These data
are typically collected within emission factor programs,
which usually adopt the legislative test procedures with
respect to dilution and sampling but use near-real-time
instrumentation to obtain time-resolved PM emission over
transient cycles. The potential of such techniques has not yet
been fully evaluated for type approval applications, and
there are several on-going activities in this regard [21].
Some of these real-time techniques present additional
656 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Table 4
Comparison of the most important provisions for PM sampling of low emitting engines brought by EU Directive 1999/96/EC [54], ISO 16183
standard [56] and US 2007 Federal Register [55]
EU Directive 1999/96/EC
Sampling system requirements
Dilution air temperature: 25 ^ 5 8C.
Preheating above the upper limit if
ambient temperature is below 20 8C
(not exceeding 52 8C). Dehumidifi-
cation permitted. Dilution air filtration
or appropriate sampling to take into
account the background PM level is
recommended
Diluted exhaust gas temperature at
filter holder: maximum 52 8C
Deposition minimization requirements
Minimize deposition or alteration of PM,
all system parts electrically conductive
and grounded to prevent electrostatic
effects. DT and sample piping walls may
be heated up to 52 8C
Filter specifications
Teflon coated glass fiber or membrane filter,
minimum efficiency on 0.3 mm DOP: 95%
Filter face velocity: 35 –80 cm/s
Filter size: min diameter 47 mm, acceptable
also 70, 90 and 110 mm
Stain diameter defined as (filter diameter:
10 mm)
Filter loading
Minimum recommended (at the manufacturer’s
request, the ESC test sequence may be repeated
a sufficient number of times for sampling more
PM mass on the filter)
ISO 16183 Standard
Dilution air: temperature 15 8C.
Preheating up to 52 8C to heat
particulate sampling probe. Dehumidi-
fication permitted. Dilution air filtra-
tion or appropriate sampling to take
into account the background PM
level is recommended
Diluted exhaust gas temperature
at filter holder: maximum 52 8C
Minimize deposition or alteration of
PM, all system parts electrically
conductive and grounded to prevent
electrostatic effects, dilution tunnel
and sample piping walls may be
heated up to 52 8C
Teflon filter, minimum efficiency on
0.3 mm DOP: 99%
Filter face velocity: 35–100 cm/s
Filter size: min diameter 47 mm, accep-
table also 70, 90 and 110 mm
Stain diameter not defined
Minimum required (but lower also allowed,
with the agreement of the parties involved
and with the use of a balance of higher
resolution. Alternatively, a second run of
the test cycle on the same sample filters is
permitted, with the agreement of the
parties involved)
US 2007 Federal Register
Primary and secondary dilution
air temperature $15 8C. Air for
primary dilution filtered with
minimum filtration efficiency 98%.
Air for secondary dilution filtered
with HEPA with 99.97% minimum
efficiency, recommended also for
primary dilution. Background PM
load (primary dilution air) subtrac-
tion permitted
Diluted exhaust gas temperature
at filter holder: 47 ^ 5 8C.
Sampling at 30.5 cm (12 in.) maxi-
mum from secondary dilution
tunnel exit. A particle pre-classifier
(impactor or cyclone) must be
installed immediately upstream
of the filter holder, with 50% cut
point between 2.5 and 10 mm. It
should allow at least 99% of 1 mm
particles to pass through, in terms
of mass
Minimize diffusional and thermo-
phoretic deposition during transfer.
Double wall, thin wall, air gap in-
sulated or controlled heated sample
piping recommended. Piping sur-
faces in contact with the sample -
must be electrically conductive and
grounded
Teflon coated glass fiber or mem-
brane filter, minimum efficiency .
99%
Maximum filter face velocity
100 cm/s
Minimum filter diameter: 46.5 ^
0.6 mm
Minimum stain diameter 38 mm
No specific values are given. It is
recommended to maximize filter
loading
(continued on next page)
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672 657

Table 4 (continued)
EU Directive 1999/96/EC ISO 16183 Standard US 2007 Federal Register

Minimum recommended filter loading depending
on filter size: 0.5 mg for 47 mm; 1.3 mg for 70 mm;
2.3 mg for 90 mm; 3.6 mg for 110 mm (resulting
for the general recommendation 0.5 mg/1075 mm2
stain area)
Filter backpressure increase during sampling
Maximum 250 mbar (25 kPa)
Mass flowrate of the sample
The ratio of the sample flowrate over dilution
tunnel total flowrate must be maintained
within ^5% of the set value
Number of filters
2 (primary and backup)
Filter conditioning (empty and loaded)
Temperature: 22 ^ 3 8C
Relative humidity: 45 ^ 8% (dew point:
9.5 ^ 3 8C)
Sample filter weighing
Room conditions: as for conditioning
Analytical balance: resolution 1 mg,
precision 2 mg (for filters , 70 mm) or
resolution 10 mg, precision 20 mg (for
filters 70 mm).
Reference filter weighing permissible
deviation: 5% of the recommended
minimum filter loading
Additional specifications
Minimum required filter loading depending
on filter size: 0.11 mg for 47 mm; 0.25 mg for
70 mm; 0.41 mg for 90 mm; 0.62 mg for
110 mm (resulting from the general requirement
of 0.065 mg/1000 mm2 filter area)
Maximum 250 mbar (25 kPa)
1 (main)
Temperature: 22 ^ 3 8C
Relative humidity: 45 ^ 8%
(dew point: 9.5 ^ 38)
Room conditions: as for condi-
tioning
Analytical balance: resolution 1 mg,
precision 2 mg for all filter sizes.
If filter loading lower than the mini-
mum required is accepted, a 0.1 mg
resolution balance is required.
Reference filter weighing permissible
deviation: maximum 10 mg
In case of unstable balance reading, the
use of neutralizer is recommended, to
eliminate electrostatic effects
Not defined
The ratio of the sample flowrate
over dilution tunnel total flowrate
must be maintained within ^5%
of the set value
1 (main)
Temperature: 22 ^ 3 8C
Dew point 9.5 ^ 1 8C
Room conditions: as for
conditioning
Analytical balance: precision
(standard deviation) , 0.25 mg,
readability 0.1 mg.
Reference filter weighing
permissible deviation: maximum
10 mg (two reference filters are
recommended). The weighing
results must be corrected for
buoyancy effects. Specific calcu-
lation scheme is given, based on
ambient conditions (barometric
pressure, temperature, humidity)
and the densities of sample filter
and calibration weight
Static electricity neutralizer is
generally recommended

ISO requirements correspond to PFSSs while the EU Directive and US Regulations to full flow dilution systems.

advantages such as not requiring collection of particulates
but measuring mass in airborne conditions, or even
providing in-line separation to solid and volatile material
without the need of analytical techniques.
For the above reasons, and with a view to the future, it
will be useful to look into the alternative methods proposed
for the measurement of particulate mass. In the following
sections, the operation principles of the most promising
methods are briefly reviewed and discussed. It needs to be
stressed though that the distance in the operation principle of
some of these techniques and the established gravimetric
method might eventually prove too large for a correlation to
be established. Most importantly, it appears that the
complexity of VF and its sensitivity to sampling and
measurement conditions is the most common obstacle in
establishing such a correlation. However, one should not
evaluate available techniques based only on their ability to
correlate with filter sampling as especially as future
emission levels are concerned, properties such as sensitivity
and repeatability become equally important.
658 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
5.1. Techniques based on filter heating and gas analysis
Techniques based on filter heating aim at increasing the
sensitivity in the determination of the mass collected on a
filter by first oxidizing the collected material to gaseous
species and then use gaseous analyzers to record concen-
trations, instead of weighing the mass collected. These are
on-line but not real-time techniques and can provide
distinction of the collected mass to solid and VFs.
In the mid-1990s Rupprecht and Patashnick developed
the Series 5100 Diesel Particulate Measurement System
[74]. This device draws a sample from a probe located in
the DT onto an internal high-efficiency, self-regenerating
filter via a heated sampling tube (collection phase). After
PM collection, the device processes the sample utilizing
an automated thermal-analysis technique (analysis phase).
In this phase the filter temperature begins to rise in a
furnace, after purging any residual exhaust from the
system and measuring the amount of CO2 trapped inside.
As the filter temperature increases up to 350 8C, volatiles
which either oxidize or evaporate from the filter, enter the
gas stream and travel to the afterburner. The latter
oxidizes any volatile material, converting the carbon
based components to CO2. At a second stage, the furnace
temperature increases to 750 8C and the remaining soot
also oxidizes to CO2. The recorded initial CO2 reading is
subtracted from both subsequent signals to deduce a net
value of carbon concentration (milligram of carbon
divided by the volume of gas collected) distinguished to
soot and SOF. To the authors’ knowledge, correlation
studies with the reference method have not been
published. Although the technique has been developed
for engine development purposes, it may also be useful in
emissions characterization if on-line particulate compo-
sition is of interest.
A new measurement technique developed by Horiba [75]
uses vaporization, oxidation and deoxidation of collected
PM components as shown in Fig. 17. Sample gas from the
DT is drawn through a quartz fiber filter, according to
conventional procedures. The particulate sample is collected
on the quartz fiber filter, the characteristics of which remain
unchanged under high temperatures. The filter is then placed
into a furnace heated to 980 8C in a N2 gas flow. SOF and
sulfates of the particulates are vaporized. After vaporization,
sulfates are reduced to SO2 and measured by an SO2 NDIR
detector while the vaporized SOF is converted to CO2 and
measured by a second NDIR detector. Subsequently O2 is
introduced into the furnace at constant flowrate and the
remaining soot is oxidized to CO2 and measured by the CO2
detector. The time required to measure one sample is four
minutes. The output of the CO2 analyzer is integrated while
introducing N2 gas to determine the mass of SOF, and while
introducing O2 gas to determine the mass of soot. The SO2
analyzer output is also integrated to determine the mass of
sulfates. So far, evaluation of the performance of the system
has been conducted and published by the instrument
Fig. 17. MEXA-1370PM measurement system configuration [75].
Particulate samples are collected on the quartz fiber filter at ambient
conditions. After measurement, the quartz filter is placed at 980 8C
under nitrogen atmosphere for vaporization of VF to occur. Sulfates
are reduced to SO2 and measured by the SO2 detector while the soluble
organic fraction (SOF) is converted to CO2 by addition of O2 and is
measured by the CO2 detector. After VF determination, additional O2
is introduced into the furnace and soot is oxidized to CO2 which is also
measured by the CO2 detector. After VF determination, additional O2
is introduced into the furnace and soot is oxidized to CO2 which is also
measured by the CO2detector. This result in in-line determination of
soot, SOF and sulfate content of particulate.
manufacturer only. The detection limits reported were
0.17 mg for SOF, 0.15 mg for soot, and 6.1 mg for the
sulfates. The correlation coefficient with the reference
method was 0.96.
In order to verify the correlation with CVS at ultra low
mass concentrations, an actual particulate mass on a quartz
fiber filter was measured with a microbalance and next was
cut into 32 equal pieces. The particulate mass on a sector
piece was calculated and then measured and analyzed with
the alternative technique. The correlation coefficient
between the PM mass inferred from the ratio of the mass
of the whole filter to the mass of each cut piece, with the PM
mass obtained by the alternative technique was reported to
be 0.99. The slightly smaller value than the ideal was
attributed to losses occurred when the filter was cut. Also,
possible differences with the CVS technique due to different
filter material used should be evaluated. Quartz fiber filters
usually show a higher collection of SOFs than Teflon coated
or pure Teflon ones [76]. In any case, a thorough evaluation
of its capabilities by independent laboratories is needed.
5.2. Optical techniques
In optical detection methods, the interaction of aerosol
particles with the incident light serves as basis for the real-
time measurement of particle concentration. The operation
principles of these methods are based either on the optical
phenomena that are a direct result of the scattering/absorp-
tion of light by the aerosol particles or on the detection of
radiation emitted after particle heating. Extensive discus-
sions on the fundamental issues can be found in reference
aerosol textbooks [77 – 79]. The amount of literature
concerning the application of optical methods in the
combustion field (including diesel) is huge and the review
of it is beyond the scope of this paper. Zhao and
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Ladommatos [80] give an extensive review of the topic
whereas the recent progress of some interesting techniques
is given in the work of Bockhorn [81] and Lehre [82].
Optical methods are generally very sensitive, provide
nearly instantaneous response and avoid any physical
contact with the particles. Some can also provide infor-
mation on the size of the particles. On the other hand, light
scattering/absorption strongly depend on particle size and
refractive index and are prone to interference from gaseous
species. According to the Rayleigh law, the intensity of light
scattering scales with the sixth power of particle diameter
for particles smaller than ,0.2 mm [78] when visible
radiation is used. Therefore, techniques based on the
scattering of visible radiation are generally insensitive to
ultrafine particle concentrations. As far as light absorption is
concerned, gaseous molecule interference becomes import-
ant. NO2, which is relatively abundant in new diesel engines
equipped with oxidation catalysts, efficiently absorbs green-
light. This introduces a high background level for PM
measurements and decreases the sensitivity and representa-
tiveness of related methods. Most importantly though, light
absorption and scattering by the SOF is rather negligible.
Hence, optical techniques are very suitable when soot
concentrations are prominent but can be insensitive when
DPM is dominated by volatile species, such as downstream
of DPFs. Such limitations to the determination of the DPM
mass raise the need for many assumptions to relate the
measured signal to the total particulate mass concentration,
as obtained by the gravimetric method. These constraints
may be partially lifted using multiple wavelengths or
multiple angle scattering to obtain more than one values
[83]. Still, although such methods may be clear improve-
ments to existing techniques, their application to actual
exhaust testing and their comparability with alternative
methods remains to be proven.
5.2.1. Light-extinction methods
Aerosol particles that are illuminated by a beam of light
reradiate it in all directions (scattering) and simultaneously
transform part of it into other forms of energy (absorption).
The overall process is called extinction and deals only with
the attenuation of light along an axis. Light-extinction
methods using commercially and non-commercially avail-
able instruments (opacity meter, smokemeter, aethalometer)
have been used extensively to monitor diesel PM emissions in
1970– 1980s and there is thus considerable information in the
literature. One group of these instruments is based on opacity
principle and follows the Beer– Lambert law [84 – 89]
IT
u¼12 ¼ 1 2 expð2AE MLÞ ð3Þ
I0
where u is the opacity; I0 and IT ; the incident and transmitted
light beam intensities; L; the path length through a smoke
plume of particle mass concentration M; AE is the specific
optical extinction. The latter is the effective optical cross-
section for attenuation of light per unit particulate mass and
659
has units of m2/g, whereas the product AE M is the total
attenuation or extinction coefficient and has units of
reciprocal length. If AE is constant, which is true if the
emitted particles are constant in size, shape, density and
chemical composition, then the opacity is uniquely related to
the mass concentration [90].
The majority of correlations between PM mass concen-
tration and opacity measurements published in literature were
derived from steady-state engine tests. Since the dilution
process significantly influences the quality and composition
of the collected particulates, opacity meter measurements do
not generally provide good correlation with the total
particulate mass. Concerning transient tests, early attempts
[88,89] to make reliable measurements, suffered from errors
mainly due to organic material condensed. Krempl et al. [91]
developed a method for separate but practically simultaneous
measurement of both hydrocarbon and particles mass
concentration. This method was based on optical extinction
measurements at distinct frequency bands in the infrared (IR)
region. The authors found considerable differences between
steady state and transient tests both in PM and hydrocarbon
emissions. They correlated their measurements to total PM
emissions, which compared well to those determined
gravimetrically over the whole measurement range. Although
simple, cost-effective and with excellent time response,
opacity meters are not suitable in measuring diluted exhaust
of current vehicles because of the small solid fraction emitted.
Newer developments [83,92] using multi-wavelength extinc-
tion techniques showed the potential to measure on-line and
in situ directly the undiluted particle emission. It was found
that a refractive index of n ¼ 1:92 2 0:66i9 delivers best for
all diesel engines tested. Comparing the optical results (with
this refractive index) with filter results, the authors found
good agreement over the whole load and different engines for
soot density of 0.55 g/cm3.
The other group of instruments operating on light-
extinction is based on ‘aethalometer’ principle [93 – 95],
where the Beer – Lambert law is insufficient to describe light
extinction. These instruments use the collection of aerosol
on filters, followed by an optical measurement to determine
light absorption. In principle, a simplified version of the
aethalometer is the popular to engine research ‘smoke-
meter’. In a smokemeter a relative concentration of soot is
obtained by filtering a fixed quantity of exhaust through a
paper filter and comparing the opacity of the paper filter
with a reference opacity scale. The aethalometer is a real-
time version of such an instrument. It is mostly utilized for
ambient monitoring and recently has been tested in diesel
exhaust measurements [95]. It continuously measures
9
Refractive index is written as the sum of a real and an imaginary
component to take into account both scattering and absorption. The
imaginary part determines the attenuation of the wave as it
propagates through the medium and, therefore, gives rise to
absorption; the real part determines the velocity of propagation
and gives rise to scattering.
660 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
the amount of light transmitted through a quartz filter, while
particles are being deposited on the filter. The rate of
decrease of transmissivity, divided by the sample flowrate,
is directly proportional to the light absorption coefficient of
the particles and the rate of particle accumulation on the
filter. The measured extinction is reported as black carbon
concentration using a specific algorithm [96]. A problem
mentioned is the great variation of absorption coefficients
depending on the origin of the particles [10] and therefore, a
semiempirical approach is required to derive the appropriate
constant for each application. However, the instrument is
designed for low aerosol concentrations and a secondary
dilution is necessary in order to measure exhaust particles.
Uncertainties in the value of the secondary DR may
introduce additional errors into its readings [95].
5.2.2. Light scattering photometry
Measurement of the light intensity scattered by particles
can be used to obtain information on their mass concen-
tration. This technique is involved in the ‘nephelometer’ (or
photometer) originally designed for ambient measurements
that has recently applied in DPM measurements [95,97].
According to this method, a diluted exhaust sample is drawn
into the sensing chamber of the photometer, where a beam
of laser illuminates it. The intensity of the scattered light is
then detected by a photo-detector at 908 to the incident light
path. The nephelometer uses this measured light intensity to
determine the particulate concentration in the exhaust
sample. Studies showed good correlation with the CVS
filters. However, the correlation was changed for different
operating conditions and vehicle types. The nephelometer
tends to overestimate the DPM concentration in high engine
loads, while underestimating it in steady speed, road load
operation. However, it shows an excellent signal-to-noise
ratio, it is free of interference from non-particle sources (e.g.
gaseous molecules), it has good time resolution and is
simple and low-priced.
5.2.3. Laser induced incandescence (LII)
A more complicated, laser-based technique for particu-
late mass determination is the laser-induced incandescence
(LII). LII was identified by Eckbreth [98] and the technique
was introduced as a combustion diagnostic tool for
acquiring spatially and temporally resolved quantitative
measurements of soot particle volume fraction over a wide
range of soot concentrations [10,80]. More recently, it has
been also proposed as a tool for exhaust gas measurements
[99,100] (Fig. 18). Particle incandescence occurs when a
particle interrupts a high intensity pulse laser beam. The
particle absorbs energy from the beam, which causes its
temperature to increase. At the same time, it looses energy
by heat transfer mechanisms to the surroundings. If the
energy absorption rate is sufficiently high, the temperature
will rise to levels where significant incandescence (essen-
tially blackbody emission) and vaporization will occur. The
incandescence signal is roughly proportional to particle
Fig. 18. General layout of the Laser Induced Incandescence (LII)
measurement system in the configuration used in the study of
Snelling et al. [104], to compare with the gravimetric PM method. A
laser pulse is focused to form a sheet through the particle sampling
volume. The incandescence produced as the airborne particles are
hit by the laser pulse is recorded by three (single frequency)
photomultipliers located at a 358 plane relevant to the laser sheet.
This signal is then transformed to airborne particle volume fraction
and mass, assuming a density value for the shoot particles and is
compared to the mass of particulate collected on the filter.
volume and is recorded by photomultiplier detectors. Then,
mass can be derived by the volume reading assuming a
value for soot particle density. For variable densities, the
measurement must be calibrated to determine effective
particle density and to obtain mass concentration. LII is a
very sensitive technique, reaching orders of magnitude
higher sensitivity than the gravimetric method (i.e. mg/m3
range). Comparison with the reference PM method
[101– 105] established generally satisfactory correlations
but with discrepancies over engine modes with high PM
concentrations or high SOF contents. The latter was not
surprising since non-carbonaceous material absorbs very
little energy and, moreover, temperatures above 4000 K are
far above the vaporization temperature of any SOF. A
potential useful technique for real-time assessment of
carbon-bounded SOF is laser-induced vaporization. As
suggested by Case and Hofeldt [100] the different
dependencies of the incandescence and scattering signals
between carbon and condensed hydrocarbons can be
exploited to measure the SOF fraction of the DPM.
However, this potential has not been realized up to now.
5.2.4. Photoacoustic spectroscopy
Photoacoustic spectroscopy has been applied in exhaust
monitoring for more than two decades [88,95,106,107]. In
principle, this is not a direct optical technique because light
is only used as an energy source and not for particle
detection. In this method light energy produced by a laser
source absorbed by the aerosol is converted to heat.
Because of the high thermal conductivity of aerosol,
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
Fig. 19. Schematic view of the prototype photoacoustic spectrometer [108]. A laser beam is used to heat up the sample airborne particles. As
particles cool down, heat is dissipated to the surroundings increasing the pressure of the particle carrier air. The pressure waves are amplified
appropriately and detected. The mass of the airborne particles is then deduced by measuring the sound pressure.
the absorbed heat will flow rapidly to the surrounding air.
Heated air responds by expanding its volume and
increasing its pressure. By placing the aerosol-laden air
into an acoustic resonator and modulating the electromag-
netic power at its resonance frequency, the varying
pressure disturbance (acoustic signal) can be amplified by
the build-up of a standing acoustic wave in the resonator.
Thus, by measuring the sound pressure that is associated
with aerosol light absorption, a measure of elemental
carbon concentration can be obtained. The main conclusion
derived from photoacoustic device application in DPM
emissions measurement is that its sensitivity depends
strongly on the flowrate of the sample gases, the
composition of the diluting gases and the modulation
frequency of the light. Another problem resulting from
operation characteristics concerns the sensitivity of the
technique to the percentage of volatile material present in
the exhaust. The most recent instrument developed for
measuring light absorption by aerosol and applied in diesel
exhaust field [95] is the photoacoustic spectrometer
(Fig. 19) described in detail by Arnott et al. [108]. Similar
to LII, the photoacoustic spectrometer technique is very
sensitive to light absorbing material (e.g. elemental carbon)
and rather insensitive to volatile species.
5.3. Fast-response flame ionization detection
Flame ionization detectors (FIDs) are widely used to
measure gaseous HCs because of their fast response and
reliability. They have also applied to estimate the amount of
condensed/adsorbed HCs on the particulates [87]. More-
over, they have recently been used as a technique for the
real-time analysis of PM [109 – 111]. In an FID, a H2 – O2
flame produces relatively few ions but several highly
energetic H atoms. Such hydrogen atoms of high kinetic
energy collide with another atomic or molecular species,
which is subsequently ionized [110]. The collision produces
positive ions and electrons, which move towards the
electrodes by the application of an electrical field, thus
producing the ionization current. When trace amounts of HC
661
compounds are added to the flame, the number of ions
increases by an order of magnitude and hence a measurable
ionization current is produced. This current signal is
proportional to the number of carbon atoms present in the
flame per unit time. In a fast response FID, the sample gas is
introduced directly into the flame chamber to minimize the
gas transportation time, which otherwise leads to significant
signal delays due to the gas diffusion and mixing processes
in conventional FIDs. Cheng et al. [112] comment in detail
on the operating principle and the application of the system
in automotive research.
Arcoumanis and Megaritis [109] used a fast response
FID together with an opacity meter targeting to the
development of an alternative method of quantifying real-
time PM concentration during steady and transient engine
operation. The method was based on instantaneous
measurement of smoke and unburned HCs in the raw
exhaust and their steady state correlation with the PM mass
concentration in the diluted exhaust. The authors found that
CVS PM can be correlated within 20% of the combined
signal obtained with concurrent smoke number and gaseous
HC FID measurements over transient tests. As an alterna-
tive, the authors suggested the use of two FIDs in order to
determine the SOF of PM, rather than deducing it from
gaseous HC. In this configuration one FID would measure
the total emitted HC in the raw exhaust sampled at 190 8C
and other the total emitted HC at or below 52 8C by taking
samples from the diluted exhaust. The difference in the FID
signals should in principle correspond to the PM SOF. This
was also shown by Abbass et al. [113].
FIDs can also be used to determine particle number
concentration, recording the sharp ion pulse is generated
when a particle is introduced in the FID chamber, due to the
chemi-ionization of its attached HCs [110]. Kawai et al.
[111] examined the use of a FID spike response as an
indicator of PM concentration. In their sampling system,
exhaust was led to an FID either directly at 191 8C or
passing through a filter maintained at 52 8C. In the former
case, a spiky composite signal from HC and soot was
recorded, while in the latter, a smooth signal originating
662 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
from gaseous HC at 52 8C was recorded. Soot concentration
was then deduced by the frequency of the spikes and SOF by
the difference in the levels of the signals at the two different
temperatures. Comparisons with the standard gravimetric
method produced a linear correlation.
The potential for real-time PM measurement using an
FID was further elaborated by Fukushima et al. [114] who
applied this technique for continuously measuring soot and
volatile material separately. Over steady state tests diluted
exhaust PM was simultaneously measured by the FID
system and the standard gravimetric method. The corre-
lation coefficients ðR2 Þ yielded were ,0.9 for soot and ,0.7
for SOF. Satisfactory correlations were also found for FID
sampling directly from raw exhaust while the potential to
study SOF and soot in real time (response time ,1 s) over
transient tests was also demonstrated. This work resulted in
the commercialization of an instrument (Horiba MEXA-
1220PM) using two FIDs at different temperatures.
Although these studies showed the possibility for PM
recordings with real-time resolution and satisfactory agree-
ment with the standard CVS procedure, there is no
significant independent work with this technique to
construct any solid conclusions.
5.4. Tapered element oscillating microbalance
Tapered element oscillating microbalance (TEOM)
monitor was introduced about twenty years ago in diesel
PM emissions research [95,115 – 122]. Since its introduc-
tion, new designs have incorporated a number of subtle
improvements that have made it easier to use and able to
generate better quality data [123]. Whitby et al. [115]
describe the operation theory (Fig. 20). The key component
of the system is a hollow, tapered, cantilever element, which
is forced to oscillate at its natural frequency via a feedback
system. On its narrow end the tapered element accepts a
disposable filter cartridge and its wide end is connected to
Fig. 20. Schematic of the TEOM sampling and measurement
configuration [120]. Particulate matter accumulates on the open end
of an oscillating element changing its resonance frequency. The
change in frequency is then monotonically related to the mass of
particulate collected and is recorded by an appropriate detector.
a mass FC. The filter is mounted on the cartridge and the
diluted exhaust is drawn through it, where particles deposit.
The filtered exhaust is then drawn through the hollow tube.
An electronic feedback system initiates and maintains the
oscillation of the tapered element. The filter and the element
can be represented by a spring-mass system, where a change
in mass correlates to a change in frequency. The operating
frequencies range from having a loaded filter (low
frequency, more mass), to not having a filter installed
(high frequency, less mass). As the filter weight changes due
to PM accumulation, the oscillation frequency of the
element changes. The TEOM measures the frequency of
the tapered element oscillation and calculates a change in
filter mass. The equation that relates the mass of PM at any
point during a test to the frequency of the oscillation is
Dm ¼ K0 ðFt22 2 F022 Þ ð4Þ
where Dm is the mass of particles accumulated; F0 ; the
initial frequency; Ft ; the frequency at any other moment t;
K0 is a calibration constant for the tapered element.
Although this expression for Dm is non-linear, it is
monotonic (single-valued) independent of the mass col-
lected, and depends only on the constant K0 :
The study of Whitby et al. [115] was the first application
of TEOM in the area of diesel research. Although their
results were based on a few of exploratory tests, they
suggested that TEOM has the potential to become a valuable
tool in particulate measurement, showing reasonable
agreement with the reference method. They pointed-out,
however, that several factors such as water vapor, sampling
temperature, calibration and filter media had to be explored.
In a later study [116] the same authors examined in detail the
correspondence between TEOM and the conventional
filtration methods in more detail with a second-generation
TEOM. The focus of their study was not on the real-time
character of the emissions but on the above-mentioned
correspondence that was identified as more critical to the
acceptance of the TEOM as a practical laboratory tool. Their
main conclusion was that the TEOM vs. gravimetric
difference in mass was due to the fact that water and
organic volatile material are retained to a greater degree by
conventional filters. This difference was attributed to the
higher vacuum on a TEOM filter. They suggested a
correspondence between this higher vacuum with a
temperature increase in conventional filtration in order to
achieve improved agreement.
Shore and Cuthbertson [117] tested various light and
heavy-duty engines over different transient cycles in order
to assess the suitability of the TEOM for PM measurements
and to determine its reliability by comparing the results with
those obtained by the reference procedure. The vehicles
tested yielded real-time data significantly different from one
another. Although the authors were not in the position to
pinpoint the engine parameters crucial in determining the
shape of readouts, this finding is considered important,
indicating TEOM as appropriate in particulate measurement
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
programs during which specific areas of high particulate
emissions can be identified. Differences observed during
tests over different cycles were attributed to the driving
schedule specifications. Extensive data were given regard-
ing the correlation between TEOM results and those
determined by the reference method. The data showed a
considerable degree of variation from one vehicle to
another, one cycle to another and even from one test to
another on the same vehicle over the same cycle. In any
case, the results obtained by TEOM were lower. These
discrepancies were attributed: (1) to differences in the filter
temperature leading to lower retention of volatile material
by the TEOM filter (operated at a constant temperature
(50 8C) due to temperature dependent frequency character-
istics of the element) and (2) to differences in density and
structure of the two media, which could influence the
applicability of the K0 value used in TEOM data reduction.
As regards the influence of sample flowrate they found that
there was a near-direct proportion of filter retention to
flowrate for flows within 0.8– 3 l/min (the TEOM unit can
be set for sample flowrates of 0.5 –5 l/min) and concluded
that a rate chosen within this range was not critical.
Saito et al. [118] conducted comparison measurements
using TEOM, a high-sensitivity light extinction opacimeter
and the standard filtration method. TEOM data were well
correlated to the filter collection method under cruise and
modal operating conditions. Comparisons with opacimeter
measurements showed that the TEOM data were also
correlated except for some distinctive engine conditions. In
continuous measurements it was found that the opacimeter
is better than the TEOM method in terms of transient
response and sensitivity.
In 1998, D.A. Okrent of Pupprecht and Patashnick Co.
published a paper [123] where the third generation of TEOM
device was presented. Focusing on the reported factors thought
to affect TEOM data, the author formulated a method that
optimizes the signal to the microbalance. It was demonstrated
that the filter/microbalance temperature has the greatest
impact on the overall total mass of the sample collected, and
tended to reduce the moisture and volatile organic compounds
adsorption rate. For this reason, adequate warm-up times after
a filter change were suggested to provide sufficient tempera-
ture stabilization. The use of the TX40 Pallflex filters which,
due to their higher efficiency, shorten the time needed to build
up a particulate deposit on the filter was also suggested. In
contrast with the sample flowrate range suggested by Shore
and Cuthbertson [117], the author claims that a better
correlation between TEOM and standard filtration method
was found for higher flowrates, in the range of 5 l/min.
Although a high flowrate decreases the filter life, this finding, if
confirmed by further investigation, is of great importance
since high flowrates are necessary for the latest technology of
clean diesel engines. Consequently, filter life should be
sacrificed in the interest of obtaining better quality data.
Chan and He [120] introduced a new technique for real-
time measurement of PM mass concentration using a third
663
generation TEOM and a fast-response FID. This combi-
nation was judged necessary to compensate for HC
component, since neither TEOM nor other instruments for
mass measurement concentration have been able to fully
capture the HCs signature/component in the diesel exhaust.
By maintaining the TEOM collection temperature at its
standard value (50 8C), they derived an empirical formula
for the correlation of mass of particulate emissions such as
PM ¼ 0:981PTEOM þ 0:257HCFID ð5Þ
3
where PM, PTEOM and HCFID are all in mg/m , while the
coefficients 0.981 and 0.257 showed the weighted contri-
butions of PTEOM and HCFID in PM, respectively. Their
results showed that both TEOM and FID respond rapidly to
variations in diesel exhaust content and, consequently, they
have to be considered as usable for real-time PM mass
concentration measurement.
Jarrett et al. [121], recognizing adsorption – desorption
of moisture as an important mechanism influencing
TEOM accuracy and sensitivity, developed a model to
predict its effect on the TEOM filter. Their results showed
a strong linear correlation between moisture mass on the
filter and ambient moisture content in the air. Conducting
measurements with new and used filters concluded that
the latter ones adsorbed more moisture. This finding
suggests that filter moisture retention is a function of
accumulated PM on the filter. Therefore, they suggested
subtraction of the model predicted change in moisture
from the raw TEOM data in order to yield more accurate
representation of instantaneous PM.
Kelly and Morgan [122] carried out steady-state
measurements utilizing a TEOM at two different test
facilities, including a full-flow CVS and a partial flow
dilution system. Their aim was to evaluate the performance
of the TEOM in comparison to the reference procedure. The
correlation between the two techniques was satisfactory but
TEOM results were consistently lower than CVS PM, in
agreement with the previous studies. They investigated VF
variability by changing the sampling period, the collection
temperature, the TEOM purging period, the collection
filters, and the exhaust flowrate and concluded that
differences observed are simply explained by greater
volatilization from the TEOM filter. They analyzed their
results applying the methods of Chan and He [120] and
Jarrett et al. [121] and found out that FID data do little to
improve the relationship between TEOM and conventional
method and that moisture corrections were not able to
explain several of their observations. They suggested that a
collection temperature of 30 8C and a flowrate of 4.5 l/min
gave results that were approximately equivalent to the
conventional method. However, they underlined the need to
first understand the responsible underlying mechanisms for
VF variation and then to develop a method to measure DPM
with proximity to the CVS results.
Summarizing, TEOM is based on filtration of a particle
laden exhaust sample, similar to the standard gravimetric
664 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672

its resonance frequency decreases. Thus, a quantitative

Fig. 21. Schematic of the Quartz Crystal Microbalance [125].
Particulates are collected on a thin quartz resonator and decrease its
resonance frequency. The frequency shift and the added mass are
then quantitatively related.
method. Mass determination is not conducted gravimetrically
but using a novel technique increasing sensitivity. However,
mass is calculated by integrating a real-time signal, rather that
subtracting an initial from a final value. This increases the
uncertainty of the method. Based on the available evidence,
the representativeness of the method depends on parameters
mainly related to the filter used (temperature, face velocity,
material) and sample condition (moisture and SOF content).
Although such parameters have been investigated enough to
provide an interpretation framework for the lower PM mass
value given by TEOM compared to the CVS, more modeling
and experimental work might be needed to find for
further improvement of the correlation. Similar to most of
the techniques demonstrated so far, the comparability of the
TEOM with the standard method on DPF equipped vehicles
remains to be proven, given the negligible solid particle
emissions of such vehicles.
5.5. Quartz crystal microbalance
Quartz Crystal Microbalance (QCM) utilizes the
piezoelectric effect to provide mass measurements
(Fig. 21). As DPM is collected on a thin quartz resonator,
relationship between the oscillation frequency shift and
the added mass is established. QCM technique was very
popular in the 1970s but then it disappeared due to
problems with overloading, bouncing, diffusion losses and
calibration [10,124]. The natural frequency of oscillation
is very high (, 5 MHz), ensuring independence of the
ambient mechanical vibrations, while a resolution of
^2 mg/m3 is claimed. A new prototype design, fast
enough for transient measurements has been recently
studied in the framework of the UK Particle Measurement
Programme [125]. A broad agreement between the
prototype QCM and regulated particulate mass was
identified at Euro III mass emissions levels. More
specifically, correlation coefficients squared with the
gravimetric method were ,0.94 for steady state tests
and ,0.7 for transients when sampling from CVS diluted
exhaust at Euro III emission levels and a relationship of
mutual mass reduction is generally reported at particulate
mass levels below Euro IV and post-DPF. Overall the
study concluded that the prototype QCM is a more
suitable technique than TEOM, mainly because it
appeared to provide a more repeatable measurement, and
was subsequently recommended as complementary to the
reference measurement system. This should still be
considered as limited evidence on a prototype device.
5.6. DMM-230 mass monitor
Very recently [126], a new instrument was presented
for airborne particle mass measurements by Dekati, Ltd
(Finland). This instrument (Fig. 22) is based on the design
characteristics of the popular Electrostatic Low Pressure
Impactor [127] where particles are classified aerodynami-
cally on impactor stages and their number concentration is
deduced by recording of the charge after particles have
been charged in a unipolar corona charger. In the new
instrument, a triode-type charger has been used to
eliminate small particle losses and ion escape and

Fig. 22. Schematic of the DMM-230 Mass Monitor and operation principle [126]. Airborne particles are charged in a triode charger and a single
mobility channel measures the current measured by small particles to deduce the mobility size distribution of the sample. Particles are then
sampled by an electrical low pressure impactor to deduce the aerodynamic size distribution. Fitting of the two size distribution provides the
effective particle density, used to calculate to total mass of the particles.
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
a single mobility channel precedes the aerodynamic
classification. Based on the current measured on the
mobility channel, a lognormal mobility size distribution is
fit and it is compared with the aerodynamic size
distribution obtained from the impactor. According to
Ristimäki et al. [128], fitting of the two distributions
provides the effective particle density which can be
combined with the mobility particle distribution to deduce
the total airborne particle mass.
There is still limited experience from the use of this
instrument. Therefore only general remarks can be made at
present with regard to its expected performance. A
significant advantage is that no collection or deposition of
particles is made to weight them. Mass is deduced in near
real-time while particles are airborne with a sensitivity
down to 1 mg/m3 and time resolution of 1 – 2 s. Airborne
measurement eliminates humidity and condensation arte-
facts, such as the ones observed with the TEOM and the high
sensitivity makes it particularly interesting for low emitting
engines and vehicles. Additionally, the instrument can
provide real-time mass weighted particle size information.
On the other hand, mass measurement is not conducted
directly but it is deduced based on two number weighted
distributions of different size expressions. A log– normal
distribution is assumed for airborne particles which accord-
ing to Harris and Maricq [129] is the most common case for
diesel exhaust; therefore nanometer nucleation particles
[15] may lead to interference to the mass measurement when
they appear. Because of its significant differences with the
established mass determination method, a comparative
measurement campaign needs to be conducted to obtain
information in the instrument’s operation characteristics and
performance, before any thorough evaluation can be
attempted.
5.7. Comparison of mass measurement techniques
The selection of an appropriate instrument with the
potential to replace or complement the standard gravi-
metric measurement is a complicated task and is mainly
a decision taken depending on the focus of each study.
There are mainly two quality criteria considered in such
a selection: first the quality of the technique as such,
following the criteria in Section 2.2 and, secondly, its
comparability with the standard gravimetric technique.
The preceded summary of the measurement techniques
showed that there are potentially several instruments
fulfilling the general quality requirements for repeatabil-
ity, high sensitivity and even robustness. However, as
long as the gravimetric method is considered the
‘accurate’ one, it will be difficult to establish an equally
precise method. This shortcoming mainly originates from
the complicated mechanisms governing the VF of the
exhaust PM, which becomes the dominant part for future
DPF equipped vehicles and engines. Volatile component
contribution is a function of sampling conditions and
665
filter material; it is not detected by optical techniques and
might not form particles in the airborne phase. If this is
the case, it might be impossible to develop a method
which will measure exactly the same quantity with the
established technique with increased sensitivity.
On the other hand, there are several interesting concepts
with the potential to provide particle exhaust mass
measurement for type approval of vehicles and engines,
assuming that the outstanding issue in such a case is
measurement repeatability. Such concepts may additionally
provide either high temporal resolution or on-line identifi-
cation of particle nature (volatile, solid, etc.). There have
been several studies on the evaluation of alternative
techniques [20,21,125] and it is not aim of this review to
rank relevant instrumentation.
In order to evaluate the quality of the measurement
with different instruments, Moosmüller et al. [95] studied
five different techniques sampling exhaust emissions from
three diesel vehicles from a CVS and compared results
with the reference method. The study involved compari-
son of a nephelometer (light scattering), an aethalometer
(light absorption), an opacity smokemeter (light extinc-
tion), a Photoacoustic sensor and the TEOM. With regard
to repeatability of measurement, all instruments showed
improved characteristics over the reference method with
only the Smokemeter exceeding it (Table 5), while no
data were reported for the aethalometer. The authors
assumed that either statistical errors are larger for the
reference method or that instruments do not record
changes in PM mass concentrations as well as the
reference method. Instrument noise when sampling
through a HEPA filter can occur due to interference
with other properties of the sampled exhaust (gas
composition, temperature, pressure fluctuations). The
nephelometer was by far the least sensitive to inter-
ference while TEOM gave most noisy results, which
were attributed to temperature and pressure fluctuations,
semivolatile species collection and vibrations. However, a
more than adequate signal-to-noise ratio was established
for all instruments.
With regard to their correlation with the reference
method, Table 5 also provides the correlation coefficient
squared, the slope ðAÞ and the offset ðBÞ for each
correlation. The best correlation with the CVS filter is
achieved by the TEOM, although the slope value (0.77)
shows some loss of VF. The nephelometer follows the
TEOM both with regard to the correlation to CVS and
the ability to record volatile material (slope 0.65). The
rest of the instruments show moderate R2 values, slopes
and offsets with the reference method, indicating that
their signal is rather correlated to, e.g. elemental carbon
than DPM. Although this work provides a good baseline
for comparison, it is more than evident that larger studies
need to be conducted before a new or alternative method
has been decided.
666 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672

Table 5
Repeatability of PM mass measurements with different mass determination techniques and correlation to the reference method [95]

Reference method TEOM Nephelometer Photoacoustic Sensor Smokemeter Aethalometer

(mg/m3) (mg/m3) (mg/m3) (km21) (km21) (mg/m3)

Vehicle 1 (Model Year 1999)

Weighted average 2.01 1.89 1.77 15.01 12.88 n/a
Standard deviation 0.17 0.09 0.13 0.49 1.2 n/a
Coefficient of variance 8.6 4.8 5.5 3.3 9.3 n/a
Vehicle 2 (Model Year 1996)
Weighted average 1.35 1.13 1.77 1.77 6.62 n/a
Standard deviation 0.25 0.15 0.23 0.39 1.13 n/a
Coefficient of variance 18.6 13 12.8 5.1 17.1 n/a
Vehicle 3 (Model Years 1988–1999)
Correlation to CVS ðR2 Þ 1 0.98 0.89 0.65 0.65 0.65
Response ¼ A £ CVS þ B
A 1 0.77 0.65 2.1 m2/g 1.7 m2/g 0.27
B 0 mg/m3 0.21 mg/m3 1.0 mg/m3 7.7 km21 6.7 km21 1.2 mg/m3

6. Cost of PM measurement facilities the above requirements can be met at much more reasonable
costs with the partial flow dilution systems.
Table 6 summarizes the different cost elements, which are The cost of an up-to-date weighing room fully equipped
relevant to PM measurement. The cost of partial flow systems with the required environmental controls for temperature,
ranges between 110 and 150 ke, i.e. about 20% of a full-flow humidity and dust is in the range of 50 ke. To this cost one
dilution system, complying with the Directive 1999/96/EC should add the cost of the microbalance, which is in the
and capable of measuring engines up to 500 kW. The range of 15 ke, at 0.1 mg sensitivity. The sum of 65 – 70 ke
comparison refers only to the parts of the full-flow dilution should be contrasted to the cost of the new Horiba MEXA-
and sampling system that can be replaced by a partial flow 1370PM which is currently in the range of 200 ke.
system (i.e. CVS, primary and secondary DTs and ancil- Nevertheless, one should note that this cost could be
laries). Clearly, the partial flow dilution systems constitute an reduced to half if the instrument gets into series production
excellent low-cost possibility for new emission test labora- (the method is still considered to be experimental). Also, the
tories, especially if space requirements are taken into account. instrument offers the simultaneous measurement of SOF,
It is difficult to assess the cost of the additional sulfate and insoluble fraction of particulates, which is
requirements of the US 2007 regulations, mainly due to tedious and time consuming with the conventional
the fact that it is yet unknown how the filter holder
Table 6
temperature will be controlled. Additional requirements
Summary of the main cost elements relevant to PM measurement
such as the recommended dilution air filtration with HEPA
filters, pre-classifiers, electronic controls, etc. are not Item Cost (ke)
expected to add substantially to the cost of a full-flow
dilution system. In particular as regards dilution air Full flow dilution tunnel
filtration, most laboratories already employ thorough (180 m3/min for engine size
filtration techniques. Assuming that the temperature control up to 500 kW)
at the filter holder will be realized via heating the sample Dilution tunnel 85
CVS system 400
hose and the filter holder, then it is estimated that the overall
Secondary dilution 85
cost increase will be in the range of 10 – 15% of a full-flow Ancillaries 30
dilution installation. If dilution air heating is selected to Total 600
control the sample temperature, then this may entail Partial flow dilution system 110 –150
significant costs. In order to give an order of magnitude Weighing chamber with environmental 50
estimate: Horiba produces a system for cleaning and heating controls (temperature, humidity and
the dilution air for light duty vehicles, which employs, in dust)
addition to the air heater, a CO catalyst, a NOx scrubber and Glove box 10
Microbalance (readability 0.1 mg) 15
activated carbon for HC. The cost of such a system for a
Horiba MEXA 1370PM 200
CVS of 22 m3/min (LDV application, dimensions 3 £ 3 £ 1, Mass recording instruments 50 –100
power 45 kW) is in the range of 300 ke. It is self-evident that
 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
techniques. Finally, long-term use of such an instrument
would offer substantial cuts in operational costs, as
apparently the process is extremely fast compared to the
conventional gravimetric techniques.
Finally, a survey of the costs of existing instruments for
real-time measurement of particulates indicated a large
price range (up to 100 ke).
7. Summary and concluding remarks
The review of DPM sampling and mass measurement
techniques shows that, in spite of the improvements
implemented during the last 20 years, precise measurements
still constitute a tedious task, competing with the reduction
in the absolute emission level. Today, application of
existing reference procedures seems inadequate to accu-
rately determine low PM emission concentrations of future
vehicles. To improve the quality of the measurement, three
main research areas have been identified:
† Introduction of technical and design improvements in the
existing full-flow sampling systems.
† Replacement of the full-flow systems with partial flow
ones which allow better control of sampling and
conditioning methods.
† Utilization of more sensitive techniques for mass
quantification, than the current gravimetric procedure.
Legislation and standardization authorities invested
significant resources to examine such alternatives. In
Europe, the relevant Directive for HDE emission sampling
has in principle adopted a number of possible configur-
ations. For steady state cycles these include raw exhaust
sampling for gaseous pollutants, partial flow sampling for
PM or full-flow dilution for both gaseous and PM emissions.
For transient cycles they include full-flow dilution for both
gaseous and PM emissions, accepting in parallel the PFSS if
its equivalency according to prescribed criteria is proven.
Still the majority of (if not all) type approvals granted on the
basis of this directive is based on measurements with full-
flow CVS, as no detailed specifications have existed for
PFSSs and raw exhaust measurements. The more recent
Directive 2001/27/EC [130] (complementing Directive
1999/96/EC) has adopted the technical prescriptions of
ISO 16183 only for NOx emission measurements during the
ETC screening test, as an alternative to the requirements of
the fundamental Directive 88/77/EC.
In the United States, EPA adopted new regulations for
PM measurement for the 2007 emission standards. These
regulations concentrate on improvements of the full-flow
technique without yet approving PFSS for certification tests.
Together with several sample treatment and conditioning
improvements, the most significant refinement appears to be
the introduction of a narrow temperature range (42– 52 8C)
for the PM sampling position throughout the measurement
667
test (as opposed to today’s , 52 8C temperature limit). This
aims at more accurately controlling the VF of the PM, which
is especially important in view of the increased probability
that DPFs are widely used for compliance with future
emission standards.
On the other hand, objective of the new ISO 16183
standard was to develop the necessary specifications which
would allow the measurement of gaseous and particulate
pollutants using PFSS under transient test conditions.
Correlation studies were undertaken to unveil the relation-
ship between the conventional CVS technique and partial
flow dilution. Data from most of these correlation studies
indicated that PFSS are sufficiently developed and thus able
to keep the necessary proportionality of exhaust mass
flowrate and sampled mass into the PFFS, i.e. a constant
split ratio over the transient operation conditions. As regards
PM emissions an agreement in the range of ^ 10% was
established between full and partial sampling method in the
framework of WHDC GRPE activity. Recent improvements
of sampling probe and mini DT led to minimization of this
variability to less than 5%. On the other hand, it shall be
noted that an EPA/EMA/CARB study resulted in a less
satisfying correlation between CVS and PFSS. Although the
potential for PFSS as a substitute to the full-flow systems
was reported, the need for further work to improve the
robustness of the method was underlined in the study. Based
on this evidence and the decreasing emission levels, PFSS
should be regarded as strong candidates for future
regulations.
With respect to alternative and more sensitive mass
determination techniques compared to filter based gravi-
metric method, a number of different concepts are under
development and examination. Several techniques present
advantageous characteristics (repeatability and sensitivity)
but poor correlation with the reference method. Techniques
based on filter heating and gas analysis seem to be promising
but further work is needed to obtain correlation data to the
reference method. Optical methods applied on real-time
measurements gave reliable results for PM insoluble
fraction but present inherent difficulties in the estimation
of SOF. Fast FIDs seem to be able to perform reliable real-
time measurement even over transients, but the amount of
work conducted is not sufficient (especially in the absence of
round robin tests) to draw final conclusions concerning their
reproducibility and accuracy.
TEOM and QCM seem to be promising real-time
instruments, because they allow direct mass measurement.
In particular, improvements in the output signals, sample
flowrates, and operation temperatures increased the poten-
tial of the TEOM application. However, the behavior of the
VF when sampling with these techniques is again a source of
uncertainty. Further improvements will be probably
required to eliminate these problems which currently raise
doubts about the usability of such instruments for future low
mass emission engines (i.e. Euro 4 and beyond).
668 E. Vouitsis et al. / Progress in Energy and Combustion Science 29 (2003) 635–672
The performance of the DMM instrument needs also to be
examined.
The combination of techniques, i.e. the application of
any soot measuring device (e.g. an optical technique)
together with an FID or a multiple wavelength method
might also provide a potential solution for the compensation
of organics. However, combination of techniques will
require calibration to a reference method and can always
be questionable.
With regard to the cost of the sampling and dilution
systems the following can be concluded:
(i) The cost of partial flow systems ranges between 110
and 150 ke, i.e. about 20% of a full-flow dilution
system, capable of measuring engines up to 500 kW.
Hence, partial flow dilution systems would provide an
excellent cost-effective possibility for new emission
test laboratories.
(ii) The additional requirements of the US regulations
with regard to CVS will increase both the installation
and operating cost of the full-flow system. It is
estimated that this cost increase will be in the range of
10 – 20% of an existing installation, assuming that the
temperature control at the filter holder will be realized
via heating the sample hose and the filter holder.
(iii) The cost of more sensitive mass determination
techniques are in the range of 50 – 200 ke (the
maximum value corresponding to Horiba’s MEXA-
1370PM which additionally offers VF separation).
This should be compared to the cost of an up-to-date
conditioning room and a microbalance with 0.1 mg
readability (65– 70 ke).
Acknowledgements
The authors gratefully acknowledge the financial support
to this work of the European Commission, Enterprise
Directorate General, in the framework of the study contract
No Etd/00/503430. Special thanks go to Dr Paul Greening
(European Commission) and Dr Claire Holman (Peter Brett
Associates, UK) for their valuable remarks and comments.
Finally, we would like to express our sincere appreciation to
Mr Jürgen Stein (DaimlerChrysler Powersystems,
Germany) for his thorough review of our report. Finally,
we are thankful to the anonymous referee for his in depth
review of the manuscript with many detailed comments
which we believe substantially improve its overall quality.
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