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 Fuel 188 (2017) 603609

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journal homepage: www.elsevier.com/locate/fuel

Full Length Article

Trace metals and ions in particulates emitted by biodiesel fuelled engine

Pravesh Chandra Shukla a, Tarun Gupta a, Nitin Kumar Labhsetwar b, Avinash Kumar Agarwal c,
a
Department of Civil Engineering, Indian Institute of Technology Kanpur, Kanpur 208016, India
b
National Environmental Engineering Research Institute (NEERI), Nagpur 440 020, India
c
Engine Research Laboratory (ERL), Department of Mechanical Engineering, Indian Institute of Technology Kanpur, Kanpur 208016, India

h i g h l i g h t s

Trace metals & inorganic ions in particulate from B20 & diesel exhaust.

Inorganic ions: nitrates, chlorides, fluorides & sulphates were measured.

Trace metals & Ions in particulate decreased with increasing load.

Biodiesel particulate had slightly lower trace metals & inorganic ions.

Morphological studies showed reduction in particulate with DOC.

a r t i c l e i n f o a b s t r a c t

Article history: Particulates emitted by a transportation diesel engine fuelled with Karanja biodiesel blend (20% v/v bio-
Received 16 November 2015 diesel blended with 80% v/v mineral diesel) were tested for the trace metal content and inorganic ions.
Received in revised form 6 August 2016 These particulate were analyzed and compared with baseline mineral diesel particulate for 9 commonly
Accepted 11 October 2016
present trace metals namely Ca, Fe, Cr, Cu, Mn, Pb, Ni, Ba and Cd and inorganic anions such as nitrates,
Available online 19 October 2016
chlorides, fluorides and sulphates. Trace metals in particulate decreased with increasing engine load.
Ions analyzed in particulate from diesel and biodiesel also showed decreasing trend with increasing
Keywords:
engine load. Biodiesel origin particulate contained slightly lower amount of trace metals and inorganic
Biodiesel
Particulate
ions compared to mineral diesel for similar operating conditions except nitrates. Particulate sampled
Trace metals on the quartz filter paper were also analyzed for their morphology and 1000 magnification images were
Inorganic ions captured using scanning electron microscopy (SEM) in order to visualize bulk particulate emission from
Diesel oxidation catalyst (DOC) Karanja biodiesel exhaust compared to baseline mineral diesel.
Scanning electron microscopy 2016 Elsevier Ltd. All rights reserved.

1. Introduction
Particulate emissions from vehicles are responsible for harmful
health impact on humans and the environment. They adversely
impact health and environment because they get ingested into
the human body by inhalation, contaminate various environmental
media by toxic substances, affect visibility adversely (due to black
smoke), and accelerate global climatic change (due to black carbon
emissions) [1]. In recent years, diesel particulate matter (DPM) has
emerged as the main pollutant, which adversely affects human
health, especially in urban settlements, mainly because of
increased use of diesel fuelled vehicles. Several studies have been
performed for characterization and reduction of DPM [25]. DPM
consists of elemental carbon (EC), organic carbon (OC), sulphates,
nitrates, trace metals, etc. [6]. It is reported that transition metals
Corresponding author.
E-mail address: akag@iitk.ac.in (A.K. Agarwal).
can penetrate deep into the airways in the human body and can
even enter into the cells of the human body. These trace metals
then increase the reactive oxygen species (ROS) activity in the cell
structures [79], which results in elevated oxidative stresses
[10,11]. HEI [12] report elaborated that there are mainly four
sources of trace metal emissions from the vehicle viz. tailpipe
emissions, metals emanating from tyre wear, metals emanating
from brake liner wear and re-suspension of road dust in the ambi-
ent environment. They performed a study for characterization of
trace metal emissions from vehicles by carrying out an extensive
tunnel and lab based sampling of vehicular smoke [12]. They ana-
lyzed these four sources of trace metals due to vehicular activities
and attributed their individual contributions to the total trace
metal emission using chemical mass balance (CMB) model. Trace
metals are either crustal metals or anthropogenic metals, which
may be non-carcinogenic or carcinogenic however trace metals
emitted by the engine are considered anthropogenic metals.
IARC-1990 and IARC-1993 considered Ni, Cd and Cr as carcinogenic

http://dx.doi.org/10.1016/j.fuel.2016.10.059
0016-2361/ 2016 Elsevier Ltd. All rights reserved.
604 P.C. Shukla et al. / Fuel 188 (2017) 603609
metal elements [13,14]. Several scientific studies reported that bio-
diesel is emerging as an important alternative fuel globally. Studies
showed that total particulate mass (TPM) emissions from biodiesel
or its blends were lower compared to baseline mineral diesel [15
19]. Studies also showed the production and utilization challenges
of biodiesel for use in internal combustion engines [2022]. With
increasing possibility of biodiesel usage on a large scale worldwide,
there is a need to comprehensively investigate the chemical com-
position of diesel and biodiesel origin particulate from environ-
mental and health perspective. Betha et al. characterized the
emission of particle bound trace metals from a stationary engine
fuelled with ultra-low sulphur diesel (ULSD), waste cooking oil-
derived biodiesel (B100) and blend of both (B50), and observed
that crustal elements such as Mg, K and Al were found to be in
higher concentration in particulates than other constituents [23].
They also estimated the health risks based on exposure and
dose-response assessment and reported that exposure to biodiesel
(B100) particulate was more toxic compared to ULSD origin partic-
ulate [23]. In another study performed by Wang et al. 2003, it was
reported that crust metals were in significantly higher concentra-
tion compared to anthropogenic metals emitted by a diesel engine
operated under transient conditions [24]. Muzyka et al. reported in
their study that the trace metals were generally attached to the
fine granular matter present in the exhaust [25]. Valavanidis
et al. explored the toxic effects of Fe, when it penetrated into the
lower airways of human lungs [26]. Sharma et al. characterized
diesel particulate for trace metals and other emissions from a
40 kW diesel engine [27]. They reported that the trace metal con-
tent decreased in the particulate as the engine load increased from
idle to full load. They also reported that the crust elements Fe, Mg,
Ca were much higher as compared to other trace metals [27].
Gangwar et al. performed experiments on comparative toxicity of
diesel and biodiesel particulate using a modern common rail direct
injection (CRDI) transportation engine [28]. They reported that
trace metals in the particulate decreased with increasing engine
load [28]. Cheung et al. evaluated the emissions of trace metals
and organic species from three light-duty passenger vehicles in five
different configurations [29]. Their results showed much higher
crustal trace metal emissions compared to anthropogenic trace
metal emissions [29]. Kothari et al. performed chemical analysis
of particulate collected from a engine fuelled with mineral diesel
and biodiesel blends for trace metals, benzene soluble organic frac-
tion, etc. [30]. They reported that Ca, Mg, Fe, Zn were in relatively
higher concentration in biodiesel particulate, while Cu, Pb, Cr, Ni,
Na were in relatively higher concentration in diesel particulate
[30]. Dwivedi et al. reported that use of 20% biodiesel blend
(derived from rice-bran oil) led to increase in carcinogenic metal
element such as Cr and decrease in carcinogenic metal elements
such as Cd and Ni [31]. Trace metal concentration in exhaust
may also vary depending on type of feedstock oil used for biodiesel
production. As evident from the literature, DOC is quite an effective
tool for reduction of particulate emissions and their toxicity. How-
ever, DOCs are not widely investigated for their effect on trace
metal emissions from transport diesel engines. Therefore, there is
a need to investigate the effect of DOCs on the trace metals in
exhaust emissions from transport diesel engines. In the present
study, an attempt has been made to determine the concentrations
of trace metals and inorganic ions in Karanja biodiesel blend
(KB20) origin particulate vis--vis mineral diesel origin particulate,
emanating from a medium duty transportation engine.
2. Experimental setup and methodology
A four-cylinder naturally aspirated water-cooled transportation
engine (Tata Motors; Indica 475 IDI) was used for the comparative
chemical analysis of mineral diesel and Karanja biodiesel (KB20)
origin particulate. The test engine was equipped with a rotary fuel
injection pump and a commercial diesel oxidation catalyst (DOC).
Engine crankshaft was coupled to an eddy current dynamometer.
Fig. 1 shows the schematic of the experimental setup. Test engine
and dynamometer specifications are given in Tables 1 and 2.
Diesel and biodiesel particulate were collected from the engine
exhaust on a filter paper. Before particulate sampling, blank filter
paper sample was taken in order to account for the background
concentration of trace metals. Blank values were subtracted from
the sample values for this purpose. Sections of this filter paper
were analyzed for particulate mass, trace metals, inorganic ions
and morphology. For morphological comparison, particulate
images were taken at 1000 magnification using a field emission
scanning electron microscope (FE-SEM) for all particulate samples
collected on the filter paper. FE-SEM features magnification of
more than one million times and its resolution is up to 2 nm
(Source: Centre of Nano-Sciences, IIT Kanpur, India).
A commercial DOC was fitted in the exhaust pipe of the test
engine, and particulate were collected with and without DOC. Sam-
pling probes in the exhaust line were used to divert a fraction of
exhaust into a partial flow dilution tunnel, where it mixes with
preconditioned and filtered air. Partial flow dilution tunnel is a
device in which, a fraction of exhaust mixes with pre-
conditioned and filtered air and a fixed dilution ratio is maintained
in this device. Dilution ratio was kept at 16 and conditioned air
temperature was maintained at 52 C during the experiments.
For all operating conditions, the exhaust diluted with conditioned
air was passed through a filter paper and the particulate were col-
lected on the preconditioned quartz filter paper placed inside the
filter holder assembly of the dilution tunnel. Table 3 provides the
details of biodiesel properties measured.
2.1. Procedure
Particulate samples were collected on 47 mm diameter quartz
filter papers under different engine operating conditions. Each fil-
ter paper was placed in desiccator for 24 h before sampling, in
order to remove moisture traces. Particulate sampling was done
for 15 min under predetermined conditions and particulate laden
filter papers were again kept in desiccator immediately after the
sampling. The difference in weights before and after the sampling
gives the particulate loading on the filter paper. From these filter
papers, two filter paper portions (Circular holes of 16.5 mm diam-
eter) were extracted for ion chromatography and trace metal anal-
ysis respectively. These samples were analyzed for trace metal
concentration byinductively couple plasma-optical emission spec-
troscopy (ICP-OES) technique and for ions by using ion chromatog-
raphy technique. Details on ICP-OES and ion chromatography
analyzes can be found in our earlier publication by Chakraborty
and Gupta [32]. For comparative morphological investigations,
images of particulate laden filter paper with 1000 magnification
were taken by placing a 9.5 mm diameter punched portion of filter
paper in a scanning electron microscope (SEM). Test matrix for all
experiments and analyses in this study is given in Table 4.
3. Results and discussion
Diesel and Karanja biodiesel (B20) particulate were collected on
a filter paper, with and without using DOC. PM emissions increased
with increasing engine load for diesel and biodiesel both (Fig. 2) for
identical sampling duration. Increased fuel quantity injected at
higher engine load was the main reason for increased particulate
emission from these test fuels. Biodiesel however showed signifi-
cantly lower PM emissions (approximately 50% lower) compared
 P.C. Shukla et al. / Fuel 188 (2017) 603609 605

Fig. 1. Schematic of the experimental setup.

Table 1
Specifications of the test engine.

Make/ Model Tata motors/ Indica 475 IDI

Engine type Water cooled IDI engine
No. of cylinder/ Configuration 4/ inline
Bore/ Stroke 75 mm/ 79.5 mm
Cubic capacity 1405 cc
Maximum engine output 39 kW @ 5000 rpm
Maximum torque 85 Nm @ 2500 rpm
Compression ratio 22:1
Firing order 1-3-4-2
Fuel injection system Rotary pump with electric stop solenoid

Table 2
Specifications of eddy current dynamometer.

Make/ Model Dynalec controls/ ECB-200

Max. torque 420 Nm @ 15003500 rpm
Max. power 200 HP @ 35008000 rpm
Cooling Water cooled Fig. 2. Total particulate mass collected on filter paper with and without DOC from
Max. excitation current 6 Amps D.C. diesel and biodiesel fuelled engine exhaust.

Table 3
to mineral diesel. Biodiesel comprises of several fatty-acid mono-
Measured test fuel properties. esters, which offer advantages over mineral diesel such as higher
cetane number, and higher oxygen content (11%) [33]. These fuel
Fuel property Diesel Biodiesel (B20)
properties lead to superior combustion of fuel droplets sprayed in
Specific gravity 0.846 0.848 the combustion chamber, resulting in lower particulate mass emis-
Kinematic viscosity (cSt) @ 30 C 2.60 3.39
sions. It can be noticed that PM emissions reduced by 4050% by
Calorific value (MJ/kg) 42.21 38.28
Flash point (C) 52 79 using DOC for both test fuels. DOC is therefore an effective tool
in reducing the soluble organic fraction (SOF) of the particulate.

Table 4
Test matrix for particulate characterization.

Engine load (%) Diesel (without DOC) B20 (without DOC) Diesel (with DOC) B20 (with DOC)
p p p p
0
p p p p
25
p p p p
50
p p p p
75
p p p p
100
606 P.C. Shukla et al. / Fuel 188 (2017) 603609
Although, the particulate mass reduction is modest by employing
DOC, however it is the toxic part of the particulates, which is
knocked off by the DOC.
3.1. Trace metals in particulate
The exhaust particulate were collected on a pre-conditioned fil-
ter paper and then analyzed for trace metals. Trace metals in diesel
and B20 particulate were compared for various engine loads at
constant engine speed (2500 rpm). Trace metals such as Ca, Fe,
Cr, Cu, Mn, Pb, Ni, Ba and Cd were detected and determined
(mg/g) by ICP-OES. Trace metal content in particulate reduced with
increasing engine load for both diesel and B20 (Fig. 3). There are
three main sources of trace metals in engine exhaust: (1) trace
metals present in fuel; (2) organo-metallic additives in lubricating
oil; and (3) wear metals from the engine components such as pis-
ton rings, piston, cylinder liner, and valve seats [34,35].
The contribution of trace metals from these three sources lar-
gely depend upon engine operating conditions. Fuel-borne trace
metal contribution would always increase with increasing engine
load, because of the injection of higher fuel quantity. Since the
engine speed essentially remained constant in this study, the trace
metal contribution from lubricating oil and wear debris is not
Fig. 3. Trace metals in exhaust particulate from diesel and B20, with and without DOC.
affected significantly by engine speed but it is affected by engine
load. Therefore particulate emission would increase possibly due
to higher fuel quantity injection, but trace metal content may not
increase in the same proportion in the particulate. This result in
overall reduction in trace metal concentration per unit of mass of
particulate collected, with increasing engine load.
3.1.1. Effect of fuel
Relatively higher trace metal content was observed for B20 par-
ticulate with very few exceptions (Fig. 3), compared to baseline
mineral diesel. This suggested higher trace metal emissions per
unit particulate mass from B20, although B20 resulted in overall
lower particulate mass emissions compared to mineral diesel. All
trace metals reported in this study are an average of three separate
observations, along with the method detection limit (MDL) and
standard deviation during analysis by ICP-OES. It is established
that biodiesel has higher density and viscosity compared to base-
line mineral diesel, resulting in relatively inferior fuel atomisation
of biodiesel during fuel injection under identical conditions. Larger
droplets of biodiesel fuel spray also results in higher spray jet pen-
etration in the combustion chamber than desired level and these
fuel droplets may even impinge upon the cylinder liner walls
 P.C. Shukla et al. / Fuel 188 (2017) 603609 607

sometimes, where they come in contact with lubricating oil pre-

sent on the cylinder walls.
These fuel droplets not only dilute the lubricating oil but also
wash away the lubricating oil film present in the cylinder liner,
thus enhancing wear of the engine due to sliding contact between
piston ring-liner interfaces. This leads to increased lubricant con-
sumption, partial combustion of lubricating oil in the combustion
chamber, and higher wear debris generation, which ultimately
results in higher trace metal concentration in B20 fuelled engine
per unit mass of particulate.

3.1.2. Effect of DOC

Use of DOC leads to slight increase in trace metal concentration
at all loads for both test fuels (Fig. 3). DOC exhibits excellent per-
formance in oxidising OC (SOF part) of particulate, which lead to
reduction in total particulate mass [36]. However DOC is not effec-
tive in removing other component of particulate such as EC and
trace metals. Therefore trace metal concentration per unit mass
of particulate collected on the filter paper downstream of DOC
increased for diesel and B20. This obviously is not because of
increased trace metal emission with use of DOC, but the reduction
of OC. Table 5 lists various possible sources of trace metals in
engine exhaust particulate.

3.2. Inorganic anions in particulate

Sulphate, nitrate, fluoride and chloride anions were also deter-

mined in the particulate emitted in diesel and B20 exhaust. Fuel
impurities lead to formation of these ions. Fig. 4 shows the concen-
tration of these inorganic ions in the particulate.

3.2.1. Effect of fuel

Nitrate, chloride and fluoride were found to be in higher con-
centration in B20 compared to diesel at all loads (Fig. 4). The con-
centration of these anions per unit mass of particulate was higher
Fig. 4. Sulphate, nitrate, fluoride and chloride ion concentration per unit mass of
at lower engine loads, and it decreased with increasing engine load particulate from diesel and B20, with and without DOC.
for both fuels (with an exception of sulphate emission at full load
condition). The fraction of anions in total particulate reduced with
increasing engine load. In case of sulphates, B20 particulate
3.2.2. Effect of DOC
showed reverse trend. Sulphate concentrations were lower in
Fraction of nitrate, chloride, fluoride and sulphate ions
B20 particulate compared to diesel particulate, possibly because
increased in the particulate collected after DOC (Fig. 4). DOC is
of lower sulphur content of B20. As the engine load increases,
effective in reducing the SOF fraction of the particulate and does
the in-cylinder temperature also increases, leading to oxidation/
not affect any of these anions present in the particulate. Therefore
dissociation of a fraction of these anions. This resulted in reduced
we observe an increase in the concentration of these anions in the
anions at relatively higher engine loads per unit particulate mass
particulate with the use of DOC.
emitted by the engine.

3.3. SEM images of diesel and B20 particulate

Table 5
Typical sources of trace metals in engine exhaust particulate [22,24,29,30,32]. Fig. 5 shows the SEM micrographs of particulate collected on
the filter papers from diesel and B20 fuelled engine at various
Trace Sources of trace metals
loads. These SEM images are a good tool for qualitative analysis
metal
of particulate emission under different engine operating condi-
Ca Detergent/dispersant additives in lubricating oil; present in
tions. In general, fluffy mass lumps of carbonaceous material are
mineral diesel
Fe Present in mineral diesel; Wear of engine components seen in these images, which increase in concentration with
Cr Wear of engine parts of various alloys; piston ring coatings increasing engine load. The images were taken at 1000 magnifi-
Cu Wear of bronze and brass parts, such as crankshaft bearings; anti- cation (Fig. 5). It is difficult to appreciate comparative mass emis-
wear additive (Zinc-di-alkyl-di-thio-phosphate: ZDDP) in sion or composition of particulate from diesel and B20 by merely
lubricating oil
Mn Detergent/dispersant additive in lubricating oil; knock improver
observing these SEM images. However these SEM images clearly
additive indicate relatively less fibres (of filter paper) in images taken at
Pb Present in mineral diesel; wear of metal alloys higher load conditions, which shows higher soot collection on
Ni Present in mineral diesel; virgin engine oil the filter paper at higher engine load. The SEM images after DOC
Ba Detergent/dispersant additive in lubricating oil
also showed relatively more fibres compared to the ones taken
Cd Engine alloys; present in mineral diesel
under identical conditions but without DOC. This shows that the
608 P.C. Shukla et al. / Fuel 188 (2017) 603609

Biodiesel without
Diesel without DOC Diesel with DOC Biodiesel with DOC
DOC
1000X 1000X 1000X 1000X
0%
25%
50%
75%
100%

Fig. 5. SEM images of diesel and B20 particulate (at 1000 magnification, EHT = 5.00 kV, Signal A- In Lens), with and without DOC.

DOC is effectively reducing the particulate mass emission from the
engine [37].
4. Conclusions
1. Total particulate mass emission was significant lower for B20
compared to baseline mineral diesel, however, trace metals
concentration per unit mass of particulate for Ca, Fe, Cr, Cu,
Mn, Pb, Ni, Ba and Cd were observed to be slightly higher for
B20 at all engine operating conditions. This is due to relatively
lower particulate mass emitted by B20.
2. Three main sources of trace metals in particulate are; (i) fuel,
(ii) friction and wear debris and (iii) lubricating oil additives.
Despite increasing PM mass emission with increasing engine
load, trace metal concentration per unit mass of particulate
decreased. This indicates that trace metal emissions do not
increase in the same proportion as the particulate mass, with
increasing engine load.
3. Trace metals namely Ca, Fe, Cr, Cu, Mn, Pb, Ni, Ba and Cd were
detected in diesel and B20 particulate, with slightly higher con-
centrations in B20 particulate. Crustal metals like Ca and Fe
were approximately 80% of the mass of total detected trace
metals.
4. DOC oxidised most of the soluble organic fraction of particulate,
which resulted in higher proportion of trace metals in particu-
late collected after DOC, increasing its concentration per unit
mass. DOC does not affect the trace metals present in the
particulate.
5. Sulphate ions per unit mass of particulate were lower for B20
due to the absence of sulphur in biodiesel. However chloride,
fluoride and nitrate ion concentrations in particulate (per unit
mass of particulate) were higher for B20 compared to mineral
diesel. Increase in concentration of these anions in the particu-
late was observed with use of DOC.
6. Significant reduction in particulate mass was seen in SEM
images, when DOC was used.
 P.C. Shukla et al. / Fuel 188 (2017) 603609
In summary, B20 emitted relatively lower particulate mass
emissions compared to mineral diesel however trace metals and
inorganic ions were in higher concentration in particulate emitted
by B20 fuelled engine compared to baseline mineral diesel fuelled
engine, indicating its relative higher toxicity.
Acknowledgements
Authors would like to acknowledge the research grant from
Science and Engineering Research Board (SERB), Department of
Science and Technology, Government of India (Grant No. SR/S3/
MERC-0084/2011 dated 22nd June 2012) for carrying out this
study. Council of Scientific and Industrial Research (CSIR), New
Delhi supported Mr. Pravesh Chandra Shukla by awarding him
Senior Research Associateship (Pool Scientist) for carrying out this
study at Engine Research Laboratory of IIT Kanpur. Authors would
also like to acknowledge Mr. Roshan Lal and Staff of Engine
Research Laboratory for their valuable support during the
experiments.
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