ASTM D3685/D3685M-13(2021)
(Test Method)Standard Test Methods for Sampling and Determination of Particulate Matter in Stack Gases
Standard Test Methods for Sampling and Determination of Particulate Matter in Stack Gases
SIGNIFICANCE AND USE
5.1 The measurement of particulate matter and collected residue emission rates is an important test widely used in the practice of air pollution control. Particulate matter measurements after control devices are necessary to determine total emission rates to the atmosphere.
5.1.1 These measurements, when approved by federal and state agencies, are often required for the purpose of determining compliance with regulations and statutes.
5.1.2 The measurements made before and after control devices are often necessary as a means of demonstrating conformance with contractual performance specifications.
5.2 The collected residue obtained with these test methods is also important in characterizing stack emissions. However, the utility of these data is limited unless a chemical analysis of the collected residue is performed.
SCOPE
1.1 These test methods describe procedures to determine the mass emission rates of particulate matter and collected residue in gaseous streams by in-stack test methods (Test Method A) or out-of-stack test methods (Test Method B).
1.2 These test methods are suitable for measuring particulate matter and collected residue concentrations.
1.3 These test methods include a description of equipment and procedures to be used for obtaining samples from effluent ducts and stacks, a description of equipment and procedures for laboratory analysis, and a description of procedures for calculating results.
1.4 These test methods are applicable for sampling particulate matter and collected residue in wet (Test Method A or B) or dry (Test Method A) streams before and after particulate matter control equipment, and for determination of control device particulate matter collection efficiency.
1.5 These test methods are also applicable for determining compliance with regulations and statutes limiting particulate matter existing in stack gases when approved by federal or state agencies.
1.6 The particulate matter and collected residue samples collected by these test methods may be used for subsequent size and chemical analysis.
1.7 These test methods describe the instrumentation, equipment, and operational procedures, including site selection, necessary for sampling and determination of particulate mass emissions. These test methods also include procedures for collection and gravimetric determination of residues collected in an impinger-condenser train. The sampling and analysis of particulate matter may be performed independently or simultaneously with the determination of collected residue.
1.8 These test methods provide for the use of optional filter designs and filter material as necessary to accommodate the wide range of particulate matter loadings to which the test methods are applicable.
1.9 Stack temperatures limitation for Test Method A is approximately 400°C (752°F) and for Test Method B is 815°C (1500°F).
1.10 A known limitation of these test methods concerns the use of collected residue data. Since some collected residues can be formed in the sample train by chemical reaction in addition to condensation, these data should not be used without prior characterization (see 4.4.1).
1.10.1 A second limitation concerns the use of the test methods for sampling gas streams containing fluoride, or ammonia or calcium compounds in the presence of sulfur dioxide and other reactive species having the potential to react within the sample train.
1.10.2 A suspected but unverified limitation of these test methods concerns the possible vaporization and loss of collected particulate organic matter during a sampling run.
1.11 The values stated in either SI units or inch-pound units are to be regarded separately as standard within the text. The inch-pound units are shown in parentheses. The values stated in each system are not exact equivalents; therefore each system shall be used independently of the other. Combining values from the two systems may result in ...
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3685/D3685M − 13 (Reapproved 2021)
Standard Test Methods for
Sampling and Determination of Particulate Matter in Stack
Gases
This standard is issued under the fixed designation D3685/D3685M; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope analysis of particulate matter may be performed independently
or simultaneously with the determination of collected residue.
1.1 Thesetestmethodsdescribeprocedurestodeterminethe
mass emission rates of particulate matter and collected residue
1.8 These test methods provide for the use of optional filter
ingaseousstreamsbyin-stacktestmethods(TestMethodA)or
designs and filter material as necessary to accommodate the
out-of-stack test methods (Test Method B).
wide range of particulate matter loadings to which the test
methods are applicable.
1.2 These test methods are suitable for measuring particu-
late matter and collected residue concentrations.
1.9 Stack temperatures limitation for Test Method A is
approximately 400°C (752°F) and for Test Method B is 815°C
1.3 These test methods include a description of equipment
(1500°F).
and procedures to be used for obtaining samples from effluent
ductsandstacks,adescriptionofequipmentandproceduresfor
1.10 Aknown limitation of these test methods concerns the
laboratory analysis, and a description of procedures for calcu-
useofcollectedresiduedata.Sincesomecollectedresiduescan
lating results.
be formed in the sample train by chemical reaction in addition
1.4 These test methods are applicable for sampling particu- to condensation, these data should not be used without prior
late matter and collected residue in wet (Test Method A or B)
characterization (see 4.4.1).
or dry (Test Method A) streams before and after particulate
1.10.1 A second limitation concerns the use of the test
matter control equipment, and for determination of control
methods for sampling gas streams containing fluoride, or
device particulate matter collection efficiency.
ammonia or calcium compounds in the presence of sulfur
dioxide and other reactive species having the potential to react
1.5 These test methods are also applicable for determining
within the sample train.
compliance with regulations and statutes limiting particulate
matter existing in stack gases when approved by federal or 1.10.2 A suspected but unverified limitation of these test
state agencies. methods concerns the possible vaporization and loss of col-
lected particulate organic matter during a sampling run.
1.6 The particulate matter and collected residue samples
collected by these test methods may be used for subsequent
1.11 The values stated in either SI units or inch-pound units
size and chemical analysis.
are to be regarded separately as standard within the text. The
inch-pound units are shown in parentheses. The values stated
1.7 These test methods describe the instrumentation,
ineachsystemarenotexactequivalents;thereforeeachsystem
equipment, and operational procedures, including site
shall be used independently of the other. Combining values
selection,necessaryforsamplinganddeterminationofparticu-
from the two systems may result in nonconformance to this
late mass emissions. These test methods also include proce-
standard.
dures for collection and gravimetric determination of residues
collected in an impinger-condenser train. The sampling and
1.12 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
1 priate safety, health, and environmental practices and deter-
This test method is under the jurisdiction of ASTM Committee D22 on Air
mine the applicability of regulatory limitations prior to use.
Quality and is the direct responsibility of Subcommittee D22.03 on Ambient
Atmospheres and Source Emissions.
1.13 This international standard was developed in accor-
Current edition approved Sept. 1, 2021. Published October 2021. Originally
dance with internationally recognized principles on standard-
approved in 1978. Last previous edition approved in 2013 as D3685/D3685M–13.
DOI: 10.1520/D3685_D3685M-13R21. ization established in the Decision on Principles for the
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3685/D3685M − 13 (2021)
Development of International Standards, Guides and Recom-
C = concentration of collected residue in stack gas,
pm
3 3
mendations issued by the World Trade Organization Technical
dry basis, standard conditions, mg/m (gr/dsft ).
Barriers to Trade (TBT) Committee.
C = concentration of collected residue in stack gas, at
pm
act
3 3
actual conditions, mg/m (gr/aft ).
2. Referenced Documents
E = emission rate for particulate matter, kg/h (lb/h).
P.M.
E = emission rate for collected residue, kg/h (lb/h).
2.1 ASTM Standards:
pm
I = percent of isokinetic sampling.
D1071Test Methods for Volumetric Measurement of Gas-
M = dry molecular weight of stack gas, g/g-mol (lb/
eous Fuel Samples d
lb-mole).
D1193Specification for Reagent Water
M = molecular weight of water, 18.0 g/g-mol (18.0
H O
D1356Terminology Relating to Sampling and Analysis of
lb/lb-mole).
Atmospheres
M = molecular weight of stack gas, wet basis, g/g-mol
s
D2986Practice for Evaluation of Air Assay Media by the
(lb/lb-mole).
Monodisperse DOP (Dioctyl Phthalate) Smoke Test
P = barometric pressure at the sampling site, kPa (in.
bar
(Withdrawn 2004)
Hg).
D3154Test Method for Average Velocity in a Duct (Pitot
P.M. = total amount of particulate matter collected, mg.
Tube Method)
pm = total amount of collected residue, mg.
D3631Test Methods for Measuring Surface Atmospheric
P = absolute stack gas pressure, kPa (in. Hg).
s
Pressure
P = static stack gas pressure, kPa (in. Hg).
stat
D3796Practice for Calibration of Type S Pitot Tubes
P = absolute pressure at standard conditions, 101.3
std
D4536Test Method for High-Volume Sampling for Solid
kPa (29.9 in. Hg).
Particulate Matter and Determination of Particulate Emis-
Q = stackgasvolumetricflowrate,drybasis,standard
stp-d
3 3
sions (Withdrawn 2000)
conditions, m /h (dsft /h).
−3 3
E1Specification for ASTM Liquid-in-Glass Thermometers
R = ideal gas constant=8.32×10 (kPa·m )/(K·g −
E2251Specification for Liquid-in-Glass ASTM Thermom-
mol) for the SI system, and 21.8 (in. Hg·ft )/
eters with Low-Hazard Precision Liquids
(°R·lb−mole) for the U.S. customary system.
T = average temperature of the gas in the dry gas
d
3. Terminology
meter,obtainedfromtheaverageoftheinitialand
3.1 Definitions—For definitions of terms used in these test
the final temperatures, K (°R) (see 10.2.2.6 and
methods, refer to Terminology D1356.
10.2.2.9).
3.2 Definitions of Terms Specific to This Standard: T = absolute average dry gas meter temperature, K
m
3.2.1 collected residue, n—for the purpose of these test (°R).
methods, solid or liquid matter collected in the impingers ( T ) = absolute average stack gas temperature, K (°R).
s avg
T = absolute temperature at standard conditions, 298
employed in these test methods and remaining after solvent
std
K (25°C) (537°R).
removal.
T = temperature of the gas in the wet test meter, K
w
3.2.2 particulate matter, n—for the purpose of these test
(°R) (see 10.2.2.6 and 10.2.2.9).
methods, all gas-borne matter (solid or liquid) collected in the
V = gas volume passing through the dry gas meter, K
d
front half of the sample train (probe, nozzle, and front half of
(°R) (see 10.2.2.6 and 10.2.2.9).
filter).
V = total volume of liquid collected in impingers and
lc
3.3 Symbols:
desiccant, mL.
V = volume of gas sample through the dry gas meter,
m
2 2
A = internal cross-sectional area of stack, m (ft ). 3 3
meter conditions, m (dft ).
2 2
A = cross-sectional area of nozzle, m (ft ).
n
V = volume of gas sample through the dry gas meter,
m
act
B = proportion by volume of water vapor in the gas 3 3
wo
corrected to actual gas conditions, m (or aft ).
stream, dimensionless.
V = volume of gas sample through the dry gas meter,
m
std
C = dry gas meter correction factor, dimensionless. 3 3
m
corrected to dry standard conditions, m (dft ).
C = pitot tube coefficient, dimensionless.
p
(V ) = average stack gas velocity, m/s (ft/s).
s avg
C' = concentration of particulate matter in stack gas,
P.M.
V = volume of water vapor in the gas sample, cor-
m
std
on the dry basis, standard conditions, mg/m 3 3
rected to actual conditions, m (dsft ).
(gr/dsft )
V = gas volume passing through the wet test meter,
w
C' = concentrationofparticulatematterinstackgas,at 3 3
P.M.
act
m (aft ) (see 10.2.2.6 and 10.2.2.9).
3 3
actual gas conditions, mg/m (gr/aft ).
V = volume of water vapor in the gas sample, cor-
w
std
3 3
rected to dry standard conditions, m (dsft ).
Y = dry gas meter calibration factor.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Y = ratio of accuracy of wet test meter to dry gas
i
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
meter (see 10.2.2.6 and 10.2.2.9).
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. θ = total sampling or calibration run time, min.
The last approved version of this historical standard is referenced on
ρ = density of water, 997 kg/m , at 298 K.
H O
www.astm.org.
D3685/D3685M − 13 (2021)
5.1.2 The measurements made before and after control
∆H = average pressure drop across the orifice meter,
devices are often necessary as a means of demonstrating
kPa (in. H O).
conformance with contractual performance specifications.
∆H@ = average orifice pressure differential that develops
3 3
0.021 m (0.75 ft ) of air at standard conditions
5.2 The collected residue obtained with these test methods
for all six calibration runs, kPa (in. H O) (see
2 is also important in characterizing stack emissions. However,
10.2.2.9).
the utility of these data is limited unless a chemical analysis of
∆H@ = orifice pressure differential at each flow rate that
i
the collected residue is performed.
3 3
gives 0.021 m (0.75 ft ) of air at standard
conditions for each calibration run, kPa (in. H O)
2 6. Interferences
(see 10.2.2.9).
6.1 Gaseous species present in-stack gases that are capable
∆P = average stack gas velocity head, kPa (in. H O).
avg 2
of reacting to form particulate matter within the sample train
NOTE 1—To convert ∆H and ∆P from inches of water to inches of
avg
can result in positive interference.
mercury, divide by 13.6, the specific gravity of mercury. To convert from
inches of water to kilopascals, multiply by 0.248. 6.1.1 Examples include the potential reaction of sulfur
dioxide(SO )toaninsolublesulfatecompoundinthemoisture
4. Summary of Test Method
portion of the system (such as with limestone in flue gas
following a wet flue gas desulfurization system (FGDS) to
4.1 Test MethodA(in-stack) involves a sampling train with
a primary and a backup filter located in-stack. (Use of the form calcium sulfate (CaSO ) or the reaction with ammonia
gas (NH ) to form ammonium sulfate (NH SO ) and the
backup filter is optional.) The sample is withdrawn from the
3 4 4
potential reaction of hydrogen fluoride (HF) with glass com-
stack isokinetically through the filter system followed by a
ponents in the sample train with resultant collection of silicon
series of impingers or condensers set in an ice bath, which act
tetrafluoride (SiF ) in the impingers.
as a moisture trap and collect the collected residue. A dry gas
meter is used to measure the sample gas volume.
6.2 Volatile matter existing in solid or liquid form in the
4.1.1 The primary filter may be a thimble type filter or a
stack gas may vaporize after collection on the sample train
glassfiberfilter.Noback-upisrequiredwhentheprimaryfilter
filtration material due to continued exposure to the hot sample
is of the latter type.
stream during the sampling period. Such occurrence would
4.2 Test Method B (out-of-stack) involves a sampling train result in a negative interference.
with a filter located out-of-stack heated above the moisture-
7. Apparatus
acid dew point in order to prevent filter saturation. Sample is
withdrawn from the stack isokinetically through the filter
7.1 Sampling Train—For schematic drawings of the major
systemfollowedbymoisturecondensorssetinanicebath.The
sampling train components refer to Figs. 1 and 2 for Test
moisture condensors provide the collection mechanism for
Method A and Fig. 3 for Test Method B.
collected residue.
7.1.1 The materials of construction of in-stack and certain
4.2.1 The sample gas volume is measured with a dry gas
out-of-stack components (such as the nozzle, probe, unions,
meter.
filter holder, gaskets, and other seals) shall be constructed of
materials which will withstand corrosive or otherwise reactive
4.3 Particulate matter mass and collected residue mass are
compounds or properties of the stack or gas stream, or both.
determined gravimetrically. Particulate matter (12.10.1 and
Recommended materials for a normal range of stack and
collected residue (12.10.2) are calculated separately as mass
sample conditions include PFTE fluoro hydrocarbons (up to
per volume sampled at standard conditions, dry, and on the
175°C (350°F), 316 stainless steel (up to 800°C (1500°F), and
actual gas basis.
some resistant silicone materials (up to 150°C (300°F). Ex-
4.4 The gravimetric analysis procedure is nondestructive
treme temperature conditions may require the use of materials
and thus both the particulate matter and the collected residue
such as quartz or nickel-chromium alloy, or a water-cooled
catches are available for further physical and chemical char-
probe may be used.
acterization.
7.2 ElementsoftheSamplingTrain—Thesamplingtrainfor
4.4.1 Although procedures are not included in these test
collecting particulate matter and collected residue from a gas
methods, it is recommended that the collected residues be
stream flowing through a stack consists of the interconnected
subjected to chemical analysis or otherwise characterized prior
elements described in 7.3 – 7.10.
to use of the mass results.
7.3 Nozzles—The first part of the sampling equipment to
5. Significance and Use
encounterthedustormoisture-ladengasstream,orboth,isthe
5.1 The measurement of particulate matter and collected nozzle. In order to extract a representative samp
...
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