tmpCDF7 TMP

Downloaded from SAE International by Barouch Giechaskiel, Wednesday, October 01, 2014
2014-01-2834
Published 10/13/2014
Copyright 2014 SAE International
doi:10.4271/2014-01-2834
saefuel.saejournals.org
Engine Exhaust Solid Sub-23 nm Particles: I. Literature Survey

Barouch Giechaskiel, Urbano Manfredi, and Giorgio Martini
Joint Research Centre
ABSTRACT
In the current diesel vehicle exhaust emissions legislation Particle Number (PN) limits for solid particles >23 nm are
prescribed. The legislation was extended to include Gasoline Direct Injection (G-DI) vehicles since September 2014.
Target of this paper was to investigate whether smaller than 23 nm solid particles are emitted from engines in considerable
concentration focusing on G-DI engines. The literature survey and the experimental investigation of >15 vehicles showed
that engines emit solid sub-23 nm particles. The average percentage over a test cycle for G-DIs (30-40%) is similar to
diesel engines. These percentages are relatively low considering the emission limit levels (61011 p/km) and the
repeatability (10-20%) of the particle number method. These percentages are slightly higher compared to the percentages
expected theoretically not to be counted due to the 23 nm cut-off size (5-15%). Higher fraction can be measured with high
ethanol content fuels, at sub-zero ambient temperatures and when additives are added in the fuel or lubricant. Based on
the information today, the PN legislation should remain the same. However measurements of particles <23 nm should go
on in order to monitor the sub-23 nm fraction of current and future engine technologies.
CITATION: Giechaskiel, B., Manfredi, U., and Martini, G., "Engine Exhaust Solid Sub-23 nm Particles: I. Literature Survey,"
SAE Int. J. Fuels Lubr. 7(3):2014, doi:10.4271/2014-01-2834.
INTRODUCTION
Figure 1 gives a simplified overview of the processes from the
combustion in the cylinder of the engine until the sampling
point at the full dilution tunnel (CVS). In the combustion
chamber primary soot particles (spherules, around 20 nm) form
via the pyrolysis of fuel (and lubricant) molecules when there is
not sufficient oxygen for complete oxidation. In this stage fuel
(and lubricant) molecules can completely escape combustion
and/or be partly modified; however at this stage they remain in
the gas phase. The primary particles agglomerate and most of
them are oxidized at the high temperatures in the cylinder. As
the piston moves downward, the system cools rapidly. At this
stage if there are other non-volatile species (like metals) with
very high concentrations, they will deposit on the carbon
particles or may alternatively self-nucleate.
In the exhaust tailpipe and the transfer tube from the vehicle to
the full dilution tunnel the exhaust gas temperature is still high
and usually agglomeration goes on. Agglomerates have an
impure form of near-elemental carbon with a graphite-like
structure. Also previously stored material on transfer tube
walls can be released. Semi-volatiles such as Polycyclic
Aromatic Hydrocarbons (PAHs) can condense on particles.
In the full dilution tunnel the exhaust gas is mixed with room air
dilution air. Some volatile material (from unburned fuel and/or
lubricant) condenses on the agglomerates and/or creates
nucleation mode particles (droplets). Thus at the end of the

dilution tunnel there is a tri-modal number distribution (see
upper right panel of Figure 1) [66]:

The nucleation mode, which contains mainly volatile

droplets, but solid cores1 can also exist.
The accumulation mode, which consists mainly of the

agglomerates (soot) and the condensed on them volatile
material.
The coarse mode, which consist of deposited particles

that reenter in the full dilution tunnel.
Most particles, by mass, reside in the accumulation mode,

while by number sometimes the nucleation mode can dominate
[66]. During mixing in the dilution tunnel semi-volatile gaseous
species, organics and sulfates partition to the aerosol phase,
depending on the local temperature and species
concentrations, both of which are a function of dilution ratio
(ratio of air to exhaust gas). This partitioning occurs in the form
of adsorption and condensation onto existing soot
agglomerates or as nucleation of separate particles (droplets),
usually between 10-30 nm in diameter. Extensive condensation
can change the structure of the agglomerates [148, 122].
Whether a separate nucleation mode forms, as well as its
magnitude, depends on a number of factors. These include the
engine characteristics, the aftertreatment devices utilized [50,
9, 68, 69, 144, 40], the pre-conditioning and history of the test
1. The term core mode is used for a separate solid size distribution with peak
<23 nm to avoid confusion with the nucleation mode which is typically volatile.
Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

[41, 139], the fuel and the lubricant used [67, 70], the sampling
conditions [62, 64, 103], adsorption phenomena along the
sampling lines [95], and the amount of soot present, since this
promotes the competing process of condensation and
adsorption instead of nucleation [63, 64, 146]. In order to avoid
the variability of the volatile nucleation mode, the European
legislation introduced a particle number (PN) method based on
the thermal pretreatment of the aerosol and the measurement
of the accumulation mode only (agglomerates).
Figure 1. Typical sequence of particle transformation from the engine

to the measurement location (from [36]).
Particle Number (PN) Method

The PN method is based on the findings of the Particle
Measurement Program (PMP) [3, 37]. When the exhaust gas
enters the volatile particle remover (VPR) of the PN system it is
diluted with filtered air at temperature >150C, then heated up
to 300-400C and most volatiles and semi-volatiles evaporate
and the particle number distribution is affected (see Figure 1).
Thus at the exit of the VPR only non-volatile particles should
remain. In this paper, particles after thermal pre-treatment at
approximately 350C are called solid.
The particle number counter (PNC) of the PN system
measures particles >23 nm2; this means that the particle
number system measures only the accumulation mode and
(depending on whether there is a cyclone or not) the coarse
mode. The coarse mode in terms of number doesn't contribute
much. Note also that even if the volatiles from the
accumulation mode are not completely evaporated the total
number concentration is not affected. If the nucleation mode is
not completely evaporated, there will be an effect on the
number concentration. The 23 nm cut-off size of the PNC
ensures that this effect will be small. Note however, that if there
is a solid core mode <23 nm, this will not be counted.
2. Actually the PNC has a counting efficiency of 50%12% for particles of 23 nm
and >90% for 41 nm. The 50% cut-point is called cut-off size d50%.
The PN standard was introduced for Diesel Light Duty vehicles

in September 2011 (Euro 5b) limiting the number of solid
particles emitted over the NEDC to 61011 p/km. The new
standard effectively necessitated the installation of highefficient wall-flow DPFs in all diesel vehicles. The same
standard was introduced to gasoline vehicles utilizing direct
injection (G-DIs) at Euro 6 stage (September 2014) initially with
a limit of 61012 p/km and from September 2017 with 61011 p/
km. This 3 year delay was decided in order to allow the
manufacturers sufficient time to investigate the possibility of
compliance through improvements in the combustion process
without the need of Gasoline Particulate Filer (GPF). The PN
standard has also been introduced for heavy-duty engines
since the beginning of 2014 (Euro VI). Particle number limits
will also be introduced for most categories of Non-Road Mobile
Machinery (NRMM) engines in the near future.
Note that it is important to distinguish solid particles < 23 nm
that are part of the lognormal soot accumulation mode from a
separate small solid core particle mode. Sub-23 nm
accumulation mode particles are already regulated with the
current 23 nm cut-off size, at least to an extent, even if they are
not explicitly counted. For example for typical size distributions
with means around 50-70 nm, approximately 5-15% of the total
particles are not counted. However, one could theoretically
manipulate the size distribution to lower sizes and thus avoid
part of the emitted particles to be measured (e.g. with a mean
of 30 nm, 40% of the particles are not counted). Lowering the
cut-off size ensures that most of the particles will be measured
and is necessary when a separate core mode exists. However,
at the same time the measurement uncertainty due to different
losses in the commercial PN systems can increase.
Objectives
Target of this report is to investigate whether it is necessary to
measure <23 nm particles (i.e. to change the current
legislation). In other words it will be investigated whether
smaller than 23 nm solid particles are emitted by engines in
considerable concentration focusing on Gasoline Direct
Injection (G-DI) engines. High sub-23 nm fraction could exist
either because the mean size is lower than from diesel vehicles
or because there is a separate solid core mode. Initially the
health effects of sub-23 nm particles will be examined. Then
the typical solid emissions of vehicles will be investigated
based on the literature and experimental tests.
HEALTH EFFECTS OF VEHICLE EXHAUST

PARTICLES
Initially a short overview of the adverse health effects of small
particles will be given. Target is to see whether sub-23 nm
particles are more harmful than the >23 nm particles and
whether the nature (physical and chemical composition) is also
important.
The residence time of particles in the atmosphere depends
mainly on their size. Owing to the effect of gravity, coarse
particles are rapidly removed from the air by sedimentation

(residence time between some minutes and some hours); also,
particles in the nucleation mode are transformed into coarser
particles by coagulation processes. The highest residence time
in the atmosphere (up to some weeks) is shown by particles in
the accumulation mode, which can be easily transported by the
wind up to thousands of kilometers from the area where they
are formed. Thus, due to their lower residence time in the
atmosphere, the sub-23 nm particles should have fewer
possibilities to be inhaled. However, it should be kept in mind
that in cities people are close to cars and the diluted exhaust
gas can reach them in a few seconds/minutes.
Particulates are considered to have a negative impact on the
human health. Epidemiological (e.g. [125]) and toxicological
studies (e.g. [120]) have associated urban air quality and air
pollution, and specifically particulate matter, with adverse
health effects. Vehicle exhaust particles have long been
considered a significant source of anthropogenically generated
particles. In the most extensive and current review of the
literature [26], it was concluded that adverse health effects are
still best linked to exposure to Particulate Matter (PM) below
2.5 m. However, pioneering studies [119, 22] suggested that
the inflammatory response to particles from non-toxic materials
correlates better with the particle surface area rather than the
mass. Thus it is assumed that nanoparticles are more harmful
than bigger particles because they will have larger surface area
(for the same mass). A number of health effect studies
suggested that ultrafine particles, particles whose diameter is
<100 nm, might be more hazardous than fine particles [28, 93,
134, 130] but maybe this is not true for all materials [60]. Two
are the main reasons for the possibly higher danger of smaller
particles: Higher deposition fraction of smaller particles and
higher surface area in contact with the human cells (for the
same mass).
The three main regions of the respiratory tract are: 1) the
extrathoracic region that consists of the oro- and nasopharyngeal region and the larynx; (2) the tracheobronchial
region, the system of the conductive airways; and 3) the
pulmonary region that contains the fully alveolated alveolar
sacs and different types of alveolated airways. Hence, the lung
consists of the tracheobronchial and the pulmonary regions.
The deposition fraction, defined with respect to the inhaled total
particle number concentration, is shown in Figure 2 as a
function of particle diameter [1]. The deposition fractions in the
three characteristic regions of the respiratory tract are
presented separately. The deposition location of an inhaled
particle is a sensitive function of its diameter since diffusion is
the main deposition mechanism, inertial impaction contributing
as well, for particles in the size range of emitted diesel-exhaust
distributions. The deposition fraction in the extrathoracic and
tracheobronchial region is lower for the accumulation mode
(particle size around 50-100 nm) but increases for smaller
particles. In the pulmonary region the deposition efficiency
curve has a maximum around 30 nm and decreases for smaller
sizes. Generally the total deposition increases with decreasing
size in the size region emitted by vehicles (particles <600 nm).
The deposition location of an inhaled particle is a determining

factor in assessing its health effect. Cancers in mouth, larynx,
trachea, bronchus and other regions of the lung can be traced
to exposure to particles. In the bronchial and bronchiolar
airway generations mucociliary clearance eliminates a
significant fraction of deposited particles within 24 hours [54].
In deeper lung regions the majority of deposited particles
remain long enough to interact with lung fluid and epithelial
cells. During this interaction mutagen and carcinogen agents
such as oxidative radicals are generated [10, 58, 120].
Inflammatory [132], allergic immune response [123, 133], or
cardiovascular consequences [21] have also been reported.
Figure 2. Calculated deposition fraction of inhaled particles as a

function of particle diameter for the three region of the human
respiratory system: extrathoracic, tracheobronchial, and pulmonary.
From [1].
Some authors suggest that the soot is the component that

stimulates the most adverse reaction [31, 87, 112]. Many
studies have concluded that the toxicity response of PM
primarily depends on its chemical composition (e.g. organics)
[14, 15, 42, 81, 114, 151]. Transition metals (like iron, copper,
vanadium and zinc) and metal oxides [55] also contribute to
the oxidative stress resulting from exposure to PM [32] and
maybe even more than soot [130]. The high surface activity of
metals, which are used in emission control catalysts, seem to
increase their adverse health effects [20]. Moreover, these
insoluble nanoparticles can transport other surface adhered
toxic substances, a phenomenon that is described as the
Trojan horse effect [85].
It should also be added that the concept of translocation
proposes that inhaled solid nanoparticles pass through the
lungs' alveolar membrane and go via the blood to the heart and
other organs where they exert a directly toxic effect [121]. They
can cross the blood-brain barrier and can also cross the
placenta and enter into the fetus. This doesn't apply for volatile
nanoparticles which will dissolve in lipid and aqueous bodily
fluids.
Conclusions
From the available studies the main conclusions are:

Total mass still correlates best with adverse health effects,

but other metrics like surface area (for the same mass)
might be proven more important in the future.

Both soluble and insoluble fractions have been identified

as potential contributors. Metal oxides were also identified
as potential contributors to adverse health effects.
The size of particles determines the deposition location

and deposition fraction. Generally, it increases with
decreasing size in the range of particle sizes emitted by
vehicles.
Thus in the presence of excessive sub-23 nm solid

particle fractions, the regulated procedure might fail to
quantify the number concentration of potentially harmful
(i.e. owing to their chemical nature) particles.
Next chapters will focus on the concentration of vehicle

emitted solid sub-23 nm particles and their nature, since
volatile particles are out of the European regulation scope
at the moment.
LITERATURE SURVEY ON SOLID PARTICLE

EMISSIONS FROM VEHICLES
In this chapter it will be examined whether the 23 nm cut-off
size makes sense based on studies of primary particles formed
inside the combustion chamber, typical vehicle size
distributions and specific studies of solid sub-23 nm particles.
Primary Particles
The cut-off size of the PNC was chosen to be 23 nm in order to
include the primary soot particles and at the same time avoid
any artifact from volatile nucleation mode particles, which, if
they still exist after thermal pretreatment, are <20 nm. This
section will examine the first assumption i.e. the size of primary
particles for different engine categories.
Several studies have investigated the morphology of soot
particles from combustion processes using Transmission
Electron Microscopy (TEM). Diesel engine soot is composed of
agglomerated carbonaceous primary particles [8, 136, 72, 124,
108]. The soot particle nanostructure is highly dependent on
conditions such as temperature, time, and fuel properties [147].
The diameter of primary soot particles determined by TEM
analysis has been reported to be 23 nm for diesel soot in a
smog chamber [149]. In [75] the primary particle size ranged
from 16 to 28 nm. The primary soot particle diameter ranged
from 19 to 33 nm for a light-duty engine and from 28 to 35 nm
for a heavy-duty engine [77, 78, 80]. Similar results were found
in [102] with sizes ranging from 18 to 32 nm and in [113] with
sizes between 20 and 35 nm. For diesel engines solid sub-23
nm particles can be found when additives are added [76].
Regarding G-DI engines, primary particles from 16 nm to 23
nm were found in [30] and from 10 to 30 nm in [126]. In [101]
an image of a nanoparticle agglomerate with about 27 nm
primary particle was shown. In [7] it was shown that primary
particles were distributed in a range of 7 to 60 nm in diameter,
which is somewhat wider than the size range of diesel
particulates. In [79], for early fuel injection strategy, liquid

droplets were prevalent, and the primary particle diameter was
between 20 and 25 nm with graphitic structure. For a fuel
injection strategy which produced low particle number
concentration there were many single solid sub-25 nm particles
and fractal like agglomerates with primary particle size
between 10 and 15 nm with more amorphous structure. In
[101] it was observed that the 20 nm particles of a G-DI vehicle
evaporated within 60 s of exposure to the electron beam.
Conclusions
The mean value of the primary particles is around 25 nm for
both diesel and G-DI engines. However the following points
should be considered for G-DIs: The distribution of particles
and primary particles can be wider, so larger percentage of
particles can exist <23 nm. The structure of primary particles is
sometimes different (more amorphous) and more unburned
hydrocarbons or volatile organics can be found. This means
that differences in the thermal pre-treatment (temperature,
residence time of the PN systems) might lead to different
results. High concentration of smaller than 23 nm solid
particles could also exist from fuel or lubricant additives as with
diesel engines.
Typical Size Distributions

Typical PN size distributions of various engine technologies
were summarized in [38]. The results were based on more than
15 light-duty diesel vehicles without DPF, 5 with DPF, 10 G-DI
vehicles and 30 G-PFI vehicles [35, 44, 46, 61, 88, 89, 96, 98,
100, 109, 110, 111, 115, 117, 126, 143]. The HD results were
based on more than 20 engines without DPF and 5 with DPF
[4, 35, 39, 46, 142, 145]. The standard deviations were derived
from approximately the 1/3 of the vehicles for which there was
information in the texts. The size distributions had count
median diameters in the range of 50-75 nm (light-duty) and
60-85 nm (heavy-duty) with standard deviations around
1.8-1.9, with no separate core modes <23 nm.
Conclusions
The PMP legislation was based on typical engine exhaust size
distributions with means of 50-85 nm and standard deviations
of 1.8-1.9. It was also observed that DPFs trap almost equally
all particle sizes.
Solid <23 nm Particles Studies

Although it was believed that there were no solid particles <23
nm (except when additives were present), the last years many
studies showed that this is not the case. Table A1 in the
Appendix summarizes the studies that have investigated solid
particles <23 nm. Only the studies with thermal pre-treatment
and those that measured both >23 nm and <23 nm solid
particles were considered. Some studies with lower
temperatures than 250C were included in grey. Studies
without any thermal pre-treatment that typically favor the
volatile nucleation mode formation were not considered at all. It

should be also mentioned that many of these studies that
found a soot-like solid nucleation were conducted with
thermodenuders which have been found to form artifacts at
small particle sizes [138]. It should be also noted that in many
studies it was recognized that the solid nucleation mode [57,
150] was actually volatile, thus an artifact of the PMP method
and the dilution factors employed (e.g. [91, 153]). This will be
topic of a separate publication. Focusing on the studies that
found solid sub-23 nm particles, and were considered reliable,
the following conclusions can be drawn. In brackets the
number of engines or vehicles that were found with sub-23 nm
solid particle fraction.
Diesel (41 Engines and Vehicles)

A solid core mode has been measured with older and modern
diesel engines without exhaust aftertreatment [68, 128] or with
low particle collection efficiency filters [49] and/or DOCs [19,
73, 74]. It appears mostly at idle and low loads [19, 106] but
even at high [73]. It becomes more prominent when the EGR is
forced low. The solid core mode increases along with NO and
overall NOx emissions, in contrast with the accumulation mode
[74]. The solid core could consist of soot, metal oxides or low
volatility organic compounds [68, 71, 128, 131]. The nature of
these particles will be discussed below.
Low Volatility Components
Chemical analysis of nucleation mode particles of a heavy-duty
engine showed that although organic carbon was the primary
component (79%) elemental carbon (8%), elements (4%) and
ions (9%) existed as well [29]. The authors also found that
lubricating oil was the primary component of the nuclei
particles. Recently it was also measured high concentration of
sub-23 nm oil particles (20-30% of total) during deceleration
and engine braking [129].
Metal Oxides (Lubricant)
Elements such as S, Ca, Zn and P have been found in high
concentrations in diesel nanoparticles <30 nm [29]. These
elements are used as antioxidants (e.g. ZnDTP) and detergentdispersants (e.g. CaCO3). The assumption is that metal
particles from the lubricant are partially vaporized during
combustion and nucleate. Emissions can reach 1 mg/km (or 1
mg/kWh) [106]. High solid nucleation mode is found when the
soot mode is low and at idle. The lube oil consumption is high
in this case because the engine blow-by gas flow from cylinder
to oil sump, which usually pushes back the lubrication film, is
weak. Thus more lubrication oil intrudes in the combustion
[106]. Metals from the coatings of catalytic converters and
particulate filters (e.g. Pt, Va) are assumed to be low (ng/km)
and in the m range. Similarly for abrasion metals (e.g. Fe, Cr,
Ni, Cu, Pb) from piston rings, valves and bearings. They will
probably be washed away by the oil film and may end up in the
lubrication oil sump or oil filter, however it cannot be excluded
that they can re-entrain in the combustion chamber and thus
be vaporized and form solid nucleation mode particles [106].
Metal Oxides (Fuel)

Fuel additives (fuel borne catalysts, like Fe and Ce) can also
result in a solid core mode [59]. Additives are added in small
concentrations to promote regeneration in DPFs. At low
concentrations no solid core peak is observed [11, 137]. The
additives are deposited on larger soot particles to catalyze the
soot combustion. Overdosing the additives (fuel born catalyst)
results in a separate solid core mode peak [106] due to
self-nucleation and reduced soot surface for condensation [84].
Additives that are used for the regeneration of DPFs are
typically captured in the DPF and don't escape in the
environment. However, sometimes they can escape filtration
[83].
Soot
Another assumption is that the solid core mode consists of
soot-like particles. In light-duty diesel TEM images were
unsuccessful and only by defocusing the TEM could faint
roughly 10 nm smudges be seen [19]. The explanation was
that these solid nucleis were amorphous and couldn't be
distinguished from the carbon substrate. The lack of a clear
TEM image, their low volatility and the charge distribution ruled
out that these particles derived from ash or sulfate and
suggested rather that they had composition similar to the
incipient soot mode observed at <10 nm in rich flames [135,
94], or derived from heavy hydrocarbons that nucleated
already in the engine cylinder [19, 73]. How the two solid
particle modes (core and accumulation) can originate during
diesel combustion is currently not known. Possibly the multiple
fuel injection pulses per engine cycle used in new engine
technology diesel engines to control soot formation and noise
can produce separate particle populations [19].
An important finding from many studies is that DPFs remove
the solid nucleis with an efficiency comparable or higher than
accumulation mode particles [45]. However, regeneration can
also result in increased emissions of sub-23 nm solid particles
[13]. It is suggested that they originate from the fragmentation
of the soot cake of the DPF. However, they could also be metal
oxide particles previously adhered to soot particles [106].
G-PFI (8 Vehicles)
Solid nucleation mode is often observed in Gasoline Port Fuel
Injection (G_PFI) engines and it is assumed to originate from
the metals of the lube oil [106]. Big differences can be found
between old and new engines. A solid core mode has been
observed when fuel additives were used [33]. The fuel
additives were Mn, Fe and Pb in concentrations up to 18 ppm
and very high metal oxide emissions at a size of 10 nm were
measured. This case is still realistic in some countries.
G-DI (12 Engines and Vehicles)

A shoulder at 20 nm appears quite often at G-DIs [56, 140]. A
separate solid nucleation mode is not typical, but the size
distribution can peak at small sizes (20 nm or lower) in some
engine operation modes [99, 48] with EGR and high speed.

Fuel with 85% ethanol has also been shown to result in small
particle sizes [140]. A relative increase in species associated
with the lubricating oil (calcium, phosphate, zinc, etc.) is
observed as fuel ethanol content increases. This does not
indicate that more oil-associated species are being emitted;
just that these are proportionately increased in the particle
mass spectra as products of incomplete combustion are
reduced [23].
2-Wheelers (9 Mopeds and Motorcycles)

Very often the mopeds (2-stroke) size distribution after thermal
pre-treatment peaks at or below 20 nm [105, 18]. Although in
some cases it can be a sampling artifact [35], probably they are
particles remaining from the lube oil. The 2-stroke engines are
lubricated by adding 2% of lubrication oil to the fuel. The
specific fuel consumption is also high. Thus the metal oxide
emissions are typically much higher than the 4-stroke engines.
With a 2% lubricant addition in the fuel more than 2000 ppm of
metals are added. Metal free lubrication oils reduce the
emissions. Low levels of black carbon have also been
measured suggesting also soot nucleis [35].
Conclusions
Recent studies, in contrast to older studies, showed that there
are solid particles <23 nm in significant concentrations in some
engine operation modes. These particles are considered to be
either metals from the lubricant, additives in the fuel or soot
particles (heavy molecular hydrocarbons) formed in the
combustion chamber. Thus cases with fuel or lubricant (metal)
additives or high lubricant consumption need special attention.
However these solid sub-23 nm particles are not a unique
characteristic of G-DI engines but they appear very often at
diesel engines as well.
EXPERIMENTAL INVESTIGATION ON SOLID

PARTICLE EMISSIONS FROM VEHICLES
Older Study
The Joint Research Center (JRC) in Ispra, Italy did a
preliminary investigation in 2011 [89, 90, 91, 92]. The vehicle
sample consisted of a conventional Euro 5 compliant Port Fuel
Injection (PFI) vehicle, a Euro 5 DPF-equipped diesel, a Euro 6
DPF-equipped diesel, a Euro 5 Flexi Fuel Ethanol Gasoline
Direct Injection (G-DI) running on 5% and 85% ethanol/
gasoline blends, a Euro 5 G-DI with and without a wall flow
particulate filter (GPF), a Euro 4 Bi-Fuel PFI vehicle running on
gasoline or on either CNG or CNG/H2 mixtures up to 70/30%
and a Euro 4 certified vehicle with twin-injector system that
allowed for fuel injection on both the intake port and inside
each cylinder (GDI_PFI). The vehicles were tested over the
legislated New European Driving Cycle (NEDC) at ambient and
sub-zero test cell temperature as well as over the Common
Artemis Driving Cycle (CADC). The emissions were measured
according to the PMP method and in addition with a PNC
(d50%=5 nm) measuring downstream of the VPR (Figure 3).
Figure 3. Sub-23 nm particles in function of the solid >23 nm PN

emissions (various cycles). From [89, 90, 91, 92].
The two Euro 5 G-DI vehicles had emission levels under the
legislated procedure exceeding the diesel limit by 4 to 6 times.
The use of 85% ethanol in the fuel resulted in a 70% reduction
of the number concentrations over the NEDC, where the
emissions averaged at 81011 p/km. The data collected with
the low d50% PNC suggested that the fraction of undetected
sub-23 nm particles was lower than 30% under most driving
conditions. Concerns for volatile artifact were raised for higher
fractions, as they depended on the dilution factor employed
[92]. No clear trend was observed regarding the sub-23 nm
fraction at lower ambient temperatures or higher ethanol
content fuel.
The use of a wall flow particulate filter, optimized for G-DI
applications, was found to effectively reduce the regulated
particle number emissions bellow the diesel threshold of 61011
p/km and at the same time effectively remove sub-23 nm
particles. The GDI_PFI had lower emissions than the G-DIs
when the engine was hot. The sub-23 nm fraction was similar
with the rest G-DIs.
The emissions from the G-PFI vehicles were found to be
systematically below the diesel limit even when employing the
5 nm PNC. Most of the particles were emitted during short
periods of sharp accelerations. Particle formation was
enhanced under cold start operation with the emissions over
the urban part of the cycle being up to 20 times higher of those
during the extra-urban part. The particles >5 nm were around
50% higher compared to the >23 nm particles over the NEDC.
The use of CNG and CNG/H2 mixtures on the Bi-Fuel vehicle
resulted in an order of magnitude reduction in the particle
number emissions, which averaged at 2.21010 p/km over the
NEDC. In this case, almost all particles were emitted during a
sharp spike occurring over the first 50 s of the urban part; then
they remained at near background levels. Sub-23 nm fraction
was >100%. This might point towards the presence of a distinct

core mode of nonvolatile nature peaking at a size bellow 23
nm. It needs to be emphasized though, that the emission levels
were very low, with the maximum number emission >5 nm over
the NEDC being 91010 p/km.
The DPF-equipped diesel vehicles tested were found to comply
with the Euro 5 limit. The actual emission levels strongly
depended on the fill status of the DPF. The sub-23 nm
contribution of nano-particles was found to be around 50%.
Tests at an ambient temperature of 7C only slightly
increased the sub-23 nm fraction but in one case they
increased the absolute emission levels above the Euro 5b limit.
The much higher sub-23 nm fraction at lower emission levels
was attributed to volatile artifact (re-formation of particles
downstream of the evaporation tube in the PN systems) [91].
Newer Study
During the last months of 2013 the existence of solid sub-23
nm particles was investigated again at the JRC. All G-DIs were
Euro 5 certified. Two DPF equipped vehicles were Euro 5 and
another was Euro 6 with SCR system. A moped (2-stroke) was
also tested. A PNC (d50%=3 nm) was connected in parallel with
a PNC (d50%=23 nm) in a PMP system [36] connected to the
CVS. The Particle number Concentration Reduction Factor
(PCRF) was always 1000 (10010) for all vehicles examined.
The results of WLTCs can be seen in Figure 4. WLTCs were
chosen as more representative of future and real world
emissions. Nevertheless, NEDCs had similar results (not
shown). The following conclusions were drawn:

The emission levels of the DPF vehicles for the WLTC

spanned from very low emissions close to the background
of the PN method (2109 p/km) to 5 times the legislation
limit. The fraction of particles not counted by the legislative
method was typically <30% for levels >1011 p/km.
The percentage was >100% for emission levels close

to the background and when the soot concentration
was low (favoring the volatile re-nucleation artifact). In
addition, the specific PNC >3 nm that was used has an
internal averaging at low concentrations which led to
overestimation of the emissions.
G-DIs emissions ranged from 61011 p/km to 61012 p/km.

G-DIs had 30-40% solid sub-23 nm particles.
Low ambient temperatures (7C) increased this

percentage and the absolute levels for the G-DI vehicles.
The emissions increased 3 times from 1-21012 p/km to
4-61012 p/km and the percentage of sub-23 nm particles
increased from 30-40% to 60-100%.
High ethanol content (E85 vs E5) resulted in significant

decrease of the emissions to levels close to the Euro 5b
diesel limit. The sub-23 nm particles fraction was around
30-70%.
It should be also noted that the losses in the VPR in

the 10 nm range can be more than 50%, thus the real
concentration of solid sub-23 nm particles could be 2
times higher.
Figure 4. Sub-23 nm particles in function of the solid >23 nm PN

emissions (WLTC). The Euro 5b limit refers to the NEDC type approval
cycle.
Figure 5 gives some examples of size distributions. These

were measured with an Engine Exhaust Particle Sizer (EEPS)
from TSI connected to a PMP system connected to the tailpipe.
The PCRF was 1515.
Figure 5. Examples of size distributions measured with G-DI and DPF

vehicles. EEPS was measuring downstream of a VPR connected to the
tailpipe. Size distributions were not corrected for losses in the VPR
(only multiplied by the PCRF).
Size distribution measurements showed sometimes a

solid core mode peaking approximately at 10 nm, usually
as a small shoulder, and rarely as a separate nucleation
mode. It should be mentioned that this core mode could
be a result of the not accurate algorithm of the EEPS to
convert current to number concentration for agglomerates
(EEPS is based on electrical charge of particles and not
on optical detection like the PNCs). This could also be the
reason of wider size distribution for G-DI vehicles.
In general the fraction of sub-23 nm particles estimated

by the EEPS measuring at the tailpipe, was in agreement
with the PNCs' ratio (>3nm to >23 nm) from the CVS.
Size distribution measurements during the regeneration

and after the regeneration from one vehicle revealed that

there were no significant increase of solid particles <23
nm. One case with high emissions during regeneration
was due to re-nucleation after the evaporation tube (see
Figure 4).

Tests with mopeds also revealed that volatiles can be

measured as solids (<23 nm) (see Figure 4). It should be
mentioned that the solid size distribution peaked at 20 nm
and the PMP method could detect only a small fraction of
the total solid particles.
particles escaping detection with the PNC at 23 nm was

>100%. However, in this case the absolute emissions with the
low cut-point PNC were still well below the Euro 5b diesel limit
of 61011 p/km. The sub-23 nm fraction of G-DIs was 30-40%,
but higher fraction sometimes was measured either due to
re-nucleation of volatiles inside the PN system or at lower
ambient temperatures or at higher ethanol content fuel. In
general, no separate solid core mode was observed for most
vehicles.
These tests didn't include heavy-duty engines, which, based on

the previous literature survey, were shown to form solid core
mode very often. This needs to be further investigated.
Real Time Signals

Some more insight on the sub-23 nm particle emissions can be
gained by looking at the real time signals of the EEPS and the
PNCs. Figure 6a shows the real time patterns at CVS with the
>23 nm and >3 nm PNCs for one specific test with one G-DI.
Figure 6b shows the real time pattern of an EEPS connected to
a PMP system at the tailpipe. The >23 nm emissions with the
PNC are also shown but the PNC was measuring above its
measuring range due to the low dilution employed in the
specific test. The EEPS was measuring 80% higher than the
PMP method even when comparing with the PMP system at
CVS. Overestimation of the soot emissions with EEPS has also
been observed by others [155], but generally the
overestimation is around 30-50%. Experimental uncertainties
like different sampling locations (tailpipe - CVS), different
principles of operation, not ideal concentration levels measured
by the instruments can partly justify this big difference.
The sub-23 nm fraction not counted by the PMP method is
around 20% (based on EEPS size distributions) to 40% (CPCs
in CVS). For the specific vehicle there was no indication of high
concentration of sub-23 nm particles. Depending on the
vehicle, some high peaks were observed during some
accelerations. No high peaks were observed during
decelerations or those observed were significantly lower
compared to the emissions at normal speed. However, it
should be emphasized that there is a lot of smoothening of the
signal from the engine until the tailpipe and then inside the
PMP system. Similar conclusions were drawn also with the
other G-DI vehicles.
Conclusions
The results of the two JRC studies suggested the presence of
nano-sized particles in the exhaust of all vehicles tested, that
cannot be counted by a PMP compliant PNC due to the
relatively large cut-off size. The fraction of particles escaping
detection was 50% for PFI vehicles and for the late technology
DPF equipped diesel vehicles with emission levels below the
Euro 5b limit. At the even lower emission levels of the bi-fuel
PFI vehicle running on CNG or CNG/H2 mixtures and the DPF
vehicle tested at sub-zero ambient temperatures the fraction of
Figure 6. Real time signals of a G-DI over a NEDC. a) measurements

from the CVS b) measurements from the tailpipe.
SUMMARY/CONCLUSIONS
Particle Number (PN) systems consist of a Volatile Particle
Remover (VPR) and a Particle Number Counter (PNC). The
VPR removes volatile particles and dilutes the sample. The
PNC measures the number concentration of particles >23 nm
in order to exclude possible confounding of measurements by
low volatility species present as nucleation mode particles,
while including the primary soot (spherule) size of 23 nm.
Target of this report was to investigate whether it is necessary
to measure <23 nm particles. In other words it was investigated
whether smaller <23 nm solid particles are emitted by engines
in considerable concentration focusing on Gasoline Direct
Injection (G-DI) engines.

Initially the importance of solid sub-23 nm particles it was
investigated. The size of particles determines the deposition
location and deposition fraction. It increases with decreasing
size. The nature (physical and chemical composition) of
particles might also be important, e.g. metal oxides might have
more adverse health effects compared to other solid nanoparticles. Thus, in the presence of excessive sub-23 nm solid
particle fractions, the regulated procedure might fail to quantify
the number concentration of potentially harmful (i.e. owing to
their chemical nature) particles.
4.
Then a literature survey on primary particles, vehicle exhaust

size distributions and solid <23 nm particles followed. It was
confirmed that the mean size of the primary particles is around
25 nm, without significant differences between different
technologies. However the distribution of particles and primary
particles of G-DIs can be wider, so larger percentage of
particles <23 nm can exist. The structure of primary particles is
sometimes different (more amorphous) and unburned
hydrocarbons or volatile organics can be found. This means
that differences in the thermal pre-treatment (temperature,
residence time of PN systems) might lead to different results.
8.
A lot of studies have found a solid core mode with older and
modern diesel engines, both at low and high loads. Solid core
mode is often observed at gasoline engines with port fuel
injection (G-PFI) and it is assumed to originate from the metals
of the lube oil or from fuel additives. At G-DIs a shoulder at
10-20 nm appears quite often. For mopeds very often the size
distribution after thermal pre-treatment peaks at or below 20
nm. It should be mentioned that in many studies it was
recognized that the solid core mode was re-nucleation artifact
of the PMP method and the dilution factors employed.
Finally, the experimental investigation at JRC (solids <23 nm)
showed that for emission levels around 1012 p/km, the
percentage of solid particles not measured (i.e. <23 nm) is
30-40% for G-DIs; similar to diesels. Higher percentages can
be measured at low ambient temperatures or high ethanol
fuels.
Based on the results of this review at the moment there is not
enough data to support a change of the legislation. However
due to increased <23 nm solid particle emissions in some
cases (additives in fuel or lubricant, special calibration of an
engine etc.) sub-23 nm particle emissions should be
monitored.
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DEFINITIONS/ABBREVIATIONS
CONTACT INFORMATION
PMP - Particle Measurement Programme
Barouch Giechaskiel
Sustainable Transport Unit
Joint Research Centre of the European Commission
I-21027 Ispra (VA), Italy
barouch.giechaskiel@jrc.ec.europa.eu
http://iet.jrc.ec.europa.eu/sustainable-transport
ACKNOWLEDGMENTS
The authors would like to acknowledge Dr. Athanasios
Mamakos and Dr. Matti Maricq for their helpful comments on
the first drafts of the manuscript.
CNG - Compressed Natural Gas

CPC - Condensation Particle Counter
CRT - Continuous Regenerating Trap
CS - Catalytic Stripper
CVS - Constant Volume Sampler
DMS - Differential Mobility Spectrometer
DOC - Diesel Oxidation Catalyst
DPF - Diesel Particulate Filter
EEPS - Engine Exhaust Particle Sizer
EGR - Exhaust Gas Recirculation
EJ - Ejector
ELPI - Electrical Low Pressure Impactor
ET - Evaporation Tube
FMPS - Fast Mobility Particle Sizer
G-DI - Gasoline Direct Injection
GPF - Gasoline particulate Filter
HD - Heavy Duty
JRC - Joint Research Center
LD - Light Duty
MD19 - Matter Diluter
MPI - Multi-Port Injection
NRMM - Non Road Mobile Machinery
PAH - Poly-Aromatic Hydrocarbons
PCRF - Particle Concentration Reduction Factor
PFI - Port Fuel Injection
PM - Particulate Matter
PN - Particle Number
PNC - Particle Number Counter
POC - Particle Oxidation Catalyst
SCR - Selective Catalytic Reduction of NOx
SMPS - Scanning mobility Particle Sizer
TD - Thermodenuder
TEM - Transmission Electron Microscopy
TWC - Three-Way Catalyst
VPR - Volatile Particle Remover
WLTC - World harmonized Light duty Test Cycle
APPENDIX
Table A1. Summary of studies that measured solid particles <23 nm. In grey studies that used lower than 250C as thermal pre-treatment of the aerosol.

Table A1. (cont.) Summary of studies that measured solid particles <23 nm. In grey studies that used lower than 250C as thermal pre-treatment of the
aerosol.
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photocopying, recording, or otherwise, without the prior written permission of SAE International.
Positions and opinions advanced in this paper are those of the author(s) and not necessarily those of SAE International. The author is solely responsible for the content of the
paper.

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Engine Exhaust Solid Sub-23 nm Particles: I. Literature Survey

nucleation mode particles (droplets). Thus at the end of the

The nucleation mode, which contains mainly volatile

The accumulation mode, which consists mainly of the

The coarse mode, which consist of deposited particles

Most particles, by mass, reside in the accumulation mode,

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

Figure 1. Typical sequence of particle transformation from the engine

Particle Number (PN) Method

The PN standard was introduced for Diesel Light Duty vehicles

HEALTH EFFECTS OF VEHICLE EXHAUST

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

The deposition location of an inhaled particle is a determining

Figure 2. Calculated deposition fraction of inhaled particles as a

Some authors suggest that the soot is the component that

Total mass still correlates best with adverse health effects,

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

Both soluble and insoluble fractions have been identified

The size of particles determines the deposition location

Thus in the presence of excessive sub-23 nm solid

Next chapters will focus on the concentration of vehicle

LITERATURE SURVEY ON SOLID PARTICLE

particulates. In [79], for early fuel injection strategy, liquid

Typical Size Distributions

Solid <23 nm Particles Studies

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

Diesel (41 Engines and Vehicles)

Metal Oxides (Fuel)

G-DI (12 Engines and Vehicles)

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

2-Wheelers (9 Mopeds and Motorcycles)

EXPERIMENTAL INVESTIGATION ON SOLID

Figure 3. Sub-23 nm particles in function of the solid >23 nm PN

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

The emission levels of the DPF vehicles for the WLTC

The percentage was >100% for emission levels close

G-DIs emissions ranged from 61011 p/km to 61012 p/km.

Low ambient temperatures (7C) increased this

High ethanol content (E85 vs E5) resulted in significant

It should be also noted that the losses in the VPR in

Figure 4. Sub-23 nm particles in function of the solid >23 nm PN

Figure 5 gives some examples of size distributions. These

Figure 5. Examples of size distributions measured with G-DI and DPF

Size distribution measurements showed sometimes a

In general the fraction of sub-23 nm particles estimated

Size distribution measurements during the regeneration

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

Tests with mopeds also revealed that volatiles can be

particles escaping detection with the PNC at 23 nm was

These tests didn't include heavy-duty engines, which, based on

Real Time Signals

Figure 6. Real time signals of a G-DI over a NEDC. a) measurements

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

Then a literature survey on primary particles, vehicle exhaust

Alfldy, B., Giechaskiel, B., Hofmann, W., and Drossinos, Y.,

Andersson, J., Wedekind, B., Hall, D., Stradling, R. et al.,

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

45. Happonen, M., Matilainen, P., Kanniainen, K., Kinnunen, T. et al.,

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

Giechaskiel et al / SAE Int. J. Fuels Lubr. / Volume 7, Issue 3 (November 2014)

125. Pope, C. III, Epidemiology of Fine Particulate Air Pollution and