STACK SAMPLING 1121
to be analyzed along with the actual samples. The address
for obtaining these samples is included in the Method.
As with all of these Test Methods, they should only be
attempted by properly trained individuals, using appropriate
equipment.Test Method 111Test Method 111 is used for measuring the emissions of
Polonium (Po)-210 in stack gases. The sampling is exactly
as in Method 5. In the analysis, the particulate Po-210 is
dissolved in solution and deposited on a silver disc. The
radioactive disintegration rate is measured using an alpha
spectrometry system.
After sampling using the Method 5 train and techniques,
the filter containing the sample is prepared for analysis. Care
must be taken to complete analysis within 30 days of sam-
pling to ensure that the results are not biased high as the
result of decay of lead 210.
Sample preparation consists of repeated dissolution of
the sample filter in concentrated hydrofluoric acid and heat-
ing to dryness until the filter is gone. The sample is then
dissolved in a mixed acid solution and prepared for screen-
ing. The screening is designed to determine the approxi-
mate radioactivity of the sample, allowing the selection of
an appropriate sample concentration to protect the detec-
tor. Once the aliquot size is chosen, an amount of Pb-209 is
added in approximately equal activity. This will be used to
assess Po recovery in the spectrometry system.
A specially prepared 3.8 cm silver disc, with one side
painted to prevent deposition, is suspended in the heated
sample solution for 3 hours. After rinsing in distilled water, the
disc is placed in the alpha spectrometry system and its emis-
sions counted for 1000 minutes. The picocuries of Po- 210 per
filter are then calculated from the counts in the Po-210 region,
the counts of Po-209, and the Po recovery, based on the Po-209
counts.
The emission rate of Po-210 is then calculated based
on the stack flow rate, as measured by Method 2. In most
cases, the emission rate desired would be for rock processing
plants, such as for phosphate rock. In that case, the process-
ing rate is placed in the denominator or the rate equation.
Detailed procedures for all typical calculations are included
in the Method.
Several quality assurance steps are required by this
method. First, the Alpha Spectrometry System must be stan-
dardized. This is accomplished by filtering a standardized
solution of a different alpha-emitting actinide element and
exposing the detector to the dried filter. Second a standard-
ized Po-209 solution must be filtered and exposed to the
detector in the same way. Next, each sample is analyzed in
duplicate, with the difference between pairs required to be
below stated limits. Finally, an independent analyst, under
the direction of the Quality Assurance Officer for the testing
project, should prepare a performance evaluation sample of
Po, unknown to the analyst, for every 10 samples analyzed.
As with all of the Test Methods, Method III should not be
attempted by anyone not trained to perform stack sampling.In particular, the analysis should only be performed by
individuals experienced in dealing with radioactive sample
analyses and hydrofluoric acid digestion.Method 0010 (Modified Method 5)Modified Method 5, or MM5, as it is usually called is used
for Resource Conservation and Recovery Act (RCRA) trial
burns to determine semi-volatile organic emissions from
hazardous waste incinerators. This method, under the desig-
nation method 0010, can be found in SW-846.
In many ways, the equipment and operation of this
train are similar to Test Method 5. A sample is extracted iso-
kinetically from the stack and filtered to collect particulate
material. In addition, the gases are cooled in a condenser
and then trapped with Amberlite XAD-2 resin. A methy-
lene chloride/methanol mixture is used for the probe wash
instead of acetone.
The semi-volatile compounds on the filter and XAD-2
resin are extracted using an appropriate continuous extractor,
and are concentrated for analysis. The condensate in the first
impinger and, if required, the contents of the other impinger,
are extracted using a separatory funnel and concentrated for
analysis. The solvent rinses from the train are concentrated
for analysis.
Analysis of these samples is done using Method 8270
which is also found in SW-846. The discussion of this
method is beyond the scope of the next.
Modified Method 5 contains detailed descriptions of the
quality control, calibration procedures, and sampling proce-
dures in addition to a list of references. It should be read
in detail before the Method is attempted. Testing should be
performed only by personnel trained and experienced with
the equipment being used.Test Method 0030 Volatile Organic Sampling
Train (VOST)The Volatile Organic Sampling Train (VOST) is used to col-
lect volatile organic compounds during resource Conservation
and Recovery Act (RCRA) trial burns. This method can be
found in SW-846 as Method 0030. It provides for the collec-
tion of gas samples in a pair of sorbent traps with subsequent
desorption, concentration, and analysis of the contents of
each tube. This method has been validated for many organic
compounds boiling between 30°C and 100°C. This method
should not be used for low boiling chlorofluorocarbons.
Compounds which are water soluble may not be purged
from the condensate completely and therefore should not be
analyzed by this method. This method has been successfully
used for some compounds boiling higher than 100°C.
In this method, a 20 liter gas sample is extracted from
the stack with a glass lined probe at the rate of either 1 liter/
minute or 0.5 liter/minute. Samples are collected from the
center of the stack, not isokinetically. The sample gas is
cooled with a condenser that has ice water pumped through
it. The objective is to cool the gas to below 20ºC before the
organic components are adsorbed onto a pair of sorbent resinC019_003_r03.indd 1121C019_003_r03.indd 1121 11/18/2005 11:07:18 AM11/18/2005 11:07:18 AM