METHOD 5A -
DETERMINATION OF PARTICULATE MATTER EMISSIONS FROM THE ASPHALT PROCESSING AND
ASPHALT ROOFING INDUSTRY
NOTE: This method does not include all of the
specifications (e.g.,
equipment and supplies) and procedures (e.g., sampling and analytical) essential to its
performance. Some material is incorporated by reference from other methods in
this part. Therefore, to obtain reliable results, persons using this method
should have a thorough knowledge of at least the following additional test
methods: Method 1, Method 2,
Method 3, and Method 5.
8.0. Sample Collection,
Preservation, Storage, and Transport.
8.2 Preliminary
Determinations.
8.3 Preparation of
Sampling Train.
8.6 Calculation of
Percent Isokinetic.
9.1 Miscellaneous
Quality Control Measures. Section Quality Control Measures
10.0 Calibration and
Standardization.
12.0 Data Analysis and
Calculations.
12.2 Dry Gas Meter
Temperature, Orifice Pressure Drop, and Dry Gas Volume.
13.0 Method
Performance. [Reserved]
14.0 Pollution
Prevention. [Reserved]
15.0 Waste Management.
[Reserved]
17.0 Tables, Diagrams,
Flowcharts, and Validation Data.
1.0 Scope and Applications.
1.1 Analyte.
Particulate matter (PM). No CAS number assigned.
1.2 Applicability.
This method is applicable for the determination of PM emissions from asphalt
roofing industry process saturators, blowing stills, and other sources as
specified in the regulations.
1.3 Data Quality
Objectives. Adherence to the requirements of this method will enhance the
quality of the data obtained from air pollutant sampling methods.
2.0 Summary of Method.
Particulate matter is
withdrawn isokinetically from the source and collected on a glass fiber filter
maintained at a temperature of 42 ± 10 ¡C (108 ± 18 ¡F). The PM mass, which
includes any material that condenses at or above the filtration temperature, is
determined gravimetrically after the removal of uncombined water.
3.0 Definitions. [Reserved]
4.0 Interferences. [Reserved]
5.0 Safety.
5.1 Disclaimer. This
method may involve hazardous materials, operations, and equipment. This test
method may not address all of the safety problems associated with its use. It
is the responsibility of the user of this test method to establish appropriate
safety and health practices and to determine the applicability of regulatory
limitations prior to performing this test method.
6.0 Equipment and Supplies.
6.1 Sample Collection.
Same as Method 5, Section 6.1, with the following
exceptions and additions:
6.1.1 Probe Liner.
Same as Method 5,
Section 6.1.1.2, with the note that at high stack gas temperatures greater than
250 ¡C (480 ¡F), water-cooled probes may be required to control the probe exit
temperature to 42 ± 10 ¡C
(108 ± 18 ¡F).
6.1.2 Precollector Cyclone.
Borosilicate glass
following the construction details shown in Air Pollution Technical Document
(APTD)-0581, "Construction Details of Isokinetic Source-Sampling
Equipment" (Reference 2 in Method 5,
Section 17.0).
NOTE: The cyclone shall be used when the stack gas
moisture is greater than 10 percent, and shall not be used otherwise.
6.1.3 Filter Heating System.
Any heating (or
cooling) system capable of maintaining a sample gas temperature at the exit end
of the filter holder during sampling at 42 ± 10 ¡C (108 ± 18 ¡F).
6.2 Sample Recovery.
The following items
are required for sample recovery:
6.2.1 Probe-Liner and
Probe-Nozzle Brushes, Graduated Cylinder and/or Balance, Plastic Storage
Containers, and Funnel and Rubber Policeman. Same as in Method 5, Sections 6.2.1, 6.2.5, 6.2.6, and
6.2.7, respectively.
6.2.2 Wash Bottles.
Glass.
6.2.3 Sample Storage
Containers. Chemically resistant 500-ml or 1,000-ml borosilicate glass bottles,
with rubber-backed Teflon screw cap liners or caps that are constructed so as
to be leak-free, and resistant to chemical attack by 1,1,1-trichloroethane
(TCE). (Narrow-mouth glass bottles have been found to be less prone to
leakage.)
6.2.4 Petri Dishes.
Glass, unless otherwise specified by the Administrator.
6.2.5 Funnel. Glass.
6.3 Sample Analysis.
Same as Method 5,
Section 6.3, with the following additions:
6.3.1 Beakers. Glass,
250-ml and 500-ml.
6.3.2 Separatory
Funnel. 100-ml or greater.
7.0. Reagents and Standards.
7.1 Sample Collection.
The following
reagents are required for sample collection:
7.1.1 Filters, Silica
Gel, Water, and Crushed Ice. Same as in Method
5, Sections 7.1.1, 7.1.2, 7.1.3, and 7.1.4, respectively.
7.1.2 Stopcock
Grease. TCE-insoluble, heat-stable grease (if needed). This is not necessary if
screw-onconnectors with Teflon sleeves, or similar, are used.
7.2 Sample Recovery.
Reagent grade TCE, ²
0.001 percent residue and stored in glass bottles. Run TCE blanks before field
use, and use only TCE with low blank values (²0.001 percent). In no case shall
a blank value of greater than 0.001 percent of the weight of TCE used be
subtracted from the sample weight.
7.3 Analysis.
Two reagents are
required for the analysis:
7.3.1 TCE. Same as in
Section 7.2.
7.3.2 Desiccant. Same
as in Method 5, Section 7.3.2.
8.0. Sample Collection, Preservation, Storage, and Transport.
8.1. Pretest Preparation.
Unless otherwise
specified, maintain and calibrate all components according to the procedure
described in APTD-0576, "Maintenance, Calibration, and Operation of
Isokinetic Source-Sampling Equipment" (Reference
3 in Method 5, Section 17.0).
8.1.1 Prepare probe
liners and sampling nozzles as needed for use. Thoroughly clean each component
with soap and water followed by a minimum of three TCE rinses. Use the probe
and nozzle brushes during at least one of the TCE rinses (refer to Section 8.7
for rinsing techniques). Cap or seal the open ends of the probe liners and
nozzles to prevent contamination during shipping.
8.1.2 Prepare silica
gel portions and glass filters as specified in Method
5, Section 8.1.
8.2 Preliminary Determinations.
Select the sampling
site, probe nozzle, and probe length as specified in Method 5, Section 8.2.
Select a total sampling time greater than or equal to the minimum total sampling
time specified in the "Test Methods and Procedures" section of the
applicable subpart of the regulations. Follow the guidelines outlined in Method 5, Section 8.2 for sampling time per
point and total sample volume collected.
8.3 Preparation of Sampling Train.
Prepare the sampling
train as specified in Method 5, Section 8.3,
with the addition of the precollector cyclone, if used, between the probe and
filter holder. The temperature of the precollector cyclone, if used, should be
maintained in the same range as that of the filter, i.e., 42 ± 10 ¡C (108 ± 18 ¡F). Use no stopcock
grease on ground glass joints unless grease is insoluble in TCE.
8.4 Leak-Check Procedures.
Same as Method 5, Section 8.4.
8.5 Sampling Train Operation.
Operate the sampling
train as described in Method 5, Section 8.5,
except maintain the temperature of the gas exiting the filter holder at 42 ±
10 ¡C (108 ± 18 ¡F).
8.6 Calculation of Percent Isokinetic.
Same as Method 5, Section 8.6.
8.7 Sample Recovery.
Same as Method 5, Section 8.7.1 through 8.7.6.1, with
the addition of the following:
8.7.1 Container No. 2
(Probe to Filter Holder).
8.7.1.1 Taking care
to see that material on the outside of the probe or other exterior surfaces
does not get into the sample, quantitatively recover PM or any condensate from
the probe nozzle, probe fitting, probe liner, precollector cyclone and
collector flask (if used), and front half of the filter holder by washing these
components with TCE and placing the wash in a glass container. Carefully measure the total amount of
TCE used in the rinses. Perform the TCE rinses as described in Method 5, Section 8.7.6.2, using TCE instead
of acetone.
8.7.1.2 Brush and
rinse the inside of the cyclone, cyclone collection flask, and the front half
of the filter holder. Brush and rinse each surface three times or more, if
necessary, to remove visible PM.
8.7.2 Container No. 3
(Silica Gel). Same as in Method 5, Section 8.7.6.3.
8.7.3 Impinger Water.
Same as Method 5, Section 8.7.6.4.
8.8 Blank.
Save a portion of the
TCE used for cleanup as a blank. Take 200 ml of this TCE directly from the wash
bottle being used, and place it in a glass sample container labeled "TCE
Blank."
9.0 Quality Control.
9.1 Miscellaneous Quality Control Measures. Section Quality Control
Measures
9.2 Quality Control Check
A quality control (QC)
check of the volume metering system at the field site is suggested before
collecting the sample. Use the procedure outlined in Method 5, Section 9.2.
10.0 Calibration and Standardization.
Same as Method 5, Section 10.0.
11.0 Analytical Procedures.
11.1 Analysis.
Record the data
required on a sheet such as the one shown in Figure 5A-1.
Handle each sample container as follows:
11.1.1 Container No.
1 (Filter). Transfer the filter from the sample container to a tared glass
weighing dish, and desiccate for 24 hours in a desiccator containing anhydrous
calcium sulfate. Rinse Container No. 1 with a measured amount of TCE, and
analyze this rinse with the contents of Container No. 2. Weigh the filter to a
constant weight. For the purpose of this analysis, the term "constant
weight" means a difference of no more than 10 percent of the net filter
weight or 2 mg (whichever is greater) between two consecutive weighings made 24
hours apart. Report the "final weight" to the nearest 0.1 mg as the
average of these two values.
11.1.2 Container No.
2 (Probe to Filter Holder).
11.1.2.1 Before
adding the rinse from Container No. 1 to Container No. 2, note the level of
liquid in Container No. 2, and confirm on the analysis sheet whether leakage
occurred during transport. If noticeable leakage occurred, either void the
sample or take steps, subject to the approval of the Administrator, to correct
the final results.
11.1.2.2 Add the
rinse from Container No. 1 to Container No. 2 and measure the liquid in this
container either volumetrically to ±1 ml or gravimetrically to ±0.5 g. Check to
see whether there is any appreciable quantity of condensed water present in the
TCE rinse (look for a boundary layer or phase separation). If the volume of
condensed water appears larger than 5 ml, separate the oil- TCE fraction from
the water fraction using a separatory funnel. Measure the volume of the water
phase to the nearest ml; adjust the stack gas moisture content, if necessary
(see Sections 12.3 and 12.4). Next, extract the water phase with several 25-ml
portions of TCE until, by visual observation, the TCE does not remove any
additional organic material. Transfer the remaining water fraction to a tared
beaker and evaporate to dryness at 93 ¡C (200 ¡F), desiccate for 24 hours, and
weigh to the nearest 0.1 mg.
11.1.2.3 Treat the
total TCE fraction (including TCE from the filter container rinse and water
phase extractions) as follows: Transfer the TCE and oil to a tared beaker, and
11.1.3 Container No.
3 (Silica Gel). This step may be conducted in the field. Weigh the spent silica
gel (or silica gel plus impinger) to the nearest 0.5 g using a balance.
11.1.4 "TCE
Blank" Container. Measure TCE in this container either volumetrically or
gravimetrically. Transfer the TCE to a tared 250-ml beaker, and evaporate to
dryness at ambient temperature and pressure. Desiccate for 24 hours, and weigh
to a constant weight. Report the results to the nearest 0.1 mg.
NOTE: In order to facilitate the evaporation of TCE
liquid samples, these samples may be dried in a controlled temperature oven at
temperatures up to 38 ¡C (100 ¡F) until the liquid is evaporated.
12.0 Data Analysis and Calculations.
Carry out
calculations, retaining at least one extra significant figure beyond that of
the acquired data. Round off figures after the final calculation. Other forms of
the equations may be used as long as they give equivalent results.
12.1 Nomenclature.
Same as Method 5, Section 12.1, with the following
additions:
Ct = TCE blank residue concentration, mg/g.
mt = Mass of residue of TCE blank after evaporation, mg.
Vpc = Volume of water collected in precollector, ml.
Vt = Volume of TCE blank, ml.
Vtw = Volume of TCE used in wash, ml.
Wt = Weight of residue in TCE wash, mg.
¥ t = Density of TCE (see label on bottle), g/ml.
12.2 Dry Gas Meter Temperature, Orifice Pressure Drop, and Dry Gas Volume.
Same as Method 5,
Sections 12.2 and 12.3, except use data obtained in performing this test.
12.3 Volume of Water Vapor.
where:
K2 = 0.001333 m3/ml for metric units.
= 0.04706 ft3/ml for English units.
12.4 Moisture Content.
NOTE: In saturated or water droplet-laden gas streams,
two calculations of the moisture content of the stack gas shall be made, one
from the impinger and precollector analysis (Equations 5A-1 and 5A-2) and a
second from the assumption of saturated conditions. The lower of the two values
of moisture content shall be considered correct. The procedure for determining
the moisture content based upon assumption of saturated conditions is given in Section 4.0 of Method 4. For the purpose of this
method, the average stack gas temperature from Figure
5-3 of Method 5 may be used to make this determination, provided that the
accuracy of the in-stack temperature sensor is within 1 ¡C (2 ¡F).
12.5 TCE Blank Concentration.
NOTE: In no case shall a blank value of greater than 0.001
percent of the weight of TCE used be subtracted from the sample weight.
12.6 TCE Wash Blank.
12.7 Total PM Weight.
Determine the total
PM catch from the sum of the weights obtained from Containers 1 and 2, less the
TCE blank.
12.8 PM Concentration.
where: K3 = 0.001 g/mg for metric units
= 0.0154 gr/mg for English units
12.9 Isokinetic Variation.
Same as in Method 5, Section 12.11.
13.0 Method Performance. [Reserved]
14.0 Pollution Prevention. [Reserved]
15.0 Waste Management. [Reserved]
16.0 References.
Same as Method 5, Section 17.0.
17.0 Tables, Diagrams, Flowcharts, and Validation Data.
