Aerosol Sci Eng
DOI 10.1007/s41810-017-0010-4
REVIEW
Filter Processing and Gravimetric Analysis for Suspended
Particulate Matter Samples
1,2 • 1 •
John G. Watson Richard J. Tropp Steven D. Kohl
1,2
Judith C. Chow
Received: 30 June 2017 / Revised: 10 July 2017 /Accepted: 12 July 2017
Institute of Earth Environment, Chinese Academy Sciences 2017
Abstract Aerosol sampling onto filter media with labora-
tory weighing before and after drawing air through the
filter is the most commonly applied method to determine
PM 2.5 and PM 10concentrations. Although simple in con-
cept, determining the net gain in weight from an aerosol
deposit is complicated by adsorption of gases onto the
filter, retention of water by the filter and the deposit,
electrostatic charges that result in attraction of the filter to
balance surfaces, contamination during filter handling,
losses or additions to filter material, evaporation of semi-
volatile aerosols, and inhomogeneous sample deposits.
Additional restrictions apply when the weighed filters are
submitted to subsequent chemical speciation analyses. A
precisely controlled environment, with clean air and con-
stant temperature and humidity, is required for filter
weighing and processing, and filters must be equilibrated at
these conditions. Balances must have sensitivities of
B1 lg, be calibrated with well-established primary stan-
dards, and be regularly serviced. Ionizing sources are used
Disclaimer References to specific suppliers are not an endorsement
of those vendors, but are included as hardware and software
descriptions that may be available from other sources. Several
vendors may represent the same supplier. References cited here are to
the original manufacturer, to the extent possible.
Electronic supplementary material The online version of this
article (doi:10.1007/s41810-017-0010-4) contains supplementary
material, which is available to authorized users.
& Judith C. Chow
Judith.chow@dri.edu
1 include a size-selective inlet, filter substrate, filter holder,
Division of Atmospheric Sciences, Desert Research Institute,
Reno, NV 89512, USA
2 Chow 2011). Air enters the sampling inlet where 50% of
State Key Laboratory of Loess and Quaternary Geology
(SKLLQG), Institute of Earth Environment, Chinese
Academy of Sciences, Xi’an, People’s Republic of China
1 • 1 •
Xiaoliang Wang
to neutralize electrostatic charges. Regular quality control
and quality assurance procedures involve filter inspection
for defects before and after sampling, periodic balance zero
and span checks, replicate filter weights, and independent
system and performance audits.
Keywords Aerosol sampling Mass measurement
Weighing laboratory Filter measurements Gravimetric
analysis
1 Introduction
Suspended particulate matter (PM) collection by filtration
and gravimetric analysis is the earliest and most widely
used technique for obtaining ambient concentrations
(Beamish and McBryde 1949; Dunmore et al. 1964; Fee-
ney et al. 1984; Goetz 1953; Vaughan et al. 1989). A blank
filter is weighed on a laboratory balance, ambient air is
drawn through it at known flow rates and durations, PM is
retained while particle-free air exits the filter, the filter is
re-weighed, the blank filter weight is subtracted, and the
weight gain is divided by the sample volume to determine
the PM concentration over the sample period. As simple as
this process seems, PM concentrations by this method can
be inaccurate and imprecise because the PM deposit is
quite small compared to the weight of the filter. There are
many procedural and environmental variables that can
affect the initial and final filter weights.
The basic components of an aerosol sampling system
flow mover, and flow controller (Chow 1995; Watson and
the particles greater than the specified size are removed.
Particles larger than the reported ‘‘cut point’’ are still
123

sampled because inlet sampling effectiveness is not a step
function (Watson et al. 1983). The inlet defines the sam-
pled size fraction, with PM 2.5and PM (particles
10 with
aerodynamic diameters \2.5 and \10 lm, respectively)
being the most common. The air stream containing the
remaining particles passes through a transfer tube and is
directed toward a filter holder containing the collection
filter (Lippmann 2001). Filters are selected to be compat-
ible with the intended physical, chemical, and optical
analysis methods (Chow and Watson 2013; Watson et al.
2016), including the weight of the collected PM. A pump
draws air through the sampling system. A flow meter
behind the filter monitors the volume of air and may con-
trol the pump to maintain a pre-set flow rate (Baker and
Pouchot 1983a, b; Bean 1971).
This review addresses the filters, filter holders, and
weight determination aspects of this measurement method
by: (1) describing the filters used for PM mass concentra-
tions and the environmental and handling effects on their
weights; (2) identifying filter holders and processing
methods to minimize these effects; and (3) specifying
standards, hardware, and software for laboratory gravi-
metric analysis.
2 Filter Processing Facility
A clean laboratory environment is required for filter
inspection, equilibration, and weighing. The ideal case is a
separate room with an independent ventilation system
through a high efficiency particulate air (HEPA) filter and
positive pressure to prevent contaminated air from entering
when access doors are open (Rudnick 2004). Accept-
able environments can be maintained inside glove boxes,
but these are uncomfortable and awkward for processing
large numbers of filters (Allen et al. 2001; Kuo et al. 2015).
Different filter conditioning environments can result in
different mass measurements as a function of relative
humidity (RH). Both the filter media and the deposit can
retain liquid water that may bias PM concentrations
(Brown et al. 2006;Cahn1963; Charell and Hawley 1981;
Kajino et al. 2006; McInnes et al. 1996; Perrino et al.
2013, 2016; Tierney and Conner 1967). Soluble particles
take on water as RH increases, especially above the deli-
quescence point of approximately 70% RH (Tang 1980;
Watson 2002). Increases in the collected mass of 50% or
more have been observed as RH increases to 100% (Tier-
ney and Conner 1967). The hysteresis effect as RH
decreases precludes a constant mass measurement unless
samples are equilibrated at an RH of less than 30% prior to
and after exposure. U.S. EPA (1997) procedures call for
mean temperatures between 20 ± 2 and 23 ± 2 C and
mean RH between 30 ± 5 and 40 ± 5% over 24 h.
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Aerosol Sci Eng
European Union procedures (Belis et al. 2012) call for
equilibration at 20 ± 1 C and 50 ± 3% RH. In China, the
conditions are 15–30 C and 50 ± 5% RH (HJ 2011).
Temperature and RH in the controlled environment are
measured, recorded, and inspected continuously, as indi-
cated in Figure S-1 of the supplemental information. Dig-
ital sensors are preferred because they are easily interfaced
to data loggers and/or computer systems for subsequent
data processing and validation. Adjustments are made to
the environmental control system when equilibration con-
ditions exceed pre-set tolerances, and these are preferably
made by feedback from the sensors to the air handlers.
The microbalance (MettlerToledo 2017c; Sartorius
0
2017) is placed on a flat, stable, stone within a 183 cm (6 )
to 244 cm (8 )0 laminar flow hood (PureAire 2017) that
continuously blows air toward the weighing technician to
minimize contamination; exhaled ammonia can neutralize
acidic components in the deposit (Fig. S-2). The stone
minimizes balance vibration. Microbalance sensitivity is
±1 lg for the weight range of 0–250 mg, and ±0.1 lg for
the weight range of 0–25 mg. Modern microbalances can
be interfaced to a computer with a barcode reader for data
acquisition, eliminating the need for manually recording
weights and entering them into a database. Many modern
balances also have internal zero and span checks.
Automated weighing systems have been used in which
filters are loaded into cassettes and robotically moved to
and from the microbalance for automatic weighing (Pres-
ler-Jur et al. 2016). While weights have been shown to be
comparable to those derived from manual weighing, there
is little technician time saved as the filters must be trans-
ferred from the Petri slide to the cassettes and back again.
There is a high potential for associating filters with the
wrong label with so many out of their Petri slides at the
same time, and there are some reports of filter loss due to
jamming of the filter handling system.
A light table (HallProductions 2017) is used for filter
inspection. Upon receipt, each filter is examined for dis-
coloration, pinholes, and surface non-uniformity, with
rejection of filters that show these defects. An equilibration
tray (Figure S-2) separates filters from one another so that
the equilibration air can reach all parts of the filter surface.
Grounding wires, with alligator clips on one end connected
to the equilibration trays and banana clips on the other end
connected to a ground, can be used to minimize electro-
static charges. After equilibration, blank filters are placed
into individual Petri slides (MilliporeSigma 2017) made of
00
molded polystyrene, typically of 51 mm (2 ) 9 76 mm
(3 00) dimensions that can accommodate filters up to 47 mm
in diameter. An adhesive label, preferably with a barcode
generated specific to each project, is placed on the slide to
uniquely identify that sample. Some filters are available
with pre-assigned IDs printed on them, but these are not
Aerosol Sci Eng
recommended because they preclude future chemical
analysis.
Electrostatic charges on filter materials may interfere
with accurate weighing by creating an attraction between
the filter and its surroundings (Engelbrecht et al. 1980;
Hanninen et al. 2002; Hawley and Williams 1974; Lawless
and Rodes 1999; Swanson and Kittelson 2008; Tsai et al.
2002; Weil 1991). Polonium-210 ( Po) 210
charge neutral-
izers (HealthPhysics 2017; Niemeyer et al. 1978) can
minimize these effects. Ionizing blowers (SimcoIon 2017)
can also be used to reduce static charges. Noisy balance
readouts, drifts, and sudden shifts are indicators of exces-
sive electrostatic charge. Polycarbonate filters are espe-
cially prone to this interference, and they have been
observed to leap to other surfaces prior to discharging.
210
Po neutralizers should be handled per manufacturers’
instructions. They have half-lives of 138 days, so they need
to be replaced every 6 months with the spent units properly
disposed of. Antistatic solutions can be used to coat the
interior and exterior non-metallic surfaces of the weighing
chamber to drain electrostatic charges by conduction.
Earth-grounded conductive mats are also used to reduce
electrostatic charge buildup.
Ammonium nitrate and some organic particles evaporate
during sampling when the sample temperature exceeds that
of ambient air (Cheng et al. 2009; Chow et al. 2005). To
minimize changes during aerosol sampling, U.S. EPA
federal reference method (FRM) field samplers bathe the
filter cassette in ambient air to maintain a filter temperature
within 5 C of ambient air. After post-gravimetric analysis,
the exposed PM 2.5samples need to be sealed and kept in
the refrigerator (\4 C) for a minimum period of 1 year
after sampling. Filter storage requirements are not part of
the FRM, but they are part of program implementation.
3 Filters
Figure 1 illustrates the types of parallel filter samples that
are used for different chemical analyses. Gravimetry is
commonly applied to the ringed Teflon-membrane filter, as
it is the most durable, stable, and artifact free of all the
filter media. With careful processing and environmental
control, however, other filter types can also be successfully
weighed before and after sampling (Pall 2017b). Fibrous
filters are composed of a mat of cellulose, glass, quartz,
asbestos, or polystyrene fibers in random orientation within
the plane of the filter sheet. Membrane-type filters have
straight-through or sinuous pores (Raynor et al. 2011) and
are made of Teflon, polycarbonate, nylon, polyvinyl chlo-
ride (PVC), and cellulose esters. Membrane filters have a
more limited loading capacity than fiber filters, because
most of the deposit is confined to the surface where some
may be lost with heavy deposits. The small pores in
membrane filters may also clog with heavy loadings, as
indicated by decreasing flow rates over the sample dura-
tion. The surface deposit is advantageous for subsequent
elemental analyses by X-ray fluorescence (XRF) (Watson
et al. 1999) and microscopy (Casuccio et al. 1983). Fiber
filters have a higher capacity, as the sampled particles
penetrate into the filter and the weave is less prone to
clogging. The particle penetration, however, requires
greater effort or precludes some subsequent analyses.
Optimal filter loadings should range from *40 to 250 lg/
cm 2 , or *500 to *3000 lg/47 mm filter.
The selection of a particular filter type for a specific
application is a compromise among factors that include
cost, availability, collection efficiency, requirements of the
analytical procedures, and the ability of the filter to retain
its collection properties and physical integrity under the
ambient sampling conditions. More details on these issues
are found in Watson and Chow (2011).
Ringed Teflon-membrane filters consist of a thin, porous
polytetrafluoroethylene [PTFE, (C F ) ] Teflon 2 4 n sheet
stretched across a polypropylene or polymethylpentene
support ring (GE 2017b). These have [99% sampling
efficiencies and are the most stable filters available, with
little effect from temperature and RH on their weight
changes and minimal interference during sampling.
Table 1 summarizes the relevant properties of these filters
specified for U.S. PM 2.5 compliance sampling (CFR 2016).
They have low background levels for all species except
carbon and fluoride. These filters cannot be cut into sepa-
rate pieces for different analyses as the membrane col-
lapses when cut. Non-ringed Teflon-membrane filters are
thicker than the ringed filters, but they are more econom-
ical (TischScientific 2017). Non-ringed filters can be sec-
tioned into smaller pieces, but their added thickness
increases detection limits for some of the potential chem-
ical analyses (Chow and Watson 2013).
Etched polycarbonate membranes (GE 2017a) (often
called Nuclepore filters, after their first manufacturer)
consist of a thin polycarbonate sheet through which pores
of uniform diameter have been produced by radioactive
particle penetration and chemical etching (Spurny et al.
1969a, b). Depending on the pore size, these filters have
variable particle collection properties. They have low ele-
mental blank levels, are appropriate for elemental and ion
analyses, and are used in microscopy, as the membrane
surface and pores are very uniform. Nuclepore filters are
most susceptible to electrostatic forces and require longer
neutralization periods than the other filters (Romo-Kro ¨ger
1989). The Nuclepore 8.0 and 0.4 lm filters are most
commonly used in ambient PM sampling (Cahill et al.
1977). While the 0.2 lm pore size filter provides a higher
sampling effectiveness, its higher flow resistance requires a
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 Aerosol Sci Eng

Ringed Teflon-membrane filter

a
Functional Multi-λ light GRAV: Gravimetric analysis
Mass Elements groups absorption b
XRF: X-ray fluorescence spectroscopy
(GRAV )
a (XRF b) (FTIR c) (UV-VIS d) c
FTIR: Fourier Transform Infrared
Rare earths Spectroscopy,
Acid digestion and isotopes d
UV-VIS: Ultraviolet-visible light
(ICP-MS )e spectroscopy
e ICP-MS: Inductively coupled plasma-

mass spectrometry
Quartz-fiber filter f Multiwavelength TOR/TOT:
Multiwavelength thermal/optical
reflectance and transmittance; uses 7
OC/EC wavelengths (i.e., 405, 445, 532, 635, 780,
Non-polar Polar organic 808, and 980 nm) for organic and
(Multi- organic compounds
wavelength (ID-TD- elemental carbon
TOR/TOT ) compounds
f GC/MS )
h
(TD-GC/MS )g g TD-GC/MS: Thermal desorption-gas
chromatography/mass spectrometry
Nylon-membrane filter h ID-TD-GC/MS: In-situ derivatization-
Extracted in water after processing thermal desorption-gas
chromatography/mass spectrometry
i
IC-CD: Ion chromatography with
Short-chain Anhydrosugars, conductivity detection
Anions and carboxylic polyols, WSOC ,
k
j
cations acids saccharides WSON l IC-PAD: Ion chromatography with
(IC-CD )i (IC-CD) (IC-PAD ) (TOCm) pulsed amperometric detector
j k
WSOC: Water-soluble organic carbon
l
WSON: Water-soluble organic nitrogen
m
TOC: Total organic carbon analysis
Polycarbonate-membrane filter n
SEM: Scanning electron microscopy
o
PIXE: Proton-induced x-ray emission.

Particle
Morphology Elements
(SEM n) (PIXE o)

Fig. 1 Commonly used filters for gravimetric and other chemical gravimetric analysis. In the absence of a nylon filter, a section of the
analyses. Although analysis methods are associated with a single quartz-fiber filter can be used for water-soluble ion analysis
filter, they may be performed on sections of other filters, after

-1
large pressured drop across the filter for[10 L min flow
rates.
Nylon-membrane filters (Pall 2017a) consist of thin
sheets of porous nylon. Although these filters are normally
used to collect nitric acid (HNO ) 3and total nitrate (Appel
et al. 1981; Tsai et al. 2004), they can also be weighed.
Nylon filters have high flow resistance that increases with
filter loading, making their loading capacity less than that
of other filters. Since these filters passively adsorb HNO ,
depending on how long they have been exposed to an acid-
rich environment, they need to be tested prior to sampling,
and if nitrate is detected, they must be washed in a sodium
bicarbonate solution followed by distilled-deionized water
(DDW) rinse prior to use in the field. They also adsorb
small amounts of ammonia (NH 3 , Masia et al. 1994) and
sulfur dioxide (SO , Chan2 et al. 1986; Eldred and Cahill
1997; Japar and Brachaczek 1984; Masia et al. 1994;
3 Sickles and Hodson 1999b; Sickles and Hodson 1999a).

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Table 1 U.S. EPA PM 2.5 filter specifications for federal reference method (FRM) sampling to be certified by the manufacturer (CFR 2016)
Attribute Specification

Filter medium and size Polytetrafluoroethylene (PTFE) Teflon with polymethylpentene (PMP) or equivalent inert material support ring.
Outer diameter 46.2 ± 0.25 mm with a width of 3.68 mm and ring thickness of 0.38 ± 0.04 mm support ring
Pore size 2 lm as measured by ASTM F316-94
Filter thickness 30–50 lm
Maximum pressure drop 30 cm H O2 column with 16.67 L min -1
clean air flow on unexposed filter
Maximum moisture No more than 10 lg weight increase after 24-h exposure to air at 40% RH, relative to the weight after an initial 24-h
pickup exposure to air at 35% RH
Collection efficiency Exceeding 99.7%, as measured by dioctyl phthalate (DOP) test (ASTM D-2986-95a) with 0.3 lm particles at the
sampler’s operating face velocity
Filter weight stability Less than 20 lg for minimum of 0.1% per lot or 10 filters. Drop test from 25 cm three times to verify loose surface
particle contamination. Heat to 40 ± 20 C for\48 h to test temperature stability
Alkalinity Less than 25 microequivalents per gram of filter
Chemical composition Non-detectable quantities of species to be submitted to chemical analysis after FRM compliance sampling.
(optional) Applicable only if such analysis is anticipated

The adsorption of these gases will cause a bias in PM
concentrations in areas with high HNO , NH 3 , and
3 SO
concentrations.
Teflon-coated glass-fiber filters (Pall 2017b) imbed a
Teflon slurry onto a loosely woven glass-fiber mat. These
filters were developed for the Sulfate Regional Experiment
(SURE, Mueller et al. 1983) to minimize the adsorption of
gases, especially SO , 2that was found for the then-common
glass-fiber filter material. The most common application of
these filters is for samples amenable to polycyclic aromatic
hydrocarbon (PAH) analysis, and they are often weighed as
part of these measurements (Correa and Arbilla 2006).
Quartz-fiber filters (Pall 2017b) consist of a tightly
woven mat of quartz filaments. Quartz-fiber filters are
commonly used for carbon (Chow et al.
1993, 2007, 2011, 2015b) and ion analyses (Chow and
Watson 1999, 2017), with a parallel Teflon sample used for
gravimetric analysis. Quartz filters adsorb organic vapors
(Chow et al. 2010; Watson et al. 2009), which yields a
positive bias to gravimetric measurements. They are usu-
ally baked at high temperatures (up to 900 C) to reduce
carbon blank values caused by organic vapor adsorption,
and this makes them brittle, with potential loss of filter
material during filter pack loading and unloading. This
results in a negative bias. Whatman QMA filters (GE
2017c) contain a 5% borosilicate glass binder that mini-
mizes its fragility. This makes it more useful for
gravimetry, but it increases the propensity for non-carbon
gas adsorption. The glass binder melts under the high
temperature conditions of carbon analysis. Brown et al.
(2006) and Quincey et al. (2009) report water uptake by
quartz filters with changing RH during equilibration that
can also affect gravimetric mass.
Cellulose acetate membrane, cellulose-fiber membrane,
2 PVC, and glass-fiber filters were commonly used in the
early days of filter sampling, but as more was learned
about their adsorption and desorption of water at different
RHs, their variable sampling efficiencies, and contami-
nants that preclude other analyses, these are no longer
used for PM and10 PM gravimetry.2.5 These limitations
are documented in other reviews (Chow 1995; Watson
and Chow 2011).
4 Filter Holders
Filter holders (Lippmann 1995, 2001; Puskar et al. 1992)
are designed for the specific filter size used, and several
of these are illustrated and described in Figure S-3. Filter
holders provide a seal at the edge (Vandenheever 1994)
and a bottom support so that the filter is not deformed or
sucked through by the vacuum created by the sampler
pump. Open-faced filter holders permit uniform air flow
across the filter face, resulting in a homogeneous deposit
(Lai et al. 2006; McDade et al. 2009). This homogeneity
is not necessary for gravimetric analysis or when the
entire filter is submitted to subsequent analyses, but it is
necessary when a portion of the filter is submitted to
analysis. Deposit uniformity also mitigates against losses
of particles from overloaded sections of the filter. For this
reason, in-line filters are to be avoided, as sampling
through them creates a spot in the middle of the filter, as
shown in Figure S-4. With an open-face filter holder, the
air velocity is uniform across the filter holder. An inho-
mogeneous or low-porosity support grid can also cause an

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Table 2 Summary of quality control (QC) activities for filter processing and gravimetric analysis
QC Purpose Frequency Standard Acceptance criteria Response/action
Activity

Balance Assure no weight reading with Every None ±0 lg Rezero

tare nothing on balance pan *10
samples
Balance Normalize balance output to Every Certified Class 1 ±3 lg Adjust span
span standard weight *10 or Class E
samples weights
Check Ensure instrument accuracy with Every Certified Class 1 ±3 lg Re-tare, re-span
weight independent standard 10th or Class E and re-weigh all
sample weights filters
Replicates Ensure and estimate sample 10–100% NA ±10 lg for pre-weight and ±15 for Re-weigh sample
precision of post-weight, unless flagged as batch
samples volatile
Level 1 Identify and flag sample Every NA NA Enter flagged
data appearance and deviations from sample sample into the
validation procedures database
NA not applicable

uneven deposit that may bias analyses of a portion of the
filter (Fig. S-5).
Filter holders should be made of inert materials that will
not contaminate the filter with the chemical species to be
quantified. Injection-molded fluorinated ethylene propy-
lene (FEP) Teflon and polycarbonate filter holders meet
these specifications. Rubber O-ring seals have been found
to outgas with adsorption onto quartz-fiber filters, so these
are replaced with inert Viton O-rings (Tombach et al.
1987).
The PM 2.5 FRM filter ring (CFR 2016) is used as a
common 47 mm filter holder (Figu. S-3). This holder
consists of Delrin plastic rings with a stainless steel
support grid into which 100 lm diameter holes are etched
100 lm apart. Most FRMs use a white-colored Delrin
holder, but when these are new they may contaminate the
quartz-fiber filters used for carbon analysis (Clark 2002;
Gutknecht et al. 2001). Similar blue-colored holders made
of a different material were created by hot injected-mol-
ded ABS plastic, but these are much harder material and
sometimes tear the Teflon-membrane filter. The stainless
steel support grid adsorbs certain gases, so if an
impregnated backup filter is used to measure HNO ,NH 3 3expected
or SO 2, it is advisable to use a Teflon filter holder and
support grid.
Several stainless steel filter holders are available, many
of them with in-line connectors (Fig. S-4) that should be
avoided. These are usually costly and increase shipping
costs between the laboratory and the field owing to their
greater weight.
Most filter holders come with protective covers for their
faces and pump connectors. These covers are removed in
the field when filters are installed in a sampler, then
replaced on the filter holders after sampling prior to ship-
ment back to the laboratory. The FRM filter holders can be
placed in a labeled Petri dish for protection during
shipping.
5 Quality Control (QC) and Quality Assurance
(QA)
Tables 2 and 3 outline the different QA procedures and
their frequencies, some of which are described in more
detail in the following section. Table S-1 includes example
validation flags as well as the indicators for their applica-
tion. When elemental, carbon, and ionic analyses are car-
ried out, as in a speciation network, a further validation test
is a comparison of the weighted sum of the measured
species with the gravimetric mass (Chow et al. 2015a).
Equipment-specific operating manuals are available
from the manufacturers, copies of which should be located
near the appropriate instrument. Laboratory-specific stan-
dard operating procedures (SOPs) need to be created that
include: (1) summary of measurement method, principles,
, accuracy and precision, and the assumptions for
validity; (2) materials, equipment, reagents, and suppliers;
(3) individuals responsible for performing each part of the
procedure; (4) traceability path, primary standards or ref-
erence materials, tolerances for transfer standards, and
schedule for transfer standard verification; (5) start-up,
routine, and shutdown operating procedures and an
abbreviated checklist; (6) data forms; (7) routine mainte-
nance schedules, maintenance procedures, and trou-
bleshooting tips; (8) internal calibration and performance
testing procedures and schedules; (9) external performance

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Table 3 Example of quality assurance (QA) activities for gravimetric analysis

a
QA activity Purpose Frequency Performer Acceptance criteria Response action

Balance Ensure proper functioning Every year or Manufacturer Balance performer as Document maintenance schedule
maintenance of weighing system when representative specified by
malfunction is manufacturer
detected
Internal system Ensure compliance with Every year or Internal QA Conformance with Prepare preventive or corrective
and operational and quality when manager laboratory SOPs, actions based on audit findings and
performance system procedures malfunction is QAPPs, and quality follow up to ensure completion of
audits detected manual specified actions
Technical system Assess adequacy of and Every 3 years External Conformance with good Prepare and implement preventive
audits conformance with good auditor laboratory practices and corrective actions as needed
laboratory practices and and adherence to based on audit findings
QA/QC procedures laboratory SOPs
Quality system Assess adequacy of and Every 3 years External Conformance with good Prepare and implement preventive
audit conformance with quality auditor laboratory practices and corrective actions as needed
system and adherence to based on audit findings
laboratory SOPs
Performance Assess comparability of Every year External Within specified limits Prepare and implement preventive
evaluations and analytical results with auditor or and agreement with and corrective actions as needed
laboratory standards and other audit team other laboratories based on findings
inter- laboratories
comparisons

SOP standard operating procedure, QAPP quality assurance project plan

a
In the USA, external auditors include the U.S. Environmental Protection Agency (U.S. EPA 2017) and the Environmental Laboratory
Accreditation Program of the NELAC Institute (TNI 2016)

auditing schedules; (10) safety measures; and (11) refer-
ences to relevant literature and related SOPs. The following
section provides direction that can be useful in preparing
these procedures.
Class 1 or Class E gravimetric standards (Bignell and
Fen 2003; MettlerToledo 2017a) need to be procured for
calibration and performance tests. Standard masses of 100,
200, 300, and 500 mg are used to define the span. The span
maximum should be slightly more than the typical filter
weight. Weights from 10 to 200 mg are used to evaluate
balance linearity after it is spanned. A separate set of
weights is verified against these primary standards and used
as check weights.
6 Filter Handling and Gravimetric Analysis
Procedures
Figure 2 presents a flow diagram of the routine operating
procedure. New blank filters are placed in an equilibration
tray at controlled temperature and RH environment for at
least 4 weeks to allow for outgassing of any residues from
the manufacturing process that might change the blank
filter weight. Exposed filters returned from the field are
equilibrated in the same environment for a minimum of
24 h prior to weighing to allow soluble deposits to achieve
equilibrium with the weighing environment. Unexposed
filters are separated in containers (Petri culture dishes
150 mm diameter) such that all surfaces are exposed to the
equilibration environment. For exposed filters, Petri slides
(MilliporeSigma 2017) containing the filters are located on
the counter of a laminar flow hood with the lids slightly
ajar so that the filters are exposed to the equilibration
environment.
To inspect each filter, the light table surface and flat tip
forceps are first cleaned with a methanol-moistened wiper
and allowed to dry. Filters are handled with non-powdered
latex-gloved (Kimberly-Clark 2017) hands to prevent
contamination. Holding the edge of a ringed Teflon filter
with the forceps, the filter is placed on a light table and
examined for pinholes, separation from the support ring,
loose particles, tears, creases, inhomogeneity or variations
in density, lumps, or other defects. Loose Teflon particles
may be removed by gently spraying with air from a rubber
bulb (MettlerToledo 2017b). Filters that do not meet visual
criteria are rejected and returned to the vendor. If chemical
analyses are to be performed, two filters from each lot of
100 are analyzed for blank levels and the lot should be
rejected if pre-set specifications are not met.
Sample IDs with barcodes are printed on gummed labels
that are affixed to the Petri slides. When multiple filter
types are used for parallel sampling (as illustrated in

123
 Aerosol Sci Eng

Receive
Teflon filters Receive from the
field sites

Ship to field sites

Document Disassemble filter
lot box cassette assemblies
number and place filters in
pre-assigned Petri
slides

Light
inspection
(100% of
filters)

Clean filter holders,

support screens, and Post-sampling
XRF cassette containers equilibration of filters for
acceptance a minimum of 24 hours
(2% of filters)

Equilibrate filters in a Perform

temp/RH-controlled
environment for 4-6 final weighing
weeks

Perform
replicate
Assign filter IDs and
place each filter in a weighing
Petri slide (30% of filters)

Perform
initial
weighing

Difference > 15 µg = Fail

Perform replicate weighing Difference < 15 µg = Pass

(100% of filters)
Perform data processing/validation and
merge mass/laboratory data with sampler-
acquired data and data entered from field
Difference < 10 µg = Pass Difference > 10 µg = Fail data sheets

Load filters into

filter holder
assembly and filter
cassette container
Submit to integrated filter data base
Store samples in Petri slides
with airtight seal for a minimum
of one year (< 4°C)

Document
field data sheet

Fig. 2 Flow diagram and illustrations of the filter preparation and gravimetric analysis procedures

123
Aerosol Sci Eng
Fig. 1), the same number is used, but filters are differen-
tiated by a filter code (e.g., T for Teflon, Q for quartz, N for
nylon, and P for polycarbonate). When two parallel filters
of the same type are used, a different letter is defined for
the subsequent filters. These IDs are recorded in a chain-of-
custody log book or, preferably, a computerized laboratory
data management system that associates each ID with the
filter batch number. The chain-of-custody record for each
sample includes entries for each filter ID, dates and tech-
nician identifier for filter inspection, equilibration, pre-
weighing, shipment to the field, receipt from the field, re-
equilibration, post-weighing, and storage. These records
identify the disposition of each sample and prevent the
creation of two samples with the same ID.
Filters are weighed in groups of 10–50 by a technician
wearing clean powderless latex gloves. The Petri slides con-
taining filters are placed in ascending order of filter ID num-
bers, if possible. The balance tare is adjusted to read zero with
nothing in the weighing chamber, and the span is adjusted to
(or verified against) a standard weight (typically 200 mg)
which is placed on the balance pan using a dedicated forceps.
No more than three filters are dissociated from their labeled
Petri slide at any time, one being removed from the balance
pan to its slide, one being transferred from the charge neu-
tralizer to the balance pan, and one being transferred from the
Petri slide to the charge neutralizer. This process minimizes
the filter placement in the wrong Petri slide.
The filter remains in the charge neutralization area for
30–60 s prior to being moved to the balance pan, where it
resides until a stable weight is achieved. For extremely
volatile aerosols, such as fresh wood smoke, the weight
may decrease continuously, associated with a characteristic
odor. This indicates aerosol volatilization, which cannot be
prevented, so the weight is taken at 60 s and an applicable
validation flag is assigned to that sample.
If the balance is interfaced to the appropriate computer
software, weights are recorded with the scanned filter ID.
They can also be recorded manually on a data sheet as a
backup or for later entry into the database. After the weight
is recorded, the just-weighed filter is placed into its labeled
Petri slide, the next filter is moved from the charge neu-
tralizer to the balance pan, and the next filter in line is
placed into the charge neutralizer.
Balance zero and span are verified after every ten filters
using a check weight standard. If the balance does not read
zero with nothing on the pan, or if the check weight reading
differs from its specified value by more than ±3 lg, the
balance is re-tared and re-spanned and the filters are re-
weighted. Filters weighed since the previous performance
test must be re-weighed when this limit is not attained.
Replicate weights are measured by another technician
on 10–100% of all filters in each batch. If any replicate
weight differs from the first weight by more than ±10 lg
from the routine pre-weight or ±15 lg from the routine
post-weight, re-weigh the entire batch of filters. Since
initial weights prior to field sampling cannot be recovered
if lost or missing, a 100% re-weight assures maximum data
recovery and is strongly recommended.
Filter weighing, loading, and unloading are performed in
a filter preparation room with controlled temperature and
RH. Non-powdered latex gloves are worn during all filter
handling operations. The work surface is cleaned with lab-
oratory wipes and a sheet of laboratory bench paper is laid
out. Forceps are cleaned with a methanol-moistened wipe.
Filter holders are cleaned by wiping the support ring, the
support grid, and the retaining ring with a methanol-moist-
ened wipe. Large batches can be cleaned with detergent-free
hot water in a laboratory dishwasher. Clean filter holders are
disassembled by separating the upper and lower parts and
removing their support grid. The support grid is placed into
the support ring, and a bar-coded label is affixed to the filter
holder or the container that protects it. Another label is
placed on the field data sheet that accompanies the sample
batch and that will be returned after sampling with the
sample time, place, duration, and flow rate. The Petri slide
containing the filter ID designated for sampling is opened
and forceps are inserted at the notch at thebottom of the slide
to gently secure the filter on its edge to place the filter onto the
support grid. The top of the filter holder is then attached. This
may be a pressure or threaded fit. The top must be tight
enough to ensure a good seal, but not so tight as to damage the
edge of the filter. If the blank filter isdamaged (Fig. S-6), the
process must be repeated with a clean filter. Exposed filters
with visibledamage (Fig S-6) should beweighed and flagged
per Table S-1).
Loaded filter holders are grouped by sampling site and
placed into a sealable polyethylene bag along with the field
data sheet. The field data sheet has columns for the sam-
pling site, date, initial and final flow rates, sample dura-
tions, and notes that are filled in by the field technician.
These samples are stored in a refrigerator until shipment.
It is good practice to ship filters to and from the field
under low temperature (\4 8C) conditions in a cooler with
containerized ice (blue ice). Field blanks should be pro-
vided for every 6th or 10th day of sampling.
The process is reversed when samples are returned from
the field sites. Filters are unloaded and placed back into
their labeled Petri slides and allowed to equilibrate at
standard conditions prior to re-weighing.
7 Calculations
Calculations assume that initial and final weights are
measured in the same laboratory. The Earth’s gravita-
tional attraction varies with position (Hirt et al. 2013),
123
 Aerosol Sci Eng

but the effect is negligible for practical situations. Nor- ! 0:5

X
N
ðM i M irÞ 2

mal fluctuations in air density (caused by pressure, r ¼ Mi 1 2 ð4Þ

temperature, and water vapor variations) do not require N 1
buoyancy corrections (Hanninen et al. 2002; Koistinen
and
et al. 1999; Rasmussen et al. 2010), but such corrections
! 0:5
are necessary when there is a substantial change with 1XN
ðM f M frÞ 2

balance elevation ([500 m) between the pre- and post- r Mf ¼ : ð5Þ

sample weighing. It is best to avoid changes in weighing
elevations.
The symbols and their definitions given below are used
in the subsequent subsections.
-3
C = PM mass concentration, lgm .
-3
r C = Precision of PM mass concentration, lgm .
M i = Initial weight of blank filter, lg.
M = Final weight of exposed filter, lg.
f
M = Weight of blank filter replicate, lg.
ir
fr
N = Number of replicate weights for exposed or blank
filters.
r M i = Precision of blank filter weights, lg.
r M f= Precision of exposed filter weights, lg.
3 -1
Q std = Standard volume flow rate, standard m min
3 -1
a
Q = Actual volume flow rate, actual m min . aspects. Additional attention is needed when weighed fil-
P a = Ambient barometric pressure, mmHg (or kPa).
P std = Standard barometric pressure, 760 mmHg (or
101 kPa).
T std = Standard temperature, 298 K (25 C ? 273).
T a = Ambient temperature, K (ambient C ? 273).
Q avg = Average sample flow rate over the sample
collection period.
t = Total elapsed sampling time, min.
v a = Total volume of air sampled, actual m . 3
r va = Precision of sample volume, obtained from flow
rate performance tests of field sampler, actual m . 3
PM 2.5 sampler flow rate measurement systems must be
calibrated in terms of the actual volumetric flow rate (Q )
at ambient temperature and pressure, as opposed to the
standard volumetric flow rate (Q ) stdthat is corrected to
standard temperature and pressure. If calibration is
expressed as Q std, conversion to Q will be required as
a
follows:
Q a ¼ Q stdðP std
=P ÞðT
a =Ta std Þ:
The sample volume is calculated as:
v a ¼ Q t:a
The mass concentration is then:
C ¼½ðM f
M Þ=v
i
:a
Precisions for the blank and exposed filter mass mea-
surements are (Watson et al. 1995):
N 1 2
The uncertainty of the mass concentration is then
(Watson et al. 1989):
! 0:5
2 2
r Mi þ r Mf r 2v
a
r C ¼ C ðM 2 þ v2 : ð6Þ
f M Þi
a
8 Summary and Conclusions
Accurate PM 10 and PM 2.5mass concentrations derived
from filter sampling require close attention to filter selec-
tion, laboratory preparation environments, filter handling,
and use of a high sensitivity analytical balance. Detailed
. procedures must be created and followed for each of these
ters are to be used for different chemical analyses.
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