METHOD 5E -
DETERMINATION OF PARTICULATE MATTER EMISSIONS FROM THE WOOL FIBERGLASS
INSULATION MANUFACTURING 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.
5.2.1 Hydrochloric Acid
(HCl). Highly toxic.
5.2.2 Sodium Hydroxide
(NaOH).
8.0 Sample Collection,
Preservation, Storage, and
8.1 Pretest Preparation
and Preliminary Determinations.
8.2 Preparation of
Sampling Train.
8.3 Leak-Check
Procedures, Sampling Train Operation, Calculation of Percent Isokinetic.
9.1 Miscellaneous
Quality Control Measures.
9.2 Volume Metering
System Checks.
10.0 Calibration and
Standardization.
10.1 Preparation of
Organic Carbon Standard Curve.
10.2 Preparation of
Inorganic Carbon Standard Curve.
12.0 Data Analysis and
Calculations.
12.2 Concentration of
Condensed TOC in Liquid Sample.
12.3 Mass of Condensed
TOC Collected.
12.4 Concentration of
Condensed Particulate Material.
12.5 Total Particulate
Concentration.
13.0 Method
Performance. [Reserved]
14.0 Pollution
Prevention. [Reserved]
15.0 Waste Management.
[Reserved]
17.0 Tables, Diagrams,
Flowcharts, and Validation Data.
[Reserved]
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 wool fiberglass insulation manufacturing
sources.
2.0 Summary of Method.
Particulate matter is
withdrawn isokinetically from the source and is collected either on a glass
fiber filter maintained at a temperature in the range of 120 ± 14 ¡C (248 ± 25
¡F) and in impingers in solutions of 0.1 N sodium hydroxide (NaOH). The
filtered particulate mass, which includes any material that condenses at or
above the filtration temperature,
is determined gravimetrically after the removal of uncombined water. The
condensed PM collected in the impinger solutions is determined as total organic
carbon (TOC) using a nondispersive infrared type of analyzer. The sum of the
filtered PM mass and the condensed PM is reported as the total PM mass.
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.
5.2 Corrosive Reagents.
The following
reagents are hazardous. Personal
protective equipment and safe procedures are useful in preventing chemical
splashes. If contact occurs, immediately flush with copious amounts of water at
least 15 minutes. Remove clothing under shower and decontaminate. Treat
residual chemical burn as thermal burn.
5.2.1 Hydrochloric Acid (HCl). Highly toxic.
Vapors are highly
irritating to eyes, skin, nose,
and lungs, causing severe damage.
May cause bronchitis, pneumonia,
or edema of lungs. Exposure to concentrations of 0.13 to 0.2 percent in
air can be lethal in minutes. Will react with metals, producing hydrogen.
5.2.2 Sodium Hydroxide (NaOH).
Causes severe damage
to eye tissues and to skin. Inhalation causes irritation to nose, throat, and
lungs. Reacts exothermically with limited amounts of water.
6.0 Equipment and Supplies.
6.1 Sample Collection.
Same as Method 5, Section 6.1, with the exception of the
following:
6.1.1 Probe Liner.
Same as described in Section 6.1.1.2 of Method 5 except use only borosilicate
or quartz glass liners.
6.1.2 Filter Holder.
Same as described in Section 6.1.1.5 of Method 5 with the addition of a
leak-tight connection in the rear half of the filter holder designed for
insertion of a temperature sensor used for measuring the sample gas exit
temperature.
6.2 Sample Recovery.
Same as Method 5, Section 6.2, except three wash
bottles are needed instead of two and only glass storage bottles and funnels
may be used.
6.3 Sample Analysis.
Same as Method 5, Section 6.3, with the additional
equipment for TOC analysis as described below:
6.3.1 Sample Blender
or Homogenizer. Waring type or ultrasonic.
6.3.2 Magnetic
Stirrer.
6.3.3 Hypodermic
Syringe. 0- to 100-µl capacity.
6.3.4 Total Organic
Carbon Analyzer. Rosemount Model 2100A analyzer or equivalent and a recorder.
6.3.5 Beaker. 30-ml.
6.3.6 Water Bath.
Temperature controlled.
6.3.7 Volumetric
Flasks. 1000-ml and 500-ml.
7.0 Reagents and Standards.
Unless otherwise
indicated, it is intended that all reagents conform to the specifications
established by the Committee on Analytical Reagents of the American Chemical
Society, where such specifications are available; otherwise, use the best
available grade.
7.1 Sample Collection.
Same as Method 5, Section 7.1, with the addition of 0.1 N NaOH (Dissolve 4 g
of NaOH in water and dilute to 1 liter).
7.2 Sample Recovery.
Same as Method 5, Section 7.2, with the addition of the
following:
7.2.1 Water.
Deionized distilled to conform to ASTM Specification D 1193-77 or 91 Type 3
(incorporated by reference - see ¤60.17). The potassium permanganate (KMnO4) test for oxidizable organic matter may be omitted when high
concentrations of organic matter are not expected to be present.
7.2.2 Sodium
Hydroxide. Same as described in Section 7.1.
7.3 Sample Analysis.
Same as Method 5,
Section 7.3, with the addition of the following:
7.3.1 Carbon
Dioxide-Free Water. Distilled or deionized water that has been freshly boiled
for 15 minutes and cooled to room temperature while preventing exposure to
ambient air by using a cover vented with an Ascarite tube.
7.3.2 Hydrochloric
Acid. HCl, concentrated, with a dropper.
7.3.3 Organic Carbon
Stock Solution. Dissolve 2.1254 g of dried potassium biphthalate (HOOCC6H4COOK) in CO2-free
water, and dilute to 1 liter in a volumetric flask. This solution contains 1000
mg/L organic carbon.
7.3.4 Inorganic
Carbon Stock Solution. Dissolve 4.404 g anhydrous sodium carbonate (Na2CO3) in about 500 ml of CO2-free water in a 1-liter volumetric flask. Add 3.497 g anhydrous
sodium bicarbonate (NaHCO3) to the flask, and dilute to 1 liter with CO2-free water. This solution contains 1000 mg/L inorganic carbon.
7.3.5 Oxygen Gas. CO2-free.
8.0 Sample Collection, Preservation, Storage, and Transport.
8.1 Pretest Preparation and Preliminary Determinations.
Same as Method 5, Sections 8.1 and 8.2, respectively.
8.2 Preparation of Sampling Train.
Same as Method 5,
Section 8.3, except that 0.1 N NaOH
is used in place of water in the impingers. The volumes of the solutions are
the same as in Method 5.
8.3 Leak-Check Procedures, Sampling Train Operation, Calculation of Percent Isokinetic.
Same as Method 5, Sections 8.4 through 8.6,
respectively.
8.4 Sample Recovery.
Same as Method 5, Sections 8.7.1 through 8.7.4, with
the addition of the following:
8.4.1 Save portions
of the water, acetone, and 0.1 N NaOH used for cleanup as blanks. Take 200 ml
of each liquid directly from the wash bottles being used, and place in glass
sample containers labeled "water blank," "acetone blank,"
and "NaOH blank," respectively.
8.4.2 Inspect the
train prior to and during disassembly, and note any abnormal conditions. Treat
the samples as follows:
8.4.2.1 Container No.
1. Same as Method 5, Section 8.7.6.1.
8.4.2.2 Container No.
2. Use water to rinse the sample nozzle, probe, and front half of the filter
holder three times in the manner described in Section 8.7.6.2 of Method 5
except that no brushing is done. Put all the water wash in one container, seal,
and label.
8.4.2.3 Container No.
3. Rinse and brush the sample nozzle, probe, and front half of the filter
holder with acetone as described for Container No. 2 in Section 8.7.6.2 of
Method 5.
8.4.2.4 Container No.
4. Place the contents of the silica gel impinger in its original container as
described for Container No. 3 in Section 8.7.6.3 of Method 5.
8.4.2.5 Container No.
5. Measure the liquid in the first three impingers and record the volume or
weight as described for the Impinger Water in Section 8.7.6.4 of Method 5. Do
not discard this liquid, but place it in a sample container using a glass
funnel to aid in the transfer from the impingers or graduated cylinder (if
used) to the sample container. Rinse each impinger thoroughly with 0.1 N NaOH
three times, as well as the graduated cylinder (if used) and the funnel, and
put these rinsings in the same sample container. Seal the container and label
to clearly identify its contents.
8.5 Sample Transport.
Whenever possible,
containers should be shipped in such a way that they remain upright at all
times.
9.0 Quality Control.
9.1 Miscellaneous Quality Control Measures.
9.2 Volume Metering System Checks.
Same as Method 5, Section 9.2.
10.0 Calibration and Standardization.
Same as Method 5, Section 10.0, with the addition of
the following procedures for calibrating the total organic carbon analyzer:
10.1 Preparation of Organic Carbon Standard Curve.
10.1.1 Add 10 ml, 20
ml, 30 ml, 40 ml, and 50 ml of the organic carbon stock solution to a series of
five 1000-ml volumetric flasks. Add 30 ml, 40 ml, and 50 ml of the same
solution to a series of three 500-ml volumetric flasks. Dilute the contents of
each flask to the mark using CO2-free water. These
flasks contain 10, 20, 30, 40, 50, 60, 80, and 100 mg/L organic carbon,
respectively.
10.1.2 Use a
hypodermic syringe to withdraw a 20- to 50-µl aliquot from the 10 mg/L standard
solution and inject it into the total carbon port of the analyzer. Measure the
peak height. Repeat the injections until three consecutive peaks are obtained
within 10 percent of their arithmetic mean. Repeat this procedure for the
remaining organic carbon standard solutions.
10.1.3 Calculate the
corrected peak height for each standard by deducting the blank correction (see Section 11.2.5.3) as follows:
Corrected Peak Height = A - B Eq.
5E-1
where:
A = Peak height of
standard or sample, mm or other appropriate unit.
B = Peak height of
blank, mm or other appropriate unit.
10.1.4 Prepare a linear
regression plot of the arithmetic mean of the three consecutive peak heights
obtained for each standard solution against the concentration of that solution.
Calculate the calibration factor as the inverse of the slope of this curve. If
the product of the arithmetic mean peak height for any standard solution and
the calibration factor differs from the actual concentration by more than 5
percent, remake and reanalyze that standard.
10.2 Preparation of Inorganic Carbon Standard Curve.
Repeat the procedures
outlined in Sections 10.1.1 through 10.1.4, substituting the inorganic carbon
stock solution for the organic carbon stock solution, and the inorganic carbon
port of the analyzer for the total carbon port.
11.0 Analytical Procedure.
11.1 Record the data
required on a sheet such as the one shown in Figure
5-6 of Method 5.
11.2 Handle each
sample container as follows:
11.2.1 Container No.
1. Same as Method 5, Section 11.2.1, except
that the filters must be dried at 20 ± 6 ¡C (68 ± 10 ¡F) and ambient pressure.
11.2.2 Containers No.
2 and No. 3. Same as Method 5, Section 11.2.2, except that evaporation of the
samples must be at 20 ± 6 ¡C (68 ± 10 ¡F) and ambient pressure.
11.2.3 Container No.
4. Same as Method 5, Section 11.2.3.
11.2.4 "Water
Blank" and "Acetone Blank" Containers. Determine the water and
acetone blank values following the procedures for the "Acetone Blank"
container in Section 11.2.4 of Method 5. Evaporate the samples at ambient
temperature [20 ± 6 ¡C (68 ± 10 ¡F)] and pressure.
11.2.5 Container No.
5. For the determination of total organic carbon, perform two analyses on
successive identical samples, i.e.,
total carbon and inorganic carbon. The desired quantity is the difference
between the two values obtained. Both analyses are based on conversion of
sample carbon into carbon dioxide for measurement by a nondispersive infrared
analyzer. Results of analyses register as peaks on a strip chart recorder.
11.2.5.1 The
principal differences between the operating parameters for the two channels
involve the combustion tube packing material and temperature. In the total
carbon channel, a high temperature [950 ¡C (1740 ¡F)] furnace heats a Hastelloy
combustion tube packed with cobalt oxide-impregnated asbestos fiber. The oxygen
in the carrier gas, the elevated temperature, and the catalytic effect of the
packing result in oxidation of both organic and inorganic carbonaceous material
to CO2 and steam. In the inorganic carbon channel, a
low temperature [150 ¡C (300 ¡F)] furnace heats a glass tube containing quartz
chips wetted with 85 percent phosphoric acid. The acid liberates CO2 and steam from inorganic carbonates. The operating temperature is
below that required to oxidize organic matter. Follow the manufacturer's
instructions for assembly, testing, calibration, and operation of the analyzer.
11.2.5.2 As samples
collected in 0.1 N NaOH often contain a high measure of inorganic carbon that
inhibits repeatable determinations of TOC, sample pretreatment is necessary.
Measure and record the liquid volume of each sample (or impinger contents). If
the sample contains solids or immiscible liquid matter, homogenize the sample
with a blender or ultrasonics until satisfactory repeatability is obtained.
Transfer a representative portion of 10 to 15 ml to a 30-ml beaker, and acidify
with about 2 drops of concentrated HCl to a pH of 2 or less. Warm the acidified
sample at 50 ¡C (120 ¡F) in a water bath for 15 minutes.
11.2.5.3 While stirring the sample with a magnetic stirrer, use a
hypodermic syringe to withdraw a 20- to 50-µl aliquot from the beaker. Analyze
the sample for total carbon and calculate its corrected mean peak height
according to the procedures outlined in Sections 10.1.2 and 10.1.3. Similarly
analyze an aliquot of the sample for inorganic carbon. Repeat the analyses for
all the samples and for the 0.1 N NaOH blank.
11.2.5.4 Ascertain
the total carbon and inorganic carbon concentrations (CTC and CIC,
respectively) of each sample and blank by comparing the corrected mean peak
heights for each sample and blank to the appropriate standard curve.
NOTE: If samples must be diluted for analysis, apply
an appropriate dilution factor.
12.0 Data Analysis and Calculations.
Same as Method 5, Section 12.0, with the addition of the
following:
12.1 Nomenclature.
Cc = Concentration of condensed particulate matter in stack gas, gas dry
basis, corrected to standard conditions, g/dscm (gr/dscf).
CIC = Concentration of condensed TOC in the liquid
sample, from Section 11.2.5, mg/L.
Ct = Total particulate concentration, dry basis, corrected to standard
conditions, g/dscm (gr/dscf).
CTC = Concentration of condensed TOC in the liquid
sample, from Section 11.2.5, mg/L.
CTOC = Concentration of condensed TOC in the liquid
sample, mg/L.
mTOC = Mass of condensed TOC collected in the
impingers, mg.
Vm(std) = Volume of gas sample measured by the dry gas
meter, corrected to standard conditions, from Section 12.3 of Method 5, dscm
(dscf).
Vs = Total volume of liquid sample, ml.
12.2 Concentration of Condensed TOC in Liquid Sample.
12.3 Mass of Condensed TOC Collected.
where:
0.001 = Liters per
milliliter.
12.4 Concentration of Condensed Particulate Material.
where:
K4 = 0.001 g/mg for metric units.
= 0.0154 gr/mg for
English units.
12.5 Total Particulate Concentration.
13.0 Method Performance. [Reserved]
14.0 Pollution Prevention. [Reserved]
15.0 Waste Management. [Reserved]
16.0 References.
Same as Section 17.0 of Method 5, with the addition of
the following:
1. American Public
Health Association, American Water Works Association, Water Pollution Control
Federation. Standard Methods for the Examination of Water and Wastewater.
Fifteenth Edition. Washington, D.C. 1980.