Journal of Environmental Management 319 (2022) 115749

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Journal of Environmental Management

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

Research article

Evaluation of organic aerosol filter sampling artefacts and implications to

gravimetric PM2.5 mass at a COALESCE network site - Bhopal, India
Ankur Bhardwaj, Ramya Sunder Raman *
Department of Earth and Environmental Sciences, Indian Institute of Science Education and Research Bhopal, Bhopal By-pass Road, Bhauri, Bhopal, 462066, Madhya
Pradesh, India

A R T I C L E I N F O A B S T R A C T

Keywords: Filter based PM2.5 samples are typically used to measure its chemical constituents. Such measurements are made
PM2.5 filter samples in dense sampling networks to assess regulatory compliance and for source apportionment. Thus, quantifying
Bhopal sampling artefacts is crucial. In this study, 24-h integrated PM2.5 samples collected over Bhopal, India a COA­
India
LESCE (CarbOnaceous AerosoL Emissions, Source apportionment and ClimatE impacts) site during 2019 and
Organic sampling artefacts
2020, were used to estimate particulate organic carbon (OC) artefacts. Total OC and its thermal fractions (OC1,
Quartz behind teflon (QbT)
Quartz behind quartz (QbQ) OC2, OC3, and OC4) measured on 349 bare quartz (Q) and QbQ filters each, were used to determine OC positive
PM2.5 volatilization artefacts on quartz filters. 50 QbT (Quartz behind Teflon) filters in conjunction with the simultaneous QbQ
samples (a subset of the total QbQ) were used to estimate OC volatilization from Teflon filters. On average,
adsorbed gaseous OC contributed 17% and 11% to the measured total OC during 2019 and 2020, respectively.
Further, the volatilization loss of organics from Teflon filter (used to quantify PM2.5 mass) ranged between 7%
and 9%, and 5% and 6% of the PM2.5 mass during 2019 and 2020, respectively. The results of this study provide
the first systematic long-term evaluation of thermal carbon fraction-wise sampling artefacts, estimates of organic
volatilization losses from Teflon filters and their implications to PM2.5 mass closure, over a regionally repre­
sentative location in India.

1. Introduction integrated (24 h) PM2.5 concentrations. Near real-time PM2.5 monitors

Ambient fine particulate matter (PM2.5) is a mixture of carbonaceous
components, water-soluble inorganic ions, and trace elements which
arise from natural and anthropogenic sources (Cheng et al., 2012; U.S.
EPA, 1996). PM2.5 is known to have adverse effects on human health, air
quality, and climate (Pope and Dockery, 2006). However, data on
physico-chemical characteristics of PM2.5 across locations in the world
are unevenly distributed (Chen et al., 2022; Cheng et al., 2016). In India,
PM2.5 was included in the National Ambient Air Quality Standards
(NAAQS) in 2009 and monitoring efforts have been ramped up in the
last decade. Filter-based measurements (e.g., National Ambient Air
Monitoring Programme, NAMP) and continuous PM2.5 monitors (e.g.,
Continuous Automatic Air Quality Monitoring Stations, CAAQMS) now
provide measurements to assess regulatory compliance (Pant et al.,
2018). A more recent National Clean Air Programme (NCAP) proposes to
use a combination of time-integrated and real-time PM2.5 measurements
(Ganguly et al., 2020).
Filter-based measurements are manual, typically providing time-
using optical attenuation to estimate mass concentrations (e.g., Watson
et al., 1998) and other methods to measure chemical constituents are
now available. However, these are prohibitively expensive for deploy­
ment on a routine basis in dense networks (Brauer et al., 2019).
Therefore, filter-based sampling in routine monitoring networks will
continue to be important for PM2.5 mass and its chemical constituent
measurements, for assessing regulatory compliance and for source
apportionment.
Chemical constituents measured to explain PM2.5 mass (gravimetri­
cally measured on Teflon filters) generally include: (i) water-soluble
inorganic anions and cations (usually measured by ion chromatog­
raphy on Nylon filter leachates); (ii) elements (typically measured by
Energy Dispersive X Ray Fluorescence, EDXRF on Teflon filters); and (iii)
thermal fractions of organic carbon (OC) and elemental carbon (EC) (by
thermal/optical carbon analysis on quartz filters typically using NIOSH
or IMPROVE_A methods) (Birch and Cary, 1996; Chow et al., 1993,
2007). Ideally, the sum of these chemical components (accounting for
the compounds they are likely to be present as) should be close the

* Corresponding author.
E-mail address: ramyasr@iiserb.ac.in (R. Sunder Raman).

https://doi.org/10.1016/j.jenvman.2022.115749
Received 20 January 2022; Received in revised form 14 June 2022; Accepted 10 July 2022
Available online 21 July 2022
0301-4797/© 2022 Elsevier Ltd. All rights reserved.
A. Bhardwaj and R. Sunder Raman
gravimetric mass. However, several studies over India show that often
gravimetric PM2.5 mass is lower than the reconstructed mass from
chemical species because of particulate nitrate volatilization and/or
organics volatilization from Teflon filters, which are used for gravimetry
(e.g., Jaiprakash and Habib, 2017; Kumar and Sunder Raman, 2020;
Pipalatkar et al., 2014). Difficulties in achieving and maintaining the
required temperature and relative humidity to equilibrate filters and
de-water PM2.5 prior to gravimetry and the choice of OC to organic
matter (OM) conversion factors are other reasons for inadequate mass
closure.
Organic sampling artefacts include the adsorption of volatile and
semi-volatile organic compounds (VOCs and SVOCs) onto filters and/or
volatilization of particulate organics from the filter, resulting in over­
estimation and/or underestimation of particulate OC (Malm et al., 1994;
Subramanian et al., 2004; Turpin et al., 2000), respectively. Thus, an
assessment of organic artefacts is essential to better quantify their role in
PM2.5 mass closure and to ensure that reported concentrations of OC, are
in fact reasonably close to the ambient OC. Some PM2.5 monitoring
networks across India, such as the NAMP monitor PM2.5 and other gases
(e.g., SO2, NO2), but do not focus on organics filter volatilization and
adsorption artefacts (Pant et al., 2018). Filter-based routine monitoring
networks across the globe (e.g., CSN - Chemical Speciation Network,
IMPROVE - Interagency Monitoring of Protected Visual Environments)
account for organic-artefacts (Watson et al., 2009) but over Indian lo­
cations such systematic or long-term measurements to support and guide
corrections for filter based measurements are scarce.
The pan-India COALESCE (Carbonaceous Aerosol Emissions, Source
Apportionment and Climate Impacts) project (Venkataraman et al.,
2020) uses filter based sampling at 11 locations. In this study, we utilize
over 349 Q (bare quartz) and QbQ (Quartz behind Quartz) filters each
and 50 QbT (Quartz behind Teflon) samples collected during a two-year
field campaign (2019 and 2020) at Bhopal, a COALESCE site (Lekinwala
et al., 2020). We report the estimates and implications of the temporally
varying organics adsorption and volatilization artefacts on measured OC
and gravimetrically measured PM2.5 mass.
2. Materials and methods
2.1. Site information and sample collection
The Bhopal COALESCE site is located in Madhya Pradesh, Central
India (Lekinwala et al., 2020; Venkataraman et al., 2020). Time inte­
grated (24 h) ambient PM2.5 samples were collected every-other-day for
two years (2019–2020) on a hillock (~560 m above ground level) in the
Indian Institute of Science Education and Research (IISER) Bhopal
campus (23.28◦ N, 77.28◦ E). Field blanks (FB) and QbT samples were
collected twice a month (every-15th-day) from January 01, 2019, to
December 31, 2020. In accordance with the Indian Meteorological
Department (IMD) guidelines, the annual sampling period was divided
into four seasons: (i) Winter: Jan and Feb (JF); (ii) Pre-monsoon: Mar,
Apr, and May (MAM); (iii) Monsoon: Jun, Jul, Aug, and Sep (JJAS); and
(iv) Post-monsoon: Oct, Nov, and Dec (OND). Onsite ambient air tem­
perature was recorded using the MetOne AIO2 weather sensor with a
time resolution of 1 min. This study was part of a multi-institutional
project carried out at eleven sites across India. Comprehensive details
about the sampling sites and sampling methods were previously re­
ported (Lekinwala et al., 2020; Venkataraman et al., 2020). Brief
description of the SASS® sampler (Supplemental Text S1), sampler
configuration (Supplemental Fig. S1), and number of samples collected
(Supplemental Table S1) are included in supplemental information.
2.2. Carbonaceous fraction measurements
Pre-fired quartz filters (from a single lot for all front and back up
filters) were used for particulate OC measurements to ensure compati­
bility with thermal evolution methods to determine OC/EC (Birch and
2
Journal of Environmental Management 319 (2022) 115749
Cary, 1996; Chow et al., 1993). Aliquots (punches 0.5 cm2) of quartz
fiber filters were analyzed using the DRI model 2015 multi-wavelength
thermal-optical carbon analyzer at 7-wavelengths (405 nm, 445 nm,
532 nm, 680 nm, 780 nm, 808 nm, and 980 nm). The IMPROVE-A
protocol was used for this analysis (Supplemental Table S2). This pro­
tocol is different from the NIOSH protocol (Supplemental Table S2) not
only in time-temperature steps but also in the fact that IMPROVE_A
method is slope driven (laser reflectance signals going back to baseline)
while NIOSH method is time dependent (fixed time duration during each
OC/EC fraction analysis). These operational differences mean that while
the total carbon (TC, the sum of total OC and total EC) by either one of
these methods should ideally be identical, their thermal carbon fractions
(OC1, OC2, OC3, OC4, OP, EC1, EC2, EC3) are likely to be different.
Details of the instrument, analysis protocols, and quality assurance and
quality control are available elsewhere (Bautista et al., 2015; Birch and
Cary, 1996; Chen et al., 2015; Chow et al., 2007). It is pertinent to note
that our study focuses on the effect of gaseous adsorption and volatili­
zation losses on carbon fractions. Therefore, protocol selection is an
important consideration for carbon fractionation measurements. In this
study, we used IMPROVE_A method with OP correction using 635 nm
optical reflectance signal instead of the NIOSH method. This method
was chosen because it is the most widely used method for carbon frac­
tionation studies across the globe since it does not move on to the next
temperature step without the laser reflectance signal going back to
baseline (slope driven method) unlike the NIOSH method where time
steps are too fast for laser signal to return to the baseline when it shifts to
next temperature step (time-dependent). NIOSH analysis often results in
inaccurate OC-EC split (Bautista et al., 2015; Chow et al., 2001).
IMPROVE_A method uses laser reflectance signals for pyrolysis correc­
tion because reflectance is more influenced by near-surface char (where
~80% of sample deposit is located), which evolve first in He/O2 phase,
while NIOSH method uses laser transmittance signals for pyrolysis
correction which results in longer return-to-baseline laser signal times
(delay OC-EC split) because transmittance is affected by within-filter
char (Bautista et al., 2015; Chow et al., 2004). Hence, in general, the
IMPROVE_A method provides better OC and EC fractionation compared
to the NIOSH method.
In this study, the method detection limit (MDL) was calculated as
three times the standard deviation (Chow et al., 2007) of measured total
OC (TOC) and total EC (TEC) from 90 lab blanks (LB) sample. TOC was
calculated as sum of four OC fractions and OP fraction
(OC1+OC2+OC3+OC4+OP), while TEC was calculated as sum of three
EC fractions and subtraction of OP fraction from EC1 (EC1-OP +
EC2+EC3). A MDL value of 0.50 μg cm− 2 was obtained for TOC while
TEC MDL was 0.22 μg cm− 2. The method detection limits for various
thermal carbon fractions measured in this study are summarized in
Supplemental Table S2. In all, 748 samples (349 bare quartz (Q), 349
QbQ, and 50 QbT) were analyzed by the IMPROVE_A method in this
study.
2.3. Determining the organic carbon artefacts and estimating associated
organic matter
As previously described, in this study samples were collected in the
QbQ and QbT configurations (Supplemental Fig. S2). Denuder for
organic gases coupled with back-up filter based approaches for deter­
mining organic carbon artefacts are also reported in literature. For
example, Kirchstetter et al. (2001) found that the denuded particulate
OC was slightly higher than the QbT or QbQ corrected bare quartz
particulate OC. The higher particulate OC in the denuded sample was
attributed to denuder breakthrough. There were also other issues with
denuder sampler operation including, (1) contamination of the sample
by the denuder due to shedding of the denuder material (activated
carbon) (Subramanian et al., 2010), (2) efficiency for removing gaseous
organics decreasing with time (Swartz et al., 2003) (3) material and
human resources costs to coat these denuders at on-site laboratory
A. Bhardwaj and R. Sunder Raman
(Swartz et al., 2003), and (4) potential for disturbing ambient
gas-particle equilibrium given the wide range of diffusivities of specific
organics handled using a single denuder. Thus, in this study we choose
the QbT and QbQ approach to obtain estimates of organic artefacts.
In the QbT filter configuration it was assumed that because of its
material properties, the Teflon filter only captures particulate matter
without adsorbing organic gases. However, literature suggests that
Teflon filter can adsorb specific organic compounds (Levoglucosan and
Mannose) onto particles already collected on the filter (Parshintsev
et al., 2011). In this work, we assume that the contribution of such
adsorption to the Teflon OC positive artefact is negligible. In other
words, although the particle layer on Teflon filter may act as an adsor­
bent for some gas-phase organics, it is well established that the quartz
filters retain gaseous organics, ambient particulate organics, and the
volatilized particulate organics (during sampling), much better than the
Teflon filters (Cheng et al., 2009; Chow et al., 2010; Parshintsev et al.,
2011; Subramanian et al., 2010; Turpin et al., 1994). Overall, it is
reasonable to assume that the QbT filter is exposed to the same con­
centration of organic vapors as the bare quartz filter (Q) (Turpin et al.,
1994; Watson et al., 2009). Further, both the bare quartz and Teflon
filters are also exposed to the same particulate OC and EC. Thus, in the
QbQ filter configuration, it is assumed that volatilized particulate OC on
the bare quartz filter is retained on it, unlike the Teflon filter (Cheng
et al., 2009, 2010; Chow et al., 2010; Subramanian et al., 2010; Turpin
et al., 1994).
OC from gas adsorption on QbQ was calculated assuming that no
volatilized OC from bare quartz filter was collected on it (Cheng et al.,
2010; Chow et al., 2010; Subramanian et al., 2010). Thus, TOCQ -
TOCQbQ is a measure of all particle OC on bare quartz and particle OC on
it that volatilized during sampling but was re-adsorbed (Eatough et al.,
2003; Subramanian et al., 2010). The positive artefact (i.e., adsorbed OC
on bare quartz) is then estimated as follows:
( )
% ​ Gaseous ​ OC ​ adsorbed ​ on ​ Quartz ​ filters ​ due ​ to ​ the ​ positive ​ artefact =
Based on all of the assumptions above and Teflon material proper­
ties, QbT captures the sum of adsorbed gas-phase organics and volatil­
ized particulate OC. Thus, percent volatilized particulate OC from the
Teflon filter was calculated (Kuwabara et al., 2016) as follows:
( )
TOCQbT − TOCQbQ
% ​ Particle ​ TOC ​ lost ​ from ​ Teflon ​ filters = ∗100
TOCQ − TOCQbQ
(2)
Here TOCQbT – TOCQbQ represents volatilized particle OC captured
by QbT filter. The quantification of OC volatilization from Teflon filters
has implications to gravimetric PM2.5 mass closure, as OC is directly
related to organic matter (OM) (Aiken et al., 2008). To account for the
atoms other than C (Carbon) present in OC, OC is multiplied with a
suitable factor to estimate OM (Chow et al., 2015; Philip et al., 2014;
Turpin and Lim, 2001). Thus, % OM loss from Teflon filters (used for
gravimetry) was calculated as follows:
[ ]
f ∗ (TOCQbT − TOCQbQ )
% ​ OM ​ lost ​ from ​ Teflon ​ filters = *100 (3)
PM2.5
where, PM2.5 is the gravimetrically measured mass and f is the multi­
plication factor. In this study, likely OM loss was calculated by using low
(1.7), medium (1.9), and high (2.1) f-values. Although, f-values can vary
from 1.3 (for fresh aerosol in urban areas) to 2.6 (for highly aged
3
Journal of Environmental Management 319 (2022) 115749
aerosol) (Chow et al., 2015; Turpin and Lim, 2001), we used values near
2. This is so because lower f-values (1.3–1.6) are not representative of
highly oxygenated aerosols and are not likely for aerosols in locations
dominated by aged transported aerosols (El-Zanan et al., 2009; Philip
et al., 2014) with episodic local crop residue burning emissions, such as
the study site.
3. Results and discussion
3.1. PM2.5 mass and particulate OC concentrations
The annual PM2.5 mass concentrations varied from 3 μg m− 3 to 187
μg m− 3 during the study period (average: 52 ± 39 μg m− 3 during 2019
and 48 ± 30 μg m− 3 during 2020). The annual and seasonal PM2.5 mass
concentrations are shown in Supplemental Table S3. The average mass
fraction of adsorption corrected TOC was 16% ± 8% during 2019 and
15% ± 10% during 2020, respectively. By extension, OM (assuming
OM/OC = 1.9) (Philip et al., 2014) was 30% ± 15% during 2019 and
28% ± 19% during 2020, respectively. EC mass fraction was quite
similar during 2019 and 2020 with average values of 3% ± 3% and 2%
± 3%, respectively. A detailed examination of the temporal variability
and other characteristics of OC and EC concentrations are beyond the
scope of this study. However, for completeness, the summary-statistics
for each thermal fraction, TOC, and TEC for the entire study duration
(2019–2020) are shown in Tables 1 and 2. All values shown in these
tables are field blank, lab blank, and adsorption artefact corrected
values. Details of filed blank corrections are discussed in Supplemental
Text S2.
3.2. OC and EC in field blanks, lab blanks, and QbQ filters
Average TOC in the field blanks of bare quartz, back-up quartz
TOCQbQ
*100 (1)
TOCQ − TOCQbQ
behind quartz and back-up quartz behind Teflon filter (Q-FB, QbQ-FB,
and QbT-FB), lab blanks (LB), and QbQ filters during the sampling
period are shown in Fig. 1. Mean TOC Q-FB (0.65 ± 0.43 μg cm− 2 and
0.44 ± 0.32 μg cm− 2 during 2019 and 2020, respectively) was not sta­
tistically different from TOCQbQ (0.68 ± 0.47 μg cm− 2 and 0.51 ± 0.48
μg cm− 2 during 2019 and 2020, respectively). Comparable values of
TOC Q-FB and TOCQbQ reinforce the assumption that QbQ filters only
adsorb gaseous organics and that no volatilized OC was captured by
QbQ.
Further, as expected, mean QbQ-FB (0.39 ± 0.37 μg cm− 2 and 0.13
± 0.12 μg cm− 2 during 2019 and 2020, respectively) was lower than
mean Q-FB (0.65 ± 0.43 μg cm− 2 and 0.44 ± 0.32 μg cm− 2 during 2019
and 2020, respectively) because of higher exposure to passive gaseous
organics adsorption together with some passive deposition of particulate
OC compared to only gaseous adsorption on QbQ-FB (Dillner, 2016).
Also, TOC and TEC values were identical in simultaneously collected
QbQ-FB and QbT-FB filters (Table 3), indicating similar passive gaseous
adsorption on filters. The results observed in this study were similar to
the results reported in the IMCA (Improved Measurement of Carbona­
ceous Aerosols) project in Beijing (Cheng et al., 2009, 2010).
Average TEC Q-FB and TECQbQ were 0.01 ± 0.03 μg cm− 2 and 0.01
± 0.03 μg cm− 2 during 2019, respectively. TEC values were at or near
MDL (0.03 μg cm− 2) accounting for 0%–10% of the total carbon (TC),
indicating very little passive particulate matter deposition on filters. TEC
Q-FB and TECQbQ were below detection limits during 2020. As a result,
A. Bhardwaj and R. Sunder Raman Journal of Environmental Management 319 (2022) 115749

Table 1
Summary statistics of thermal fractions, TOC, TEC, and OP concentration on bare quartz samples (Q) collected during 2019.
Species Annual (unit: μg m− 3) Winter (JF) Pre- Monsoon (MAM) Monsoon (JJAS) Post- Monsoon (OND)

Min Max 25th percentile Median 75th percentile Avg ± SD Avg ± SD Avg ± SD Avg ± SD Avg ± SD

OC1 0.1 2.5 0.1 0.1 0.1 0.2 ± 0.4 0.3 ± 0.5 0.1 ± 0.1 0.1 ± 0.0 0.5 ± 0.6
OC2 0.1 16.4 0.8 1.5 3.0 2.2 ± 2.1 3.1 ± 2.9 1.5 ± 0.5 0.6 ± 0.3 4.0 ± 2.0
OC3 0.1 16.5 1.2 1.9 3.5 2.9 ± 2.7 3.4 ± 3.0 2.0 ± 0.7 1.0 ± 0.5 5.0 ± 3.0
OC4 0.1 10.4 0.3 0.7 1.9 1.7 ± 2.2 2.3 ± 2.4 0.9 ± 0.8 0.3 ± 0.2 3.6 ± 2.7
EC1 0.04 4.8 0.1 0.1 0.1 0.3 ± 0.8 0.2 ± 0.3 0.2 ± 0.4 0.1 ± 0.0 0.8 ± 1.3
EC2 0.05 32.3 0.8 2.0 4.4 3.0 ± 3.4 4.8 ± 5.6 2.1 ± 1.3 0.6 ± 0.4 5.2 ± 2.4
EC3 0.10 15.7 0.5 0.9 1.9 1.5 ± 1.8 2.8 ± 3.0 0.9 ± 0.5 0.3 ± 0.2 2.4 ± 1.5
TOC 0.1 66.8 3.7 6.2 13.0 9.7 ± 9.5 13.2 ± 11.8 6.1 ± 2.3 2.5 ± 1.2 17.9 ± 9.6
TEC 0.10 24.5 0.2 0.9 3.2 2.1 ± 3.0 3.5 ± 4.6 1.4 ± 1.6 0.3 ± 0.3 3.6 ± 2.8
OP 0.04 23.4 1.0 2.1 3.8 2.7 ± 2.6 4.2 ± 4.0 1.7 ± 0.9 0.7 ± 0.6 4.7 ± 1.9

Avg- Average; SD- Standard Deviation; Min- Minimum; Max- Maximum.

Table 2
Summary statistics of thermal fractions, TOC, TEC, and OP concentration on bare quartz samples (Q) collected during 2020.
Species Annual (unit: μg m− 3) Winter (JF) Pre Monsoon (MAM) Monsoon (JJAS) Post Monsoon (OND)

Min Max 25th percentile Median 75th percentile Avg ± SD Avg ± SD Avg ± SD Avg ± SD Avg ± SD

OC1 0.1 2.5 0.1 0.1 0.1 0.1 ± 0.3 0.1 ± 0.1 0.1 ± 0.3 0.1 ± 0.0 0.2 ± 0.5
OC2 0.1 9.2 0.5 1.6 2.9 2.0 ± 1.9 2.3 ± 0.8 2.1 ± 1.6 0.4 ± 0.5 3.8 ± 2.0
OC3 0.1 17.7 1.0 2.0 3.5 2.9 ± 2.9 2.6 ± 0.8 3.2 ± 2.4 0.9 ± 0.7 5.5 ± 3.9
OC4 0.1 13.8 0.3 0.8 2.0 1.7 ± 2.3 1.4 ± 0.8 1.6 ± 2.0 0.3 ± 0.4 3.9 ± 3.1
EC1 0.04 6.0 0.1 0.1 0.1 0.1 ± 0.6 0.1 ± 0.2 0.2 ± 0.7 0.1 ± 0.0 0.3 ± 0.9
EC2 0.05 9.9 0.6 1.8 3.9 2.4 ± 2.2 3.0 ± 1.3 2.5 ± 2.3 0.6 ± 0.7 4.4 ± 1.9
EC3 0.1 3.9 0.1 0.6 1.3 0.8 ± 0.9 1.6 ± 0.8 0.8 ± 0.8 0.1 ± 0.3 1.3 ± 0.8
TOC 0.1 43.1 2.3 6.4 12.1 8.47 ± 7.6 9.7 ± 3.2 8.5 ± 5.8 2.2 ± 2.3 16.0 ± 8.6
TEC 0.1 17.6 0.2 0.4 2.0 1.5 ± 2.6 1.4 ± 1.0 1.9 ± 3.7 0.1 ± 0.2 3.2 ± 2.6
OP 0.04 7.6 0.04 1.5 2.9 1.8 ± 1.6 3.4 ± 1.4 1.5 ± 1.1 0.6 ± 0.8 2.7 ± 1.5

Avg- Average; SD- Standard Deviation; Min- Minimum; Max- Maximum.

comparable and all the OC collected by QbQ filter can be assumed to be

Fig. 1. Annual TOC values of lab blanks (LB), field blanks (Q-FB and QbQ-FB),
and QbQ filters between January 1, 2019, and December 31, 2020. ‘Box’ is
outlined by the 25th and 75th percentile values while ‘whiskers’ indicate the
10th and 90th percentile values and dots show the 5th and 95th percentile
outliers. The median is represented by the solid line and mean by the dashed
line. With reference to the x-axis labels, N in parentheses shows number of
samples while “− 19” and “-20” refer to year 2019 and 2020, respectively.
total carbon (TC) and TOC were not statistically different in blanks and
QbQ filters. Descriptive statistics of blanks and QbQ filters are presented
in Table 3.
3.3. Organic artefacts
As discussed above, values of TOC Q-FB and TOCQbQ values were
gaseous organics passing through and in equilibrium with the front filter
adsorbed organics (Aiken et al., 2008), i.e., OC positive artefact.
Therefore, it is reasonable to use TOCQbQ to correct for the positive
artefact in the measured OC on bare quartz filters. The average annual
OC gas adsorption as a percentage of total particulate OC, as estimated
by Eq. (1), were 17% (0.9 μg m− 3) and 11% (0.6 μg m− 3) during 2019
and 2020, respectively (Supplemental Fig. S3).
The annual mean volatilized OC as a percentage of total particulate
OC that was likely re-captured by bare quartz (Subramanian et al., 2010)
but lost from Teflon filters were 27% (1.6 μg m− 3) and 21% (1.1 μg m− 3),
during 2019 and 2020, respectively. These values were comparable with
reports from Pennsylvania (Subramanian et al., 2010) and Beijing
(Cheng et al., 2010). The seasonal trend of total particle phase organic
carbon volatilization loss from Teflon filters during the sampling period
indicated that losses were high during the pre-monsoon season, on
average, 30% of particulate TOC during 2019 and 36% of particulate
TOC during 2020 (Fig. 2). High volatilization losses during the
pre-monsoon season likely occurred due to high ambient temperature
(mean: 30 ± 5 ◦ C; maximum: 43 ◦ C) and the presence of some
low-boiling organics (e.g., propane, butane, methyl chloride which
volatilize around 40 ◦ C–50 ◦ C) in thermal OC fractions, particularly in
the OC1 fraction (Grabowsky et al., 2011; Kuwabara et al., 2016 Turpin
et al., 1994). The value of OC1 fraction was negligible or zero in all
sample filters (Q, QbQ, and QbT) because it is very likely that all high
volatile organics and much of the semi-volatile organic compounds
(SVOCs) volatilized during sample collection and/or before the analysis
(Grabowsky et al., 2011).
On the other hand, volatilization losses were low during the winter
and post-monsoon seasons (Fig. 2), with averages of 16% and 20%
(2019) of total particulate OC and 11% and 12% (2020) of total par­
ticulate OC, respectively. These results support the hypothesis that low
ambient temperature enhances some organics binding-affinity to the
quartz filter (Kuwabara et al., 2016). During the monsoon seasons, the

4
A. Bhardwaj and R. Sunder Raman Journal of Environmental Management 319 (2022) 115749

Table 3
TOC and TEC comparison between lab blank (LB), bare (Q-FB) and back-up quartz field blanks (QbQ-FB), sample back-up quartz filters (QbQ), and simultaneously
collected backup quartz field blank (FB_QbQ & FB_QbT) during 2019 and 2020.
2019 2020 2019 2020 2019 2020 2019 2020 2019–2020

Species LB (N = LB (N = Q-FB (N = Q-FB (N = QbQ-FB (N = QbQ-FB (N = QbQ (N = QbQ (N = Simultaneous

60) 60) 26) 26) 26) 26) 166) 183) FB_QbT and
FB_QbQ (N = 10)

QbT- QbQ-
FB FB

TOC (μgC/ Minimum 0.00 0.00 0.13 0.02 0.00 0.00 0.00 0.00 0.04 0.04
cm2) 25th 0.09 0.06 0.31 0.27 0.19 0.05 0.33 0.17 0.07 0.07
percentile
Median 0.21 0.21 0.48 0.38 0.25 0.10 0.58 0.39 0.08 0.08
75th 0.33 0.34 0.87 0.53 0.42 0.19 0.84 0.69 0.10 0.10
percentile
Maximum 0.41 0.45 1.74 1.58 1.53 0.42 2.39 2.18 0.19 0.19
Average 0.20 0.19 0.65 0.44 0.39 0.13 0.68 0.51 0.09 0.09
Stdev 0.13 0.15 0.43 0.32 0.37 0.12 0.47 0.48 0.04 0.04

TEC (μgC/ Minimum 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
cm2) 25th 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
percentile
Median 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
75th 0.00 0.00 0.00 0.00 0.00 0.00 0.01 0.00 0.00 0.00
percentile
Maximum 0.05 0.16 0.12 0.00 0.07 0.00 0.18 0.04 0.00 0.00
Average 0.00 0.01 0.01 0.00 0.00 0.00 0.01 0.00 0.00 0.00
Stdev 0.01 0.02 0.03 0.00 0.01 0.00 0.03 0.00 0.00 0.00

Table 4
Estimated average volatilization loss from Teflon filters between 2019 and 2020.
Year Season % OC1 lossa %OC2 loss %OC3 loss %OC4 loss

2019 Winter 23 34 29 7
Pre-monsoon 0 52 33 23
Monsoon 0 42 50 16
Post-monsoon 0 32 33 8
2020 Winter 0 29 13 4
Pre-monsoon 0 52 46 59
Monsoon 0 10 31 5
Post-monsoon 0 17 20 7
(OC1 )
a QbT − OC1QbQ
% ​ OC1loss = ∗100
OC1Q − OC1QbQ

Fig. 2. Seasonal variation of the % TOC loss from Teflon filters with reference
to total particulate OC. Data are shown for the 50 samples collected during
2019 (upper panel) and 2020 (lower panel) (No samples were collected on
August 5, 2019, and August 19, 2019 due to power failure at the sampling site).
(Baudic et al., 2016; Lei and Wania, 2004). On four days during 2019
(Feb 18, Jul 8, Oct 28, and Sep 9) volatilization loss of OC2, OC3, and
OC4 fractions exceeded 90%. During 2020, on one day during the
pre-monsoon season (Mar 2) volatilization loss in OC4 fraction exceeded
90%. These filters were re-analyzed multiple times to over-rule analysis
artefacts. Thus, although the reason for these observations are not clear
in the absence of individual organic species measurements, one possible
explanation is the dominance of low molecular weight alkanes in OC on
these days (Kuwabara et al., 2016; Sihabut et al., 2005). Season-wise %
fractional OC volatilization losses are shown in Supplemental Figs. S4
and S5. It is relevant to note that OC1 was below detection limits on most
days.
Overall, as expected, fraction-wise % OC loss and % TOC loss
increased with ambient temperature (Fig. 3). Covariance between OC
(OC2, OC3, OC4, and TOC) and ambient temperature was in the range of
39–56 in 2019, while in 2020 it was 29–60. Positive values of covariance
indicated that OC volatilization losses from Teflon filters increased with
temperatures.

average volatilization losses were 36% (2019) and 20% (2020).

3.4. OC volatilization from Teflon filters and its implication to
Season-wise and thermal fraction-wise OC volatilization losses from the
gravimetrically measured PM2.5
Teflon filter are summarized in Table 4.
OC2 and OC3 losses during the monsoon seasons (Table 4) are likely
The quantification of OC volatilization has implications to PM2.5
due to the presence of certain VOCs that evaporate at room temperature
mass closure, as the loss of particle-phase SVOCs from the Teflon filter

5
A. Bhardwaj and R. Sunder Raman
Fig. 3. The average % loss of TOC and OC fractions (i.e.., volatilized OC from Teflon with reference to adsorption corrected total particulate OC) in (a) 24 samples
collected during 2019 (b) 26 samples collected during 2020. Error bars in these plots correspond to one standard deviation in the values.
Fig. 4. Percentage PM2.5 loss from Teflon filters during 2019 (upper panel) and
2020 (lower panel). Error bars correspond to f = 1.7 and f = 2.1, while the
triangles correspond to f = 1.9.
results in lower gravimetric PM2.5 mass than the ambient and that
reconstructed from its chemical constituents (Aiken et al., 2008; Gani
et al., 2019). OM is known to be a major constituent of PM2.5, estimated
at about 20–60% (Behera et al., 2011) across locations in India. Thus,
estimates of OM loss (Fig. 4) from Teflon filters can help better reconcile
gravimetric PM2.5 mass with that reconstructed from chemical species.
The 2009 NAAQS annual average PM2.5 standard is 40 μg m− 3. Thus,
PM2.5 over the study site was in NAAQS violation (Supplemental
Table S3). It follows that PM2.5 24 h NAAQS (60 μg m− 3) was also
6
Journal of Environmental Management 319 (2022) 115749
violated on several occasions. On accounting for volatilized OM lost
from Teflon filters (Supplemental Table S4), 24 h PM2.5 violations
increased by 5 days each during 2019 and 2020 (Supplemental
Table S5).
4. Summary and conclusions
Given that long-term PM2.5 surface monitoring networks are now
being established in India and other South-Asian countries for assessing
regulatory compliance and for source apportionment, it is essential to
develop a good understanding of filter sampling artefacts. In this study,
we utilize a robust two year-long dataset (every-other-day measure­
ments made during 2019 and 2020) from Bhopal, a COALESCE network
site, to assess organic adsorption and volatilization artefacts on Quartz
and Teflon filters, respectively. The average annual OC gas adsorption
was 17% and 11% (of the total particulate OC) during 2019 and 2020,
respectively while the annual mean volatilized OC lost from Teflon fil­
ters was 27% and 21% (of the total particulate OC) during 2019 and
2020, respectively. Seasonality in both adsorption and volatilization
artefacts of organics were observed. In general, though, OC2 and OC3
fractions contributed significantly to the positive adsorption artefact on
Quartz filters all-year-round, while OC1 and OC2 fractions were the
major contributors to the negative volatilization artefact from Teflon
filters all-year-round. It is pertinent to note that the results discussed in
this study, especially for various thermal carbon fractions, is applicable
for the operationally defined IMPROVE_A fractions. There may be some
differences in the magnitudes of these losses had the NIOSH protocol
been used for analysis.
Overall, the results from this study provide the first systematic long
term (two annual cycles) evaluation of fraction-wise OC sampling ar­
tefacts and estimates of OM volatilization losses from Teflon filters,
together with its implications to PM2.5 mass closure, over Bhopal, Cen­
tral India. Also, our work unequivocally shows that organic volatiliza­
tion artefacts from Teflon filters is likely to be substantial at most
locations in India, where temperatures exceed 30 ◦ C for most of the year,
and should be accounted in mass closure. This work provides a frame­
work for COALESCE network-wide organic artefact correction and
possible extension to other locations in the country, for gravimetric
PM2.5 mass corrections, even when OC is not measured.
Credit author statement
Ankur Bhardwaj: Methodology, sampling, chemical analyses, data
curation, formal analysis, visualization, validation, interpretation and
writing draft manuscript and revisions, Ramya Sunder Raman:
Conceptualization; validation and interpretation; writing - original draft
and editing; supervision; funding.
A. Bhardwaj and R. Sunder Raman
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
This work was supported by the Ministry of Environment, Forest, and
Climate Change (MoEF&CC), Government of India, under the NCAP-
COALESCE project {Grant No.14/10/2014-CC (Vol.II)}. The views
expressed in this document are solely those of authors and do not
necessarily reflect those of the Ministry. The Ministry does not endorse
any products or commercial services mentioned in this publication. The
authors thank the internal review committee of the NCAP-COALESCE
project for their comments and suggestions on this paper.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.jenvman.2022.115749.
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