ASTM D6331-98

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Designation:D6331–98
Standard Test Method for
Determination of Mass Concentration of Particulate Matter
from Stationary Sources at Low Concentrations (Manual
Gravimetric Method)
This standard is issued under the fixed designation D6331; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method covers a method for the measurement 2.1 ASTM Standards:
of particulate matter (dust) concentration in emission gases in D1193 Specification for Reagent Water
the concentrations below 20 mg/m standard conditions, with D1356 Terminology Relating to Sampling andAnalysis of
3 4
special emphasis around 5 mg/m . Atmospheres
1.2 To meet the requirements of this test method, the D2986 Practice for Evaluation of Air Assay Media by the
particulate sample is weighed to a specified level of accuracy. Monodisperse DOP (Dioctyl Phthalate) Smoke Test
At low dust concentrations, this is achieved by: D3154 Test Method for Average Velocity in a Duct (Pitot
1.2.1 Exercising extreme care in weighing, Tube Method)
1.2.2 Extendingthesamplingtimeatconventionalsampling D3631 Test Methods for Measuring Surface Atmospheric
rates, or Pressure
1.2.3 Sampling at higher rates at conventional sampling D3670 Guide for Determination of Precision and Bias of
times (high-volume sampling). Methods of Committee D-22
1.3 This test method differs from Test Method D3685/ C3685/D3685M Test Methods for Sampling and Determi-
D3685M by requiring the mass measurement of filter blanks, nation of Particulate Matter in Stack Gases
specifying weighing procedures, and requiring monitoring of D3796 Practice for Calibration of Type S Pitot Tubes
the flue gas flow variability over the testing period. It requires D4536 Test Method for High-Volume Sampling for Solid
that the particulate matter collected on the sample filter have a Particulate Matter and Determination of Particulate Emis-
mass at least five times a positive mass difference on the filter sions
blank.Highvolumesamplingtechniquesoranextensionofthe E1 Specification for ASTM Thermometers
sampling time may be employed to satisfy this requirement. 2.2 ISO Standards:
1.4 This test method may be used for calibration of auto- ISO 5725 Precision of test methods — Determination of
matedmonitoringsystems(AMS).Iftheemissiongascontains repeatability and reproducibility by inter-laboratory tests
unstable, reactive, or semi-volatile substances, the measure- ISO 9096 Stationary source emissions — Determination of
ment will depend on the filtration temperature, and in-stack concentrationandmassflowrateofparticulatematerialin
methods may be more applicable than out-stack methods for gas-carrying ducts. Manual gravimetric method
the calibration of automated monitoring systems. ISO 10780 Stationary source emissions — Measurement of
1.5 This standard does not purport to address all of the velocity and volume flow rate of gas stream in ducts
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 3.1 Fordefinitionsoftermsusedinthistestmethod,referto
Terminology D1356.
bility of regulatory limitations prior to use.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 filtration temperature—the temperature of the
This test method is under the jurisdiction of ASTM Committee D-22 on sampled gas immediately downstream of the filter.
Sampling andAnalysis ofAtmospheres and is the direct responsibility of Subcom-
mittee D22.03 on Ambient Atmosphere and Source Emissions.
Current edition approved October 10, 1998. Published December 1998. Annual Book of ASTM Standards, Vol 11.01.
2 4
ThistestmethodisbasedonISO/CD12141.3,“StationarySourceEmissions— Annual Book of ASTM Standards, Vol 11.03.
Determination of Mass Concentration of Particulate Matter (Dust) at Low Annual Book of ASTM Standards, Vol 14.03.
Concentrations—Manual Gravimetric Method”, available from International Orga- AvailablefromInternationalOrganizationforStandardization,CasaPostals56,
nization for Standardization, Casa Postale 56, CH-1211, Geneva Switzerland. CH-1211, Geneva, Switzerland.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6331
3.2.2 high volume sampling—sampling at higher rates than collected is subsequently measured. The particulate matter
typical in Test Methods D3685/D3685M by using larger (dust) entrained in the gas sample is separated by a pre-
diameter nozzles and higher flow rates to maintain isokinetic weighed filter, which is then dried and reweighed. Deposits
sampling conditions. upstream of the filter in the sampling equipment are also
3.2.2.1 Discussion—Nozzle sizes are typically 20 to 50 recovered and weighed. The increase of mass of the filter and
mm, with corresponding flow rates from 5 to 50 m /s. the deposited mass upstream of the filter plus the deposits
3.2.3 hydraulic diameter, d collected upstream of the filter are attributed to particulate
h
mattercollectedfromthesampledgas.Theratioofthemassof
43 area of sampling plane
d 5 (1)
h the particulate matter collected to the volume of gas collected
perimeter of sampling plane
allows for the calculation of the flue gas particulate concen-
3.2.4 in-stackfiltration—filtrationinthestackorductwhere
tration.
thefilterinitsfilterhousingisplacedimmediatelydownstream
4.2 Valid measurements can be achieved only when:
of the sampling nozzle and collects particulate matter in the
4.2.1 The gas stream in the duct at the sampling plane has a
flue gas, under flue gas conditions.
sufficiently steady and identified velocity, a sufficient tempera-
3.2.5 measurement series—successive measurements car-
ture and pressure, and a sufficiently homogeneous composi-
ried out at the same sampling plane and at the same process
tion;
conditions.
4.2.2 The flow of the gas is parallel to the centerline of the
3.2.6 out-stack filtration—a sampling technique where the
duct across the whole sampling plane;
filter, in its filter housing, collects particulate matter under
4.2.3 Sampling is carried out without disturbance of the gas
controlled temperature conditions outside of the stack or duct.
stream, using a sharp edged nozzle facing into the stream;
3.2.7 overall blank—thesampletakeninamanneridentical
4.2.4 Isokinetic sampling conditions are maintained
to the flue gas test samples, except that the sampling duration
throughout the test;
is shortened to less than 1 min.
4.2.5 Samples are taken at a preselected number of stated
3.2.7.1 Discussion—Theoverallblankvalueisexpressedin
positions in the sampling plane to obtain a representative
thesameunitsasthemeasurementresult(forexample,mg/m )
sample for a non-uniform distribution of particulate matter in
using the average sampling volume of the measurement series.
the duct or stack.
The overall blank includes possible deposits on the filter and
4.2.6 The sampling train is designed and operated to avoid
surfaces upstream of the filter in contact with the sample gas.
condensation and to be leak free;
3.2.8 particulate matter (dust)—solid particles of any
4.2.7 Dust deposits upstream of the filter are recovered or
shape, structure, or density dispersed in the gas phase at flue
taken into account, or both; and
gas temperature and pressure conditions.
4.2.8 The sampling and weighing procedures are adapted to
3.2.8.1 Discussion—According to the described test
the expected dust quantities.
method, all material that may be collected by filtration under
specifiedconditionsandthatremainsupstreamofthefilterand
5. Significance and Use
on the filter after drying under specified conditions are consid-
ered to be particulate matter. However, for the purposes of
5.1 The measurement of particulate matter and collected
some regulatory standards, the definition of particulate matter
residue emission rates is an important test method widely used
may extend to condensibles or reacted materials collected
in the practice of air pollution control. Particulate matter
under specified conditions (for example, specified temperature
measurements after control devices are necessary to determine
lower than the flue gas temperature).
total emission rates into the atmosphere.
3.2.9 sampling line—the line in the sampling plane along
5.1.1 These measurements, when approved by federal or
which the sampling points are located bounded by the inner
state agencies, are often required for the purpose of determin-
duct wall.
ing compliance with regulations and statutes.
3.2.10 sampling plane—the plane normal to the centerline
5.1.2 The measurements made before and after control
of the duct at the sampling position.
devices are often necessary to demonstrate conformance with
3.2.11 sampling point—the specific position on a sampling
contractual performance specifications.
line at which a sample is extracted.
5.2 The collected residue obtained with this test method is
3.2.12 weighing control procedures—quality control proce-
also important in characterizing stack emissions. However, the
duresutilizedfordetecting/correctingapparentmassvariations
utility of these data is limited unless a chemical analysis of the
due to climatic or environmental changes between pre- and
collected residue is performed.
post-sampling weighing series.
5.3 These measurements also can be used to calibrate
3.2.12.1 Discussion—Inthisprocedure,controlparts,which
continuous particulate emission monitoring systems by corre-
are identical to those to be weighed for dust measurement and
lating the output of the monitoring instruments with the data
arepretreatedunderthesameconditions,areused.Thecontrol
obtained by using this test method.
parts are kept free from dust contamination.
5.3.1 This test method is useful in such correlation applica-
tions when emissions are less than 20 mg/m .
4. Summary of Test Method
5.3.2 The correlation test method is most valid when the
4.1 A sample stream of the gas is extracted for a measured monitoring instrumentation samples the particulate matter
period of time at a controlled flow rate, and the volume of gas under the same test conditions as this test method.
D6331
6. Interferences 7.2.3 Iftheaboverequirementscannotbemet,thesampling
location will not be in compliance with this test method (see
6.1 Gaseous species present in stack gases that are capable
11.9.1).
of reacting to form particulate matter within the sample train
7.3 Minimum Number and Location of Sampling Points:
can result in positive interference.
7.3.1 SeeTestMethodD3154,Section8,Figs.7and8,and
6.1.1 Examples include the potential reaction of sulfur
Tables 1 and 2.
dioxide(SO )toaninsolublesulfatecompoundinthemoisture
7.4 Access Ports:
portion of the system (such as with limestone in flue gas
7.4.1 Provide sampling ports for access to the sampling
following a wet flue gas desulfurization system (FGDS) to
points selected, in accordance with 7.3 and Test Method
form calcium sulfate (CaSO ) or the reaction with ammonia
D3154.
gas (NH ) to form ammonium sulfate (NH ) SO and the
3 4 2 4
7.4.2 Ensure that the port dimensions offer ample space for
potential reaction of hydrogen fluoride (HF) with glass com-
the insertion and removal of the sampling equipment and
ponents in the sample train with resultant collection of silicon
associated devices.
tetrafluoride (SiF ) in the impingers.
6.2 Volatile matter existing in solid or liquid form in the
8. Velocity and Gas Composition Measurement
stack gas may vaporize after collection on the sample train
Apparatus
filtration material due to continued exposure to the hot sample
8.1 See Section 6, Test Method D3154
stream during the sampling period. Such an occurrence would
result in a negative interference. See Also Appendix X1.
9. Sampling Apparatus
7. Requirements for Sampling Plane and Sampling
9.1 Sampling Train—For schematic drawings of the major
Points
sampling train components refer to Fig. 1 for the in-stack
7.1 Representative sampling is possible when a suitable method and Fig. 2 for the out-of-stack method.
location that has sufficiently homogeneous gas velocity at the 9.1.1 The materials of construction of in-stack and certain
sampling plane is available. out-of-stack components (such as the nozzle, probe, unions,
7.1.1 Perform sampling at a sufficient number of sampling filter holder, gaskets, and other seals) shall be constructed of
points, which are usually located on several sampling lines. materials that will withstand corrosive or otherwise reactive
Convenient access ports and a working platform are required components or properties of the stack or gas stream, or both.
for the testing. See Test Method D3685/D3685M for addi- Recommended materials for a normal range of stack and
tional criteria. sample conditions include PFTE fluoro hydrocarbons (up to
7.2 Sampling Plane: 175°C), 316 stainless steel (up to 800°C), and some resistant
7.2.1 The sampling plane shall be situated in a length of silicone materials (up to 150°C). Extreme temperature condi-
straight duct (preferably vertical) with a constant shape and tions may require the use of materials such as quartz or a
constant cross-sectional area.The sampling shall be conducted nickel-chromium alloy, or a water-cooled probe may be used.
asfardownstreamandupstreamfromanyobstructionthatmay 9.2 Elements of the Sampling Train—Thesamplingtrainfor
cause a disturbance and produce a change in the direction of collecting particulate matter and collected residue from a gas
flow (disturbances can be caused by bends, fans, or control stream flowing through a stack consists of the following
equipment). interconnected elements:
7.2.2 Measurementsatallthesamplingpointsdefinedin7.3 9.3 Nozzles—The first part of the sampling equipment to
shall prove that the gas stream at the sampling plane meets the encounterthedustormoisture-ladengasstream,orboth,isthe
following requirements: nozzle. To extract a representative sample of gas and particu-
7.2.2.1 The angle of gas flow is less than 15° with regard to late matter, the nozzle used for sampling shall be within a
theductaxis(methodforestimationisindicatedinAnnexCof narrow range of inside diameters.
ISO 10780); 9.3.1 The probe nozzle is provided with a sharp, tapered
7.2.2.2 No local negative flow is present; leadingedgeandisconstructedofeitherseamless316stainless
7.2.2.3 The minimum velocity is measurable by the test steel tubing or glass formed in a button-hook or elbow
metho
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