Int. J. Environment and Waste Management, Vol. 13, No.

2, 2014 199

Chemical and morphological study of PM10 and PM2.5

in Pune, India

Suman Yadav and P. Gursumeeran Satsangi*

Department of Chemistry,
University of Pune,
Pune – 411 007, India
E-mail: sumaninostar@gmail.com
E-mail: pgsatsangi@chem.unipune.ac.in
*Corresponding author

Abstract: PM10 and PM2.5 ambient samples were collected by a particulate

sampler (APM 550, Envirotech) in the Department of Chemistry, University of
Pune, India. Exposed filters were used to determine the mass, ionic
composition and morphology of fine PM. The mean PM10 and PM2.5
concentrations were 16.69 ± 5.6 µg m–3 and 11.68 ± 4.1 µg m–3, respectively.
Neutralisation factors for all major cations were computed and found to be
higher for Ca2+ while for PM2.5 it was higher for NH4+. Calculation revealed
that in particulate matter 25% of SO42– in both PM10 and PM2.5 and 30% of
NO3– in PM10 is coming from anthropogenic sources, whereas other species are
coming mainly from the natural sources. Morphology and chemical
composition of 236 individual particles were determined by scanning electron
microscopy-energy dispersive spectrometer. Based on morphological study, the
particles were clustered as: Si-rich particles (56%), soot (16%), oxides (10%),
sulphates (8%), carbonates (5%), metal-rich (4%), and biological particles
(3%).

Keywords: particulate matter; chemical composition; vehicular emissions;

sea salt ratios; morphology; India.

Reference to this paper should be made as follows: Yadav, S. and

Satsangi, P.G. (2014) ‘Chemical and morphological study of PM10 and PM2.5 in
Pune, India’, Int. J. Environment and Waste Management, Vol. 13, No. 2,
pp.199–216.

Biographical notes: Suman Yadav is a Junior Research Fellow in the

Department of Chemistry, University of Pune on DST (New Delhi) project. She
has completed her Master’s in Chemistry. She has done her Master project on
particulate matter and presently working in the field of atmospheric chemistry.

P. Gursumeeran Satsangi is an Assistant Professor in Department of Chemistry,

University of Pune. She received her PhD in Atmospheric Chemistry from
Dayalbagh Educational Institute in 1999. Her major interest is in monitoring of
air pollutants and its related chemistry. She has completed two projects
sponsored by DST, New Delhi and BCUD, University of Pune, Pune. She has
guided 11 master students and three MPhil students.

Copyright © 2014 Inderscience Enterprises Ltd.

200 S. Yadav and P.G. Satsangi

1 Introduction

Rapid growth of industries, vehicles, population, and anthropogenic activities has

resulted in higher concentrations of particulate matter (PM) in the megacities of most of
the rapidly developing countries in Asia (Lawrence and Lelieveld, 2010). Among the air
pollutants identified for adverse health effects, PM has received a special attention
because of its strong association with daily total and cause-specific mortality rates. The
relative strength of association of air pollutants with cause-specific mortality was
reported as follows: PM2.5 ≥ PM10 ≥ SO2 ≥ H+ ≥ O3 ≥ NOx (Dockery et al., 1992).
Dockery and Pope (1994) reported that for each 10 μg m–3 increase in concentration of
PM less than 10 μm diameter (i.e., PM10), there is an estimate of increase in mortality of
0.6% to 1.6% with an average increase of 1% (Ostro, 1996). The health impacts of fine
PM (i.e., PM2.5) are greater because it can penetrate deep into unciliated and alveolar
sections of the lung according to the particle diameter size (Spengler et al., 1990).
PM and gaseous pollutants emitted from vehicles originate from combustion
processes of fuel and lube oil and from evaporation of the fuels itself (Cheng et al.,
2006). Thus, PM is a complex mixture of soil dust and anthropogenic particles from a
variety of sources such as street dust lofting, fuel and biomass burning. The magnitude
effect of PM on climate and atmospheric oxidants is dependent on chemical and physical
properties such as size, chemical composition and concentrations (Chakraborty and
Gupta, 2010; Kim et al., 2011). Water-soluble fraction of atmospheric PM contains many
important compounds like (NH4)2SO4, NH4HSO4, NH4NO3, CaSO4, (Na)2SO4, etc. which
can change the size, composition, number and lifetime of PM due to their hygroscopic
nature (USEPA, 1996; Jacobson et al., 2000; Novakov and Penner, 1993; Safai et al.,
2010). On the other hand, water-soluble components increase the solubility of toxic
organic compounds such as n-alkanes and polycyclic aromatic hydrocarbons (PAHs), by
acting as surface active reagents and therefore increase their toxicity to human health.
Numerous studies have also been performed in order to understand the climatic effects of
atmospheric PM (Adachi et al., 2010; Hobbs et al., 1997; Penner et al., 2001). Thus,
detailed information on the particle’s chemical and physical properties is important. The
main objective of the present study is to investigate the concentration of cations and
anions along with major acidifying (SO42– and NO3–) and alkaline (Ca2+ and NH4+)
constituents of PM (PM10 and PM2.5) at semi-urban site in Pune, India and to evaluate
their effect on the acidification/neutralisation potential and morphology of the PM. Data
obtained from this study, will delineate the physical and chemical characteristics of the
PM to understand their significance on local and regional climate system during the
monsoon season.

2 Materials and methods

2.1 Site description

Pune (18° 32N, 73° 51E) is rapidly growing city in terms of industrial installations,
vehicular population and urbanisation due to the boom in housing industry. It is situated
in the southwest part of India, at about 100 km from Arabian Sea (Figure 1). PM samples
(N = 27) were collected for the period of almost one month (from 3rd September to 29th
 Chemical and morphological study of PM10 and PM2.5 in Pune, India 201

September 2010) on the terrace of Chemistry Department, University of Pune, Pune, a

semi-urban site. The sampling site is surrounded by variety of deciduous trees.
No industries are located in the vicinity of sampling sites. Soil dust is one of the
major sources of particulate pollutants. In addition, biomass burning, vehicular activities
and constructions are sources of anthropogenic PM. Major traffic junction (i.e.,
University circle) and a railway line are nearly 1 km and 3 km from the sampling site,
respectively. At the university circle, heavy traffic is observed throughout the day on coal
tar roads. During the monsoon season (September), winds are generally from W/SW
direction (Figure 2) which contributes almost 80% of the annual rainfall. The city
receives both marine (due to westerly winds from Arabian Sea) as well as continental air
masses.

Figure 1 Map showing the sampling site (see online version for colours)
202 S. Yadav and P.G. Satsangi

2.2 Sample collection

24 h PM10 and PM2.5 ambient samples were collected with fine particulate dust sampler
(APM 550, Envirotech), which operates at a constant flow rate of 16.6 L min–1. It has a
portable Wins-Anderson impactor for the sampling of PM2.5. The particles were collected
on Whatman Polytetrafluoroethylene (PTFE) filters of 47 mm diameter with pore size
2 µm for PM2.5 and quartz fibre filters –47 mm dia. (Whatman) for PM10. Sampling of
PM was carried out at a height of ~12 m from the ground level at department terrace.

Figure 2 Wind rose during the study period (see online version for colours)

2.3 Gravimetric and chemical analysis

Filters were weighed three times before and after sampling, using digital balance
(Sartoriuos) with sensitivity of ± 0.2 mg. Filters were equilibrated in a silica gel
desiccators for 24 h before weighing, to eliminate the effect of humidity and temperature.
Field blank filters were also collected to reduce gravimetric bias due to filter
handling during and after sampling. Filters were handled only with tweezers coated
with Teflon tape to reduce the possibility of contamination. After weighing, samples
were stored in a refrigerator at 4°C to prevent the evaporation of volatile components.
It is assumed that the deposited particles are distributed uniformly over entire area
of filter. After gravimetric analysis, filters were used to analyse water soluble
components.
 Chemical and morphological study of PM10 and PM2.5 in Pune, India 203

2.4 Extraction of PM
After weighing, 1 cm2 size subsample was cut out of the main filter for the SEM analysis.
Remaining filter was used for determination of chemical composition. Filters were
extracted for water soluble components by soxhlet extractor. The extracting solvent was
poured into the distillation flask in which filter was kept and made to boil with low heat
(70°C for acid soluble, 75°C for water soluble) for 45 minutes. The vapours of the
solvent were led to the extractor through a wider tube and then reflux to condenser. Cool
water was continuously flowing around the condenser through the inlet and outlet tube.
Due to heat, vapours go to the condenser and get condensed and the solvent drain down
into the extractor. When the level of the liquid reaches the upper part of the siphon, it
automatically gets drained into the flask. The constant volume of the liquid level was
maintained in the extractor. After extraction, the water soluble extracts of PM were
analysed for Cl–, SO42–, NO3–, NH4+, Na+, K+, Ca2+ and Mg2+. Chemical analysis
of anions (Cl–, SO42–, NO3–) was carried out with an ion chromatograph
(DIONEX, DX-100), using analytical column AS4A-SC 4 mm (P/N 04317), 1.8 mM
Na2CO3/1.7 mM NaHCO3 as an eluent, Milli-Q water as regenerant, anion micro
membrane suppressor and conductivity detector. The major cations (Na+, K+, Ca2+ and
Mg2+) were analysed by atomic absorption spectrophotometer (Perkin Elmer-AAnalyst
400) with an air acetylene flame. The NH4+ was measured by indo-phenol blue method
(Weatherburn, 1967). The detection limit for ion chromatographic analysis was about
0.01 μg ml–1 and that for the atomic absorption spectrophotometric analysis varied from
0.002 to 0.02 μg ml–1. Analytical quality check was done for instruments using different
standards and external reference samples; standard deviations for these standards were
about 2% to 4% that supports good analysis.

2.5 SEM-EDS measurements

Individual particle analysis was performed using JEOL JSM-6330F (JEOL Ltd.,
Akishima, Tokyo, Japan) scanning electron microscope (SEM) combined with energy
dispersive spectrometer (EDS). Elements with atomic number less than 6 were not
determined. Carbon and fluorine were also not considered in present discussion due to
their presence on the filter substrate. The previously cut 1 cm2 of filter was mounted on
an electron microprobe SEM stubs. A very thin film of platinum (Pt) was deposited on
the surface of the samples to make them electrically conductive. In the present
investigation, the SEM was used in its emissive mode. The other conditions were as
follows, detector: lithium drifted silicon [Si(Li)] detector, limit of detection, 500,000;
accuracy, 10%; energy, 20 kV (accelerating voltages, 0.5–30 kV).
In the present study, results are confined only for the monsoon season. In monsoon
season (September 2010), the relative humidity is very high (80% to 90%). In this regard,
PTFE is very stable and absorbed negligible water or gases. It has inherently low
contamination levels. PTFE filter has a fibre structure and good for studying the
gravimetric, elemental analysis as well as morphological studies. Many studies have
reported SEM-EDS on PTFE (Pipal et al., 2011; Slezakova et al., 2008; Wheeler et al.,
2000; Xie et al., 2009). In contrast, quartz filter is causing the positive artefacts and
uncertainties because of its fibre structure. Therefore, SEM-EDS analysis was concise
only for PM2.5.
204 S. Yadav and P.G. Satsangi

3 Results and discussion

Table 1 presents the concentration of PM10 and PM2.5 along with the meteorological
parameters. The concentrations of PM10 and PM2.5 at the University of Pune during the
study period ranged between 13.8 µg m–3 to 62.4 µg m–3 and 17.5 µg m–3 to
41.66 µg m–3, respectively. The average concentration of PM10 and PM2.5 was found to be
16.69 ± 5.6 µg m–3 and 11.68 ± 4.1 µg m–3, respectively. The average PM2.5 to PM10 ratio
is 0.69 which indicate that 69% of PM10 is made up of PM2.5 at Pune. Similar results have
been reported by earlier studies (Karar and Gupta, 2006; Kulshrestha et al., 2009;
Satsangi et al., 2011; Sharma and Maloo, 2005). Kulshrestha et al. (2009) have also
reported higher PM2.5 to PM10 ratio in monsoon season as coarse particles on absorbing
water settles down and therefore re-suspension and re-entrainment of soil is minimal. The
present data was compared with National Air Quality Standards (NAAQS) of PM10 and
PM2.5. Currently, the regulatory standards for PM10 and PM2.5 in ambient environments in
India are 100 and 60 μg m–3, respectively (Krishna, 2012). It was found that observed
average concentration of PM (PM10 and PM2.5) is lower than the Indian standards.
Table 1 Summary of meteorological parameters and PM concentrations in Pune

Parameters Temperature Relative Wind speed Wind PM10 PM2.5

unit °C humidity % Km hr–1 direction ° µg m–3 µg m–3
N 30.0 30.0 30 30 20 22
Geometric 23.0 84.1 1.3 220.1 15.9 11.2
mean
Mean 23.3 85.8 1.5 221.6 16.6 11.6
SD 3.6 15.9 1.3 42.6 5.6 4.1
Min 18.0 44.2 0.0 9.0 13.8 17.5
Max 32.3 100.0 5.5 338.0 62.4 41.6

Table 2 demonstrates the average concentrations of all water soluble ions in PM10 and
PM2.5. In both PM2.5 and PM10, higher concentrations are shown by SO42– which are
followed by Cl– > Ca2+ > Na+ > K+ > NH4+ > Mg2+ > NO3– for PM2.5 and Ca2+ > Cl– >
Na+ > NH4+ > NO3– > Mg2+ > K+ for PM10. Higher concentration of SO42– over other ions
in both PM2.5 and PM10 may be due to two possible reasons: first, emissions of SO2 due
to the heavy vehicular and chemistry lab activities, wherein different acids (H2SO4 and
HNO3) used for dissolution of ores and alloys, second, high relative humidity in monsoon
(85.8 ± 15.9%) enhances the sulphate formation (Kadowaki, 1986). In the fine fraction,
SO42– and NH4+ may form compounds like (NH4)2SO4 or NH4HSO4 as these compounds
mostly occur in fine fraction of PM (Seinfeld, 1986; Safai et al., 2010). The coarse
fraction of SO42– is in the form of gypsum (CaSO4) or as a reaction product with sea salt
aerosols like Na; (Na)2SO4 (Henning et al., 2003; Safai et al., 2010). On the other hand,
high concentration of Ca2+ also indicates considerable presence of soil-oriented
component mainly by natural (wind, storms) and anthropogenic (construction activities)
which were conducted on or near the sampling site (Safai et al., 2010). The lower
concentrations of Mg2+ in both PM10 and PM2.5 suggest that it mainly occur as insoluble
bicarbonates and silicates (Kulshrestha et al., 2009). Significant higher concentrations of
K+ are found in PM2.5 (0.88 µg m-3) than PM10 (K = 0.45 µg m-3). Fine mode K+ may be
released in to the atmosphere from vegetation (Kleinman et al., 1979) and biomass
 Chemical and morphological study of PM10 and PM2.5 in Pune, India 205

burning (Penner, 1995). At high humidity, the rate of transpiration is low, plants emit
submicron K+ through the respiration mechanism known as guttation. In this process, K+
is transported from root to leaves and released into the atmosphere through hydathodes
(Sharma et al., 2007). Na+ and NH4+ are also present in appreciable amount in PM2.5 and
PM10 samples. All other chemical ions show low concentration. The percentage
contribution of each ion toward the total PM is also calculated and found that the alkaline
components (Ca2+, Mg2+, Na+ and K+) contribute 40% for PM10 and 42% for PM2.5, NH4+
10% for PM10 and 9% for PM2.5 whereas the contribution from the acidic components is
51% for PM10 and 49% from PM2.5.
It is very difficult to compare our results with the other studies as present study was
only concise to monsoon season. Therefore, the present study was compared only for
PM10 with Chhatisgarh and Agra studies where they have reported monsoon ionic
concentrations (Table 2). As depicted in the table present concentrations are found in
between the Chhatisgarh and Agra concentration, i.e., ionic concentrations of PM10 are
higher than Chhatisgarh and lower than Agra.
Table 2 Ionic concentration (μg m–3) of PM in Pune along with other Indian studies (monsoon
season)

Pune Chhattisgarh Agra

PM2.5 PM10 PM10 PM10
Mean ± SD (range) Mean ± SD (range) Mean ± SD (range) Mean
Cl– 1.59 ± 2.36 2.19 ± 0.66 0.5 ± 0.8 3.6
(0.27–6.72) (1.41–2.90) (0.02–1.8)
SO42– 1.91 ± 2.63 3.24 ± 1.29 2.8 ± 1.8 5.3
(0.43–6.98) (1.87–5.17) (1.3–6.0)
NO3– 0.2 ± 0.31 1.14 ± 0.23 0.8 ± 1.1 3.6
(0.01–0.82) (0.86–1.45) (0.03–2.6)
Na+ 1.08 ± 1.48 1.86 ± 0.51 0.5 ± 0.2 3.08
(0.20–4.22) (1.25–2.45) (0.3–0.8)
K+ 0.41 ± 1.05 0.45 ± 0.03 0.3 ± 0.3 1.75
(0.11–1.81) (0.40–0.50) (0.1–1.0)
Mg2+ 0.29 ± 0.40 0.53 ± 0.11 0.2 ± 0.1 0.24
(0.05–1.15) (0.37–0.66) (0.1–0.3)
Ca2+ 1.48 ± 2.27 2.41 ± 0.66 2.0 ± 0.7 1.86
(0.15–5.61) (1.62–3.33) (1.3–3.6)
NH4+ 0.69 ± 0.37 1.35 ± 0.56 1.0 ± 0.5 5.35
(0.14–1.31) (0.68–2.12) (0.4–1.9)
Reference Present study Deshmukh et al. Singh et al.
(2012) (2010)

3.1 Impact of sea salt and soil derived particles on PM10 and PM2.5
The ionic constituents such as SO42–, K+, Ca2+ and Mg2+ are derived from either marine or
non-marine origins, such as anthropogenic and soil emissions. In order to determine
marine influence on the composition of PM, sea salt ratios (i.e., Cl–/Na+, SO42–/Na+,
Mg2+/Na+, K+/Na+ and Ca2+/Na+) were calculated using Na as a reference element
assuming all Na from marine origin (Safai et al., 2010). The ratios are given in Table 3. It
206 S. Yadav and P.G. Satsangi

is evident from the Table 3, that the ratios of K+/Na+, Ca2+/Na+, Mg2+/Na+ and SO42–/Na+
are higher than those of sea water, whereas the Cl–/Na+ ratio is lower than in sea water.
Higher ratios indicate incorporation of non-marine constituents in PM. Lower ratio of
Cl–/Na+, indicates modifications/reaction of sea salt components by non-marine
constituents. PM composition may be affected by natural sources, like soil crust. To
investigate the contribution of these sources on PM, Ca2+ was chosen as a reference
element due to its abundance in the local soil (Parmar et al., 2001). The concentration of
ions and ratios of various ions with respect to Ca2+ in soil is shown in the Table 4. It is
found that ratios of Na+/Ca2+, NO3–/Ca2+, and SO42–/Ca2+ in PM10 and Na+/Ca2+ and
SO42–/Ca2+ in PM2.5 are higher than in soil ratio, whereas Cl–/Ca2+ and K+/Ca2+ ratios
were lower. This indicates that Na+, NO3– and SO42– in PM10 and Na+ and SO42– in PM2.5
are contributed from other sources than soil. To differentiate the influence of soil and
other sources, excess concentration of SO42–, NO3–, Na+, K+ and Mg2+ relative to soil was
calculated as follows:

SO 4excess = [SO 4 2 − ]PM − 0.99 [ CA 2 + ]PM (SO4 / CA in soil = 0.99 ) (1)

Mg excess = [ Mg 2 + ]PM − 0.63[ CA 2 + ]PM (Mg / Ca in soil = 0.63) (2)

NO3excess = [ NO3− ]PM − 0.34 [ Ca 2 + ]PM ( NO3 / Ca in soil = 0.34 ) (3)

K excess = [ K + ]PM − 0.55 [ Ca 2 + ]PM (K / Ca in soil = 0.55) (4)

From the calculation, SO42– excess, for PM10 and PM2.5 was obtained about 25% and
NO3– was 28% for PM10, suggesting that it may be due to the reaction of gaseous SO2 and
HNO3 on soil particulate by heterogeneous reactions (Parmar et al., 2001).
Table 3 Ratio values of the water-soluble components of PM10 and PM2.5 and the
corresponding value for sea water

Cl–/Na+ K+/Na+ Ca2+/Na+ Mg2+/Na+ SO42–/Na+

PM10 1.17 ± 0.2 0.24 ± 0.06 1.30 ± 0.24 0.28 ± 0.02 1.74 ± 3.3
PM2.5 1.48 ± 0.69 0.38 ± 0.18 1.34 ± 0.30 0.27 ± 0.11 1.77 ± 1.3
Sea water 1.8 0.037 0.038 0.12 0.25

Table 4 Ratio values of the water-soluble components of PM10 and PM2.5 and the
corresponding value for soil

Na+/Ca2+ NO3–/Ca2+ Cl–/Ca2+ SO42–/Ca2+ K+/Ca2+ Mg2+/Ca2+

PM10 0.76 ± 0.32 0.46 ± 0.02 0.90 ± 0.02 1.34 ± 0.16 0.18 ± 0.01 0.22 ± 0.03
PM2.5 0.74 ± 0.52 0.13 ± 0.1 1.10 ± 0.1 1.32 ± 0.38 0.28 ± 0.1 0.20 ± 0.05
Soil 0.68 0.34 4.1 0.99 0.55 0.63
 Chemical and morphological study of PM10 and PM2.5 in Pune, India 207

3.2 Correlations analysis and influence of meteorology

Correlation matrix is a common approach of hypothesising potential precursors of ions in

PM samples. Correlation between ions suggests the likely sources of pollutants and also
indicates the gaseous reactions occurring in the atmosphere. Meteorology plays a crucial
role in understanding the ambient distribution of air pollution. The pollutants reside in the
atmosphere and the formation of secondary pollutants are controlled not only by the rate
of emissions of the reaction into the air from the source but also by air temperature (T),
wind speed (WS), relative humidity (RH) and precipitation (RF) (Bhaskar and Mehta,
2010). The correlation coefficient (r) between ionic species and meteorological
parameters are shown in Table 5. The results showed that the meteorological parameters,
i.e., T, WS, RH and RF were negatively correlated with PM. Correlation coefficient
between temperature and PM are significantly negative which indicates that the higher
temperature would be against the accumulation of pollutants. Significant negative
correlation between mass concentration and WS showed a dominance of local sources in
which strong winds flush pollutants out of the system whereas weak wind allow the
pollution level to increase. Similar results have been reported by other studies (Bhaskar
and Mehta, 2010; Deshmukh et al., 2011). PM10 and PM2.5 show a significant negative
correlation with RH. Hien et al. (2002) also reported the same results and suggested that
RH remove atmospheric PM and diminish the amount of re-suspended soil dust by
making soil humid. The effect of rainfall on the concentration of PM and particle
associated water soluble ionic species was also examined. As depicted from Table 5,
precipitation is an important removal mechanism of pollutants from the atmosphere
(Budhavant et al., 2012). The results presented that the mass concentrations of PM10 and
PM2.5 were negatively correlated with rainfall.
The correlation between NO3– and SO42– with Ca2+, Mg2+ and NH4+ suggests that
acidity in PM is neutralised by these alkaline species (Table 5). NO3– and SO42– show
correlation in both PM2.5 and PM10 indicating their origin from similar sources. PM rich
with SO42–, NO3– and NH4+ are formed through the gas-to-particle conversion processes
in which the respective precursor gases for these PM, i.e., SO2 and NO2 get oxidised
when reacted with water vapour in the atmosphere. NH4 is formed from reduction of its
precursor ammonia gas (NH3). These precursor gases are emitted from various
anthropogenic sources (Seinfeld and Pandis, 1998; Safai et al., 2010) viz. emissions from
vehicular as well as from chemical laboratory or may be associated with Ca2+, Mg2+ and
Na+ after the neutralisation process. Fine fraction of NO3– is generally in the form of
NH4NO3 but its coarse fraction is present in the form of CaNO3 or NaNO3 through the
reaction of HNO3 vapours with soil and sea originated elements, respectively (Pitts and
Pitts, 2000). Coarse form of NO3– at Pune is also reported by Safai et al. (2005). These
facts are corroborated by significant correlation between Ca2+ and SO42–, Ca2+ and NO3–,
Mg2+ and SO42–, Mg2+ and NO3–, Na+ and SO42–, Na+ and NO3– in PM2.5 and Ca2+ and
SO42–, Ca2+ and NO3– and Na+ and NO3– in PM10. Ca2+ and Mg2+ which are essential
components of soil having good correlation with each other, implying a common origin.
 208

Table 5

PM2.5 Na+ K+ Ca2+ Mg2+ NH4+ SO42– NO3– Cl– Temp WS RH RF

PM10 1 0.01 0.51* 0.05 0.10 0.51* 0.60** 0.55* 0.41* –0.57* –0.62** –0.50* –0.66**
Na+ 0.02 1 0.81** 0.84** 0.91** 0.23 0.30 0.51* 0.99** 0.10 0.04 0.04 0.06
K+ 0.58* 0.97** 1 0.59* 0.71* 0.11 0.17 0.67* 0.75* –0.01 –0.08 –0.10 –0.04
Ca2+ 0.02 0.99** 0.99** 1 0.92** 0.71* 0.96** 0.80** 0.88** –0.01 –0.02 –0.03 0.03
S. Yadav and P.G. Satsangi

2+
Mg 0.08 0.95** 0.96** 0.62* 1 0.60* 0.65* 0.80** 0.94** –0.02 0.03 –0.09 –0.01
NH4+ 0.45* –0.30 –0.19 –0.22 –0.18 1 0.99** 0.74* 0.30 –0.01 –0.56* 0.48* –0.25
SO42– 0.63** 0.96** 0.89** 0.99** 0.94** 0.23 1 0.74* 0.37 0.09 –0.52* 0.55* 0.10
NO3– 0.56* 0.57 * 0.63* 0.77* 0.56* –0.42* 0.68** 1 0.63** 0.02 –0.49* 0.46* 0.08
–
Cl 0.48* 0.95** 0.99** 0.97** 0.96** –0.18 0.89** 0.60* 1 –0.01 –0.06 –0.02 0.09
Temp –0.62** 0.16 –0.16 –0.04 0.02 –0.12 0.10 0.09 0.02 1 –0.50* –0.30 –0.12
WS –0.56* 0.07 –0.12 –0.04 0.10 –0.49* –0.56* –0.51* –0.07 1 0.02 –0.20
RH –0.45* 0.02 –0.08 –0.01 –0.11 0.45* 0.59* 0.41* 0.02 –0.30 0.02 1 0.01
RF –0.55* 0.02 –0.02 0.02 0.02 –0.01 0.20 0.04 0.08 –0.15 –0.20 0.03 1
Notes: **Correlation is significant at the 0.01 level (2 tailed).
*Correlation is significant at the 0.05 level (2 tailed).
of PM2.5 (lower diagonal triangle) and PM10 (upper diagonal triangle) in Pune
Correlation analysis between PM, ionic concentration and meteorological parameters
 Chemical and morphological study of PM10 and PM2.5 in Pune, India 209

3.3 Relation of NH4 with NO3 and non-sea salt SO4 (nssSO4)
Ammonia emitted by decay and decomposition reacts with acidic gases like sulphuric and
nitric acid in the air forming ammonium salts. Ammonia is not transported to very long
distances as it rapidly converts into NH4 PM at the rate of 30% per hour (Asman and
Van Jaarsveld, 1991). Many studies performed at different places have pointed out that
this cation accumulates in the fine particle ranges and correlates well with sulphate,
suggesting that ammonium sulphate as the major ammonium salt (Wang et al., 2003; Wu
et al., 2006; Safai et al., 2010; Khemani et al., 1982). For calculating the different ratios,
non-sea salt (nss) fraction of particular ionic component was computed. For example, nss
SO42– is computed as:

nss SO 4 = [SO 4 2 − ] − [see salt fraction of SO 4 ] (5)

Computation of nss is essential for examination of acidic and alkaline nature and
neutralisation potential of components of PM. The average equivalent ratio of NH4 to
nssSO4 (NH4/nssSO4) was 2 and 1.12 for PM2.5 and PM10, respectively. The average
equivalent ratio of NH4+ to sum of nssSO4 and NO3 (NH4/nssSO4+NO3) was 1.86 and
0.86 for PM2.5 and PM10, respectively. These ratios suggest that NH3 neutralised H2SO4
and HNO3 almost completely and NH4 containing particles at this site could exist as
(NH4)2SO4 and NH4NO3.

3.4 Neutralisation of acidic components and alkalinity of PM

Relative importance of the acid neutralising capacity of different cations was estimated
by calculating neutralisation factor (NF) with regard to the particular cation (Safai et al.,
2010). It is known that NO3– and SO42– are the major acid producing anions in the
atmosphere, whereas Ca2+, NH4+, Mg2+ and K+ are major acid neutralising cations. Some
of the cations like Ca2+ and Mg2+ and anions like SO42– are measured over land partially
originated from soil in the form of neutral salt and partially from the anthropogenic
activity (Kulshrestha et al., 2009). In acid NF of a cation, only those ions are considered
which originate over land, i.e., non-sea salt components namely nssCa2+, nssMg2+, nssK+
and nssSO42-. Non-sea salt component of an anion obtained in water soluble particulate
sample was computed using the formula given by Parashar et al. (1996). The formula
used for calculating NF of a cation is given as:
⎛ Ca ⎞
NF(Ca) = nss ⎜ ⎟ + nss SO 4 (6)
⎝ NO3 ⎠

⎛ NH 4 ⎞
NF ( NH 4 ) = nss ⎜ ⎟ + nss SO 4 (7)
⎝ NO3 ⎠

⎛ Mg ⎞
NF(Mg) = nss ⎜ ⎟ + nss SO 4 (8)
⎝ NO3 ⎠

⎛ K ⎞
NF(K) = nss ⎜ ⎟ + nss SO 4 (9)
⎝ NO3 ⎠
210 S. Yadav and P.G. Satsangi

It is observed from Figure 3 that NF of Ca2+ is higher in PM10 followed by NH4+, Mg2+
and K+ while in the PM2.5 NF is observed for NH4+ followed by Ca2+, Mg2+ and K+.
Quantification of particulate alkalinity (PA) would indicate the buffering capacity of
acidic components. PA has been calculated as

PA = [ Ca 2 + ] + [ Mg 2 + ] + [ Na + ] + [ K + ] + [ NH 4 + ] − [SO 4 2 − ] − [ NO3− ] − [ Cl− ]

(10)
(all concentrations are in equivalent)

and it is found to be 90 neq m–3 for PM10 and 100 neq m–3 for PM2.5. This indicates that
PMs are in alkaline in nature. The alkalinity of PM10 is due to soil derived alkaline
components Ca2+, Mg2+ and Na+, while the alkalinity of PM2.5 is due to neutralisation of
acidity by NH3 as results shown in the NFs (Figure 3).

Figure 3 NFs for PM10 and PM2.5 (see online version for colours)

2.5 PM2.5
PM10
2

1.5

0.5

0
NFCa NFNH4 NFK NFMg

3.5 Characteristic of PM2.5 by SEM-EDS

Atmospheric PM was analysed by scanning electron microscope coupled with

energy-dispersive spectrometer (SEM-EDS) analysis with the aim to identify their origin.
A total of 236 particles were analysed. Classification of the present particles was based
on the morphology and chemical composition of particles, typically expressed in terms of
EDS. According to their morphology two main particle categories were observed (i.e.,
natural and anthropogenic). The abundance of the natural and anthropogenic particles
was found to be ~64% and ~36%, respectively. Slezakova et al. (2008) also studied the
morphology of PM2.5 particles at two sites; traffic and background sites of Portugal. They
 Chemical and morphological study of PM10 and PM2.5 in Pune, India 211

have reported that at traffic site, particles were originated as 25% natural, 67% traffic and
8% anthropogenic whereas in background site; 82% natural, 18% traffic and < 1%
anthropogenic. Our data is within the range of data reported from background and traffic
sites of Portugal as the present site is semi urban site of Pune. In present study, most
abundant groups observed were soot (16%), sulphates (8%), Si-rich particles (56%),
metal-rich (4%), oxide (10%), carbonates (5%) and biological particles (3%). The
SEM photomicrographs of some characteristic particles are shown in Figure 4(a).
Soot is present as agglomerates of many fine spherical primary particles [Figure 4(b)].
This kind of aggregate has an irregular morphology of various shapes. Soot particles
are primarily emitted from burning and incomplete combustion of fossil fuels from
vehicular emissions. Li et al. (2011) found the S-rich soot particles and suggested
that soot particles from vehicular emissions underwent aging processes during the
transport. In the present study, C-rich particles are present in substantial percentage
(by EDS data) along with the amount of S, mainly produced from the vehicular traffic as
well as from the reactions occurring in the chemical laboratory. Aggregates of soot
and S are often observed in SEM analysis. This finding is also consistent with the
Paoletti et al. (2003), who suggested that the S content on soot aggregate is probably the
result from gas-to particle conversion in the atmosphere. Such particles are constituted of
large number – hundreds of thousands of aggregates of carbonaceous microsferules
having the irregular morphology almost spherical to a long small chain (Li et al.,
2011; Paoletti et al., 2003). Furthermore, the surface of carbonaceous particles acts as a
catalyst for SO2 photochemical oxidation producing ammonium [i.e., (NH4)2SO4] and
alkaline metal sulphates. The EDS analysis show traces of S and sometimes of Na
and K. The most of naturally occurring silica particles (probably Si oxides) and
aluminosilicates (containing Al, Si, K, Fe, and Ca) present in the PM have irregular
forms (~ 50%) and originate from soil whereas spherical aluminosilicates that dominate
in the size fraction below 1 μm are anthropogenic (6%) (Chen et al., 2006). This smooth
particle could be a fly ash. Fly ash is the by-product of coal burning, contains mostly
aluminosilicates (Chang et al., 1999). Similarly, high abundance of aluminium silicate
(67%) which originates from natural sources at background site of Portugal has also been
reported by Slezakova et al. (2008). Ca/Mg carbonate particles have also been observed
in PM samples and are assumed to be soil related (i.e., natural origin). Ca2+ originates as
carbonates (CaCO3) and sulphates (CaSO4.2H2O) from soil while Mg is present in the
sufficient amount in soil as dolomite [CaMg(CO3)2] (Kulshrestha et al., 2009). These
alkaline particles could absorb the acidic gases (i.e., SO2 and NO2) and help to reduce the
acidity of PM. Biological particles were different from other particles according to their
composition and morphology. Such biological particles are attributed to the likely
presence of pollens, spores, algae, fragments of leaves and the excrements and fragments
of insects (Cong et al., 2010). Thus, results of SEM revealed that PM2.5 was composed of
soot aggregates, sulphates, bio-particles, minerals (calcium silicates and Mg silicates) and
carbonates. These results can also be in accordance with the results indicated by the ionic
composition.
212 S. Yadav and P.G. Satsangi

Figure 4 (a) SEM micrographs and EDS of particulate matter (b) SEM micrographs and EDS of
particulate matter (see online version for colours)

(a)

(b)
 Chemical and morphological study of PM10 and PM2.5 in Pune, India 213

4 Conclusions

The average concentration of PM10 and PM2.5 was found to be 16.69 ± 5.6 µg m–3 and
11.68 ± 4.1 µg m-3, respectively. In both PM2.5 and PM10, higher concentrations were
shown by SO42– followed by Cl– > Ca2+ > Na+ > K+ > NH4+ > Mg2+ > NO3– for PM2.5 and
Ca2+ > Cl– > Na+ > NH4+ > NO3– > Mg2+ > K+ for PM10. Higher ratios of K+/Na+,
Ca2+/Na+, Mg2+/Na+ and SO42–/Na+ indicate incorporation of non-marine constituents in
PM. Lower ratio of Cl–/Na+, indicates fractionation of sea salt or modifications/reaction
of sea salt components by non-marine constituents. SO42– excess, for PM10 and PM2.5 was
found to be about 25% and NO3 was 30% for PM10. NF of Ca2+ was higher in PM10
followed by NH4+, Mg2+ and K+ whereas in PM2.5 higher NF was observed for NH4+
followed by Ca2+, Mg2+ and K+. PA has also been calculated and found to be 90 neq m–3
for PM10 and 100 neq m–3 for PM2.5. The alkalinity of PM10 is due to higher concentration
of soil derived alkaline components Ca2+, Mg2+ and Na+, while the alkalinity of PM2.5 is
due to neutralisation of acidity by NH3. According to particle’s morphology two main
particle categories were observed; natural and anthropogenic with the abundance of
~64% and ~36%, respectively. The most abundant groups observed were soot (16%),
sulphates (8%), Si-rich particles (56%), metal-rich (4%), oxide (10%), carbonates (5%)
and biological particles (3%). Thus, SEM results are in accordance with ionic
composition of PM.

Acknowledgements

Authors would like to thank BCUD, University of Pune and DST, New Delhi
SR/FTP/ES-91/2009 for financial support during this work. Authors are also thankful to
the Head of the Department of Chemistry, University of Pune for providing all necessary
facilities required during the study of this project.

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