-------
represent chlorides captured in the probe rinse/filter fraction of the HC1
train and consist of metal chlorides contained in the particulate matter. The
back-half emissions represent gaseous HC1 captured in the sample train
impingers. The train-total emissions represent the sum of the front half and
back half emissions.
As shown in Table 5-11, the average train-total chloride emissions
concentration at stack oxygen levels was approximately 1980 mg/dscm.
Corrected to 3% Qy using the Radian EPA Method 3 data, this corresponds to
approximately 10,700 mg/dscm @ 3% 02. The average train-total chloride mass
emission rate from the waste heat boiler exhaust stack was about 28.4 kg/hr
(62.6 Ib/hr). More than 98 percent of the chlorides was gaseous HC1.
Chloride emissions ranged from 22.2 to 35,8 Kg/hr (48.8 to 78.8 Ib/hr)
for the three test runs. The highest chloride emission rate was for Run 3,
which also showed the highest 2378 TCDD emission rate and had highest feed
rate of wood/plastic cutoffs. Similarly, the lowest chloride emission rate
was for Run 1 which showed the lowest 2378 TCDD emissions and had the lowest
wood/plastic cutoffs feed rate.
5.6 INCINERATOR ASH DIOXIN/FURAN
Table 5-12 shows the run-specific data for the bottom ash samples from
Site ISW-A. The dioxin/furan concentrations varied considerably between the
three runs for which ash samples were analyzed. The Run 03 and 04 ash samples
contained considerably more dioxin/furan than the ash sample collected during
Run 01. The feed during Runs 03 and 04 contained higher percentages of
wood/plastic cutoff which could have contributed to the high dioxin/furan
concentrations in the ash. In addition, during Run 03 the chain-link conveyor
which removes ash from the incinerator failed. The incinerator was operated
until the ash build-up had to be removed. Operating in this mode may have
contributed to the higher dioxin/furan concentrations observed for Run 03.
5-27
-------
TABLE 5-12.
DIOXIN/FURAN CONTIENTS OF INDIVIDUAL
BOTTOM ASH SAMPLES FROM SITE ISW-A
Isomer/
Homo!ogue
Dioxin/Furan Homoloque Contents (oob)
Run 01 Run 03 Run 04 Average
Dioxins
2378-TCDD
Other TCDD
Penta CDD
Hexa CDD
Hepta CDD
Octa-CDD
Total PCDD
NR
ND
ND
0.2
0.5
0.4
1.1
0.2
1.9
2.7
28.4
126.2
143.2
302.6
0.1
1.6
5.0
10.9
44.1
56.6
118.3
0.2
1.2
2.6
13.2
56.9
66.7
140.7
Fur an s
2378-TCDF
Other PCDF
Penta CDF
Hexa CDF
Hepta CDF
Octa-CDF
Total PCDF
NR
ND
ND
ND
0.04
0.03
0.07
ND
1.2
0.9
2.6
7.8
5.2
17.7
ND
0.5
0.3
0.7
1.9
1.4
4.8
--
0.6
0.4
1.1
3.2
2.2
7.5
ND - Not detected. Analytical detection limits ranged from 10 parts
per trillion to 80 parts per trillion for specific homologues.
NR = Not reported by Troika.
5-28
-------
5.7 DIOXIN/FURAN PRECURSORS
As discussed in Section 4.0, five different incinerator feed samples were
collected during testing at Site ISW-A, including: wood/paper/cardboard,
wood/plastic cutoffs, latex (water based) paint sludge, "hytest" (oil based)
paint sludge, and fuel oil. The first four of these samples were analyzed for
chlorobenzenes, chlorophenols and chlorinated biphenyls.
In addition, composite feed samples and the fuel oil were analyzed for
total chloride and total organic halide.
The results of compound specific precursor analyses are summarized in
Table 5-13. As shown in Table 5-13, the only precursors consistently found in
the feed materials were tetrachloro and pentachlorophenols. The highest
quantities of chlorinated phenols (5.8 to 19.7 ppm) were found in the
wood/plastic cutoffs. Analysis results were not reported for chlorinated
biphenyls and chlorinated benzenes in some samples because adequate sample
extraction and cleanup procedures could not be developed within the time and
budget constraints of this program.
Results for total chlorine and organic halide (TOX) determinations are
summarized in Table 5-14. Total chlorine concentrations of 22.0 and 20.4 ppm
were found in the fuel oil for Runs 01 and 03 respectively. No chlorine was
detected in the fuel oil for Run 04. No organic halides were detected in fuel
oils for Runs 3 and 4, but a concentration of 22.2 ppm was reported for Run 2.
The total chlorine analysis for the composite feed sample showed 9670 ppm
and the TOX analysis showed 12.7 ppm, suggesting that most of the chlorine in
the feed is inorganic chlorine. This is an expected result because the
greatest source of chlorine in the feed is from PVC.
5.8 AMBIENT AIR AND SOILS DIOXIN/FURAN DATA
The ambient air and soil samples were archived pending evalaution of
analytical data.
5-29
-------
TABLE 5-13. SUMMARY OF GC/MS PRECURSOR ANALYSES ON FEED SAMPLES
Precursor Concentration
(ppm by weight, mg/kg of waste)
Test
Run
01
03
04
01
03
04
01
03
04
Wood/
Precursor Plastic
Compounds Cutoff
TOTAL CHLORINATED PHENOLS 19.7
-Tetrachloro phenol 12.5
-Pentachloro phenol 7.2
TOTAL CHLORINATED PHENOLS 5.8
-Tetrachloro phenol 1.1
-Pentachloro phenol 4.7
TOTAL CHLORINATED PHENOLS 6.2
-Tetrachloro phenol 1.1
-Pentachloro phenol 5.1
TOTAL CHLORINATED BIPHENYLS ND
TOTAL CHLORINATED BIPHENYLS NR
TOTAL CHLORINATED BIPHENYLS NR
TOTAL CHLORINATED BENZENES ND
TOTAL CHLORINATED BENZENES NR
TOTAL CHLORINATED BENZENES NR
Crate, Wood,
Paper,
Cardboard
0.11
-
0.11
NA
0.04
-
0.04
ND
ND
ND
ND
ND
ND
>
Paint Sludaes
Latex
trace
-
trace
0.02
-
0.02
0.03
-
0.03
NRC
NR
NR
NR
NR
NR
Hytest
NDa
-
-
ND
-
-
-
0.03
NR
NR
NR
NR
NR
NR
aND « not detected, detection limit was approximately 0.02 parts per million.
NA - not analyzed.
CNR » values not reported. Adequate sample extraction and cleanup procedures
not available.
5-30
-------
TABLE 5-14. SUMMARY OF TOTAL CHLORIDE AND TOTAL ORGANIC HALIDE DATA
Sampl e
Type
Fuel Oil
Test
Run
01
02
03
04
Total
Chloride
(ppm)a
22.0
NA
20.4
NDd
Total Organic
Halogen
(ppm)a
NAb
22.2
NDC
ND
Composite Feed
04
9,670
12.7
ppm = parts per million, weight basis (ug/g), blank corrected.
NA = not analyzed.
°Not detected at 4 ppm detection limit.
Not detected at 10 ppm detection limit.
Composite feed consisting of 90 weight percent wood/paper/cardboard and
10 percent wood/plastic cutoffs.
5-31
-------
-------
6.0 SAMPLING LOCATIONS AND PROCEDURES
Samples were collected from seven different locations around the
Site ISW-A incinerator. The specific sampling locations are shown in
Figure 6-1. Three of the locations were for gaseous sampling, one was for
liquid sampling, and three were for slurry and/or solid sampling. The source
sampling and analysis matrix in Table 6-1 shows the sample location, the
measured parameters, the sampling methods, and the analysis method.
Details on the sampling locations and methods are discussed in Sections
6.1 through 6.3. Analytical procedures for the continuous monitoring samples
(CO, CO-, Og, THC, and NO ) and the molecular weight determinations are
included in Section 6.1. All other analytical procedures are discussed in
Section 7.
6.1 GASEOUS SAMPLES
Four tyes of gaseous samples were taken during the testing: Modified
Method 5 (MM5), HC1 , ambient air, and continuous monitoring (CEM). The
sampling locations and methods are further discussed in this section.
6.1.1 Gaseous Sampling Locations
6.1.1.1 Outlet Exhaust Stack Location. The system outlet exhaust stack
location is shown as Point E in Figure 6-1. This location was used for
dioxin/furan sampling using MM5 and for gas velocity, molecular weight, and
moisture determinations using EPA Methods 1 through 4.
Dimensions of the outlet exhaust stack sampling location relative to the
nearest flow disturbances are shown in Figure 6-2. The sampling ports were
located 4.3 duct diameters downstream of the ambient air intake damper and
6 diameters upstream of the top of the stack. Based on EPA Method 1, a total
of 24 traverse points were required for velocity determination at this
location.
6-1
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T
ROOF
18'
13'
TO
1 ATMOSPHERE
FROM
10 FAN
36" DIAMETER DUCT
3" SAMPUF PORTS
AT 90
AMBIENT
AIR
INTAKE
DAMPER
ROOF
Figure 6-2. System exhaust stack sample location.
6-5
-------
6.1.1.2 Boiler Outlet Sample Location. The boiler outlet location is
shown as point D in Figure 6-1. This location was used for obtaining a gas
sample for continuous monitoring of
CO, NOY, and THC.
A
6.1.2 Gas Sampling Procedures
Gas sampling procedures used during this program are discussed in detail
in the Tier 4 Quality Assurance Project Plan (QAPP). A brief description of
each method and any necessary deviations from the procedures outlined in the
QAPP are provided in the following sections.
6.1.2.1. Modified Method 5 (MM5K Gas sampling for dioxins was
conducted according to the October 1984 draft of the ASME chlorinated organic
compound sampling protocol. This sampling method is a modified version of
EPA Method 5 that includes a condenser followed by a solid sorbent module for
trapping vapor phase organics. The MM5 sampling train was used to collect
samples at the system outlet exhaust stack. Following sample recovery, the
various parts of the sample (filter, solvent rinses, sorbent trap, etc.) were
sent to the EPA's Troika laboratories to quantify the 2378-TCDD, 2378-TCDF,
and the tetra- through octa-dioxin/furan homolgues present in the samples.
One modification was made to the ASME protocol for the Site ISW-A test:
the condenser preceding the XAD sorbent trap was oriented horizontally
instead of vertically. Radian has found that substitution of a horizontal
condenser (but not trap) works equally well and has the added advantage of
i
reducing the space required for traversing the sampling train.
Four MM5 test runs were conducted at the outlet exhaust stack location,
with one test run being conducted per test day. Three of the MM5 samples
were collected isokinetically over a 240-minute sampling period with a sample
flow rate of 0.78 scfm. The fourth MM5 sample was collected isokinetically
over a 172-minute period with a sample flow rate of 0.82 scfm. This test run
was aborted after completing 17 of the 24 traverse points due to failure of a
hydraulic oil line on the feed ram of the incinerator.
A schematic diagram of the MM5 sampling train is shown in Figure 6-3.
Flue gas is pulled from the stack through a nozzle and heated glass probe.
Particulate matter is removed from the gas stream by means of a fiberglass
6-6
-------
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6-7
-------
filter housed in a teflon-sealed glass filter holder maintained at 248+25 F.
The gas passes through a sorbent trap for removal of organic constituents.
The trap, which is shown schematically in Figure (5-4, consists of separate
sections for (1) cooling the gas stream, and (2) adsorbing the organic
compounds on Amberlite XAD-2R resin (XAD). A chilled impinger train is used
to remove water from the flue gas, and a dry gas meter is used to measure the
sample gas flow.
6.1.2.2 HC1 Determination. HC1 concentrations in the flue'gas were
determined using another modification of EPA Method 5. The sample train
components and operation were identical to those of Method 5 with the
following exceptions:
-1. Water in the first two impingers was replaced with 0.1 m NaOH.
2. Sampling was two-point isokinetic with the nozzle placed at points
in the stack with average velocity.
3. The moisture/NaOH in the impingers was saved for laboratory
analysis by ion chromatography. The impinger catch was stored at 4°F until
analysis.
One average velocity sampling point was selected for each of the two
sampling ports available in the outlet exhaust stack. During the first half
of the MM5 sampling period, one port was used for the HC1 train, and the
other port was used to traverse with the MM5 train. For the second half of
the MM5 sampling period, the two trains were switched. A schematic diagram
of the Method 5 train is shown in Figure 6-5.
f
6.1.2.3 Ambient Air Dioxin Determination. The ambient air sample was
collected using the procedure outlined in the QAPP for "Combustion Air Dioxin
and Precursor Determination." Dioxin in the ambient air was collected on an
XAD resin trap using a sample train similar to that used for MM5.
A schematic diagram of the "ambient XAD" sample train is shown in
Figure 6-6. The train consists of a probe, condenser/sorbent tube, water
knockout trap, silica gel container, transfer line, pump, and dry gas meter.
Ambient air is drawn into the sorbent module, where it is cooled to 68°F or
lower, and the organic constituents are adsorbed by the XAD resin. The gas
is then dried with the silica gel and the sample volume is measured by the
6-8
-------
ana
CONOCNI
ana
XAD4
COAMSIflUT-
THERMOCOUPLE
WELL
ana
Figure 6-4. Adsorbent sampling system.
6-9
-------
rd
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. 6-10
-------
R A C METER BOX
GOOSENECK
INCLINE. MANOMETER
DRY 6AS METER
FINE
COARSE
o
PUMP
O
Figure 6-6. Ambient XAD sample train.
6-11
-------
dry gas meter. Recovery of the ambient XAD sample train was performed in a
manner similar to that of the MM5 train. The probe was rinsed with acetone
and hexane three times each. This rinse and the condensate (if any) was
combined in a single sample container. The resin tube was capped with
precleaned foil, and both components of the sample were sent to Troika for
analysis.
6.1.2.4 Volumetric Gas Flow Rate Determination. The volumetric gas
flow rate was determined during this program using procedures described in
EPA Method 2. Based on this method, the volumetric gas flow rate is
determined by measuring the cross-sectional area of the duct and the average
velocity of the flue gas. The average flue gas velocity is calculabed from
the average gas velocity pressure ( P) across an S-type pitot tube, the
average flue gas temperature, wet molecular weight, and the absolute static
pressure.
6.1.2.5 Flue Gas Moisture Determination. The moisture content of the
flue gas was determined using the methodology described in EPA Method 4.
Based on this method, a known volume of particulate-free gas is pulled
through a chilled impinger train. The quantity of condensed water is
determined gravimetrically and then related to the volume of gas sampled to
determine the moisture content.
6.1.2.6 Flue Gas Molecular Weight Determination. During testing, the
integrated sampling technique described in EPA Method 3 was used to obtain
integrated flue gas samples for fixed gas (02, C02, CO, N2) analysis. A
total of eight 1/2 hour integrated flue gas samples were obtained per MM5
test run. A small diaphram pump and a stainless steel probe were used to
D
extract a single point flue gas sample which was collected in a Tedlar bag.
Moisture was removed from the gas sample by a water-cooled condenser so that
the fixed gas analysis is on a dry basis.
The composition of the gas sample was determined using a Shimadzu
Model 3BT analyzer as opposed to the Fyrite or Orsat analyzer prescribed in
Method 3. This instrument employs a gas chromatograph and a thermal
conductivity detector to determine the fixed gas composition (CO, 02, N2) of
the sample. Calibration of the Shimadzu analyzer was conducted according to
6-12
-------
the procedures outlined in the QAPP, which involved analysis of one or more
standards of appropriate composition immediately before and after sample
analysis.
6.1.2.7 Continuous Monitor. Continuous monitoring was performed.at,the
boiler outlet sampling location for 02, C02, CO, NOX, and THC. The
continuous monitoring was performed throughout the 4 to 6-hour period that
dioxin sampling was being conducted each test day. The primary intent of the
continuous monitoring effort was to (1) observe fluctuations in flue gas
parameters, and (2) provide an indication of combustion conditions. Sample
acquisition was accomplished using an in-stack filter probe and a 50 ft
rtj)
heat-traced Teflon line connected to a mobile laboratory. The heat-traced
line was maintained at a temperature of 149°C (300°F) to prevent condensation
in the sample line. The stack gas sample was drawn through the filter and
sample line using pumps located in or near the mobile laboratory. Sample gas
to be analyzed for CO, CO-, NO , and 02 was then pumped through a sample gas
conditioner, consisting of an ice bath and knockout trap, to remove moisture
and thus provide a dry gas stream for analysis. A separate unconditioned gas
slip stream was supplied to the THC analyzer for analysis on a wet basis.
An Anarad Model 412 nondispersive infrared (NDIR) analyzer was used to
measure CO and C02; a Beckman Model 755 paramagnetic analyzer was used to
measure 02; a Teco Model 10 chemiluminescent analyzer was used to measure
NO ; and a Beckman Model 402 flame ionization analyzer was used to measure
A
THC. Calibration of the continuous monitors was performed according to the
procedures outlined in the QAPP. These procedures included a three point
(two upscale plus zero) linearity check on the first test day, single point
and zero point calibration checks daily, and single point drift checks at the
end of each test day.
6.2 LIQUID SAMPLES
The only liquid sample collected at Site ISW-A was the No. 2 fuel oil
fired in the afterburner. This sample was collected from a tap valve located
in a fuel oil line leading from the fuel oil storage tank to an oil-fired
6-13
-------
boiler supplying process steam to the plant. No sample location was
available in the fuel oil line leading to the incinerator. However, since
the process boiler and the incinerator receive oil from the same storage
tank, the tap valve used for sampling should have provided a representative
sample. Grab samples of fuel oil were taken hourly during each MM5 test run.
To provide a composite sample, the sample containers (amber glass jars) were
graduated at increments of 1/5 of the total volume.
Samples of fuel oil were collected for dioxin/furan, precursor, and
total chlorine analyses. To acquire the sample, the tap valve was fitted
with an 8-inch length of 1/4-inch Teflon® tubing. The sample was collected
by placing the tubing in the sample jar and opening the valve to admit a
moderate flow of liquid. The conduit line was flushed before the sample was
taken and covered with hexane-rinsed foil between sampling times.
i
6.3 SLUDGE/SOLID SAMPLES
Sludge or solid samples collected for Site ISW-A include samples of the
waste feed materials, incinerator bottom ash, and soils adjacent to the plant
site. Sampling locations and procedures are discussed below.
6.3.1 Waste Feed Materials Sampling
Separate feed samples were obtained for (1) paint sludge, (2) wood/
plastic cutoffs, and (3) wooden crate parts, paper, and cardboard. Office
and cafeteria wastes and paint filters were neither sampled nor burned during
the test period.
Throughout the test period, each batch of material fed to the unit was
weighed using a scale provided by the plant, and the contents of the batch
were recorded. The plant reported that the scale was accurate well within
±5 percent for the range of loads weighed during the test (30 to 800 Ib).
The material feed rate data were used to formulate a weighed composite of the
three sample types collected. Samples of waste materials were brought back
to Radian's RTF laboratories and ground or reduced in size as necessary to
facilitate sample extraction (see Section 7.2;). A single weighed composite
6-14
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of the feed materials was provided to Troika for dioxin analysis. Samples to
be analyzed for dioxin precursors were analyzed separately. Procedures used
to collect the waste feed samples are discussed below.
6.3.1.1 Paint Sludge. As discussed in Section 3.1, paint sludge is fed
to the incinerator in 5-gallon plastic buckets. Two different types of
sludge, latex and "Hytest," are normally fed at a combined rate of 15 to
20 buckets per shift. An attempt was made to burn at least eight buckets of
sludge during each MM5 test run, including four latex and four Hytest
buckets. Samples were collected from two of the latex and two of the Hytest
buckets burned. Composite samples for each type of sludge were obtained by
filling sample containers (950 ml amber glass jars) halfway from one bucket
and then the rest of the way from the other bucket.
6.3.1.2 Wood/Plastic Cutoffs. The wood/plastic cutoff samples were
collected as sawdust in the area of the plant where window frame parts were
being mitered. Dust from the mitering saws is captured by a hooding system
that vents to a cyclone. The wood/plastic dust samples were collected in
amber glass jars twice per test day at the outlet of the cyclone hopper.
Samples of wood/plastic cutoffs as fed were also collected once per test run.
6.3.1.3 Wood. Crate Parts. Paper, and Cardboard. A composite or
combined sample consisting of wood, wooden crate parts, paper, and cardboard
was collected throughout each test run. Small pieces of each type of
material were collected from the various batches of incinerator feed and
placed in a single sample container. In collecting the sample, an effort was
made to collect each of the four components of the sample in a proportion (by
weight) representative of the material fed to the incinerator during the
test. Duplicate samples were collected to provide one sample for dioxin/
furan analysis and one sample for precursor analyses. Small pieces of
different wood parts were obtained using a cTean saw.
6.3.2 Bottom Ash Sampling
Bottom ash from the incinerator was conveyed to an outside storage
hopper by a chain-link conveyor. Samples of the ash were collected from the
storage hopper using a precleaned trowel either immediately following or
6-15
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during dumping of the ash. Bottom ash samples were collected once per test
run.
6.3.3 Soil Sampling
The soil sample for Site ISW-A consisted of a composite of 10 samples
collected near the ash handling area. Since most of the property in the
vicinity of the ash handling system consisted of concrete and gravel, all
10 samples were collected from a single grassy area approximately 100 feet
from the ash hoppers. A diagram of the soil sampling locations is shown in
Figure 6-7. The soil samples were collected using a bulb planter which was
pushed approximately 3 inches into the soil. The sample was first placed in
a precleaned stainless steel bucket and then transferred with hexane-rinsed
aluminum foil to amber glass sample jars.
6.4 REFERENCES
1. Palazzolo, M. A., et. al. National Dioxin Study Tier 4 - Combustion
Sources Quality Assurance Project Plan. (Draft Report prepared for
U.S. Environmental Protection Agency, Research Triangle Park, N.C. EPA
Contract 68-03-3148, December 1984.)
6-16
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7.0 ANALYTICAL PROCEDURES
Laboratory procedures used to quantify dioxins/furans and dioxin/furan
precursors in the Tier 4 samples are described in this section. MM5 train
samples were analyzed by EPA's Troika laboratories for dioxin/furan content.
Procedures used for these analyses are described in detail in the Analytical
Procedures and QA Plan for the Analysis of Tetra- through Octa- CDD's and
CDF's in Samples from Tier 4 Combustion and Incineration Processes (addendum
to EPA/600/3-85-/019, April 1985). These procedures are summarized in Section
7.1.
Combustion device feed samples from Site ISW-A were analyzed by Radian to
determine concentrations of chlorinated phenols (CP), chlorobenzenes (CB),
polychlorinated biphenyls (PCBs), total organic halogen (TOX) and total
chlorine. Procedures used for these analyses are detailed in Section 7.2.
7.1 DIOXINS/FURANS
The analytical procedures summarized in this section were used by Troika
for dioxin/furan analysis of MM5 train samples from Site ISW-A. Samples
consisting of organic solvents, aqueous solutions, and solids were prepared
for analysis using slightly different procedures. The organic solvent samples
consisted of rinses from the MM5 probe, nozzle, filter housing and condenser
coil. Aqueous samples consisted of impinger catch solutions, and solid
samples included filters and XAD resin. Isotopically-labeled surrogate
compounds were added to all samples prior to extraction to allow determination
of method efficiency and for quantification purposes.
Organic liquid samples (e.g., acetone and methylene chloride-based MM5
train rinses) were concentrated using a nitrogen blowdown apparatus. The
residue, which contained particulate matter from the MM5 train probe and
nozzle, was combined with the filter and handled as a solid sample. Solid
samples were extracted with benzene in a Soxhlet apparatus for a period of at
least 16 hours. The extract was concentrated by nitrogen blowdown and
subjected to chromatographic cleanup procedures.
Aqueous solutions (e.g., MM5 train impinger samples) were extracted with
hexane by vigorous shaking for a three hour period. This extraction procedure
7-1
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was repeated three times, with the organic fractions ultimately being combined
and concentrated for chromatographic cleanup.
The cleanup procedure involved using liquid chromatographic columns to
separate the compounds of interest from other compounds present in the
samples. Four different types of columns were used: a combination acid and
base modified silica gel column, a basic alumina column, a PX-21 carbon/eelite
545 column and a silica/diol micro column. These were used in successive
steps, with the last two being used only if necessary.
The cleaned samples were analyzed using high resolution gas
chromatography/high resolution mass spectrometry (GC/MS). Conditions for the
analyses were as follows:
Gas Chromatograph - Injector configured for capillary column, split!ess
injection; injector temperature 280°C; helium carrier gas at 1.2 ml/min;
initial column temperature 100°C: final column temperature 240°C; interface
temperature 270°C.
Mass Spectrometer - Varian/MAT Model 311A; electron energy 70ev; filament
emission 1mA; mass resolution 8000 to 10,000; ion source temperature 270°C.
7.2 DIOXIN/FURAN PRECURSORS
Feed samples for Site ISW-A were analyzed by Radian/RTP for chlorophenols
(CP), chlorobenzenes (CB) and polychlorinated biphenyls (PCBs) by GC/MS; total
organic halides (TOX) by GC/Hall detector; total chlorine by Parr bomb
combustion followed by ion chromatography. Analytical procedures are
discussed in the following sections.
7.2.1 GC/MS Analyses
The analytical procedures used for determining CP, CB, and PCB
concentrations in feed samples are modified versions of procedures typically
used for the analysis of MM5 train components; These procedures involve
7-2
-------
initial extraction of the sample with an appropriate solvent, preliminary
separation of the compounds of interest by solvent partitioning and liquid
chromatography, and analysis of the processed fractions. Solutions containing
CB and PCB are injected directly into the GC/MS, and solutions containing CP
are derivatized prior to "injection. Details'-on theprocetfuresJ-usBdv'fGr-3rte -
02 samples are provided in the sections below.
7.2.1.1 Sample Preparation
A flow chart for the sample preparation procedure used for Site ISW-A
feed samples is shown in Figure 7-1. The first step in the procedure involved
adding labeled surrogate compounds to provide a measure of extraction method
efficiency. The next step involved adding a mixture of 0.5 N NaOH and MeCK
to the sample and sonicating the sample for 30 minutes. The NaOH and MeCK
mixture converts the acid compounds to their salts and collects base/neutrals
in the organic solvent. The sonicated sample was filtered and rinsed with 0.5
N NaOH. The filtrate was extracted three times in a separatory funnel with
MeClg and the aqueous and organic fractions were saved for derivatization
and/or further cleanup. The aqueous fraction (or acids portion) was acidified
to pH2 with HC1 and then extracted three times with MeClg. The MeCU from
this extraction was dried with anhydrous Na2S04, exchanged to benzene, and
concentrated using a nitrogen blowdown apparatus. Acetylation of any CP
present in the sample involved the following steps:
2.0 ml isooctane, 2.0 ml acetonitrile, 50 uL pyridine, and 20 uL
acetic anhydride were added to the extract. The test tube
containing the extract was placed in a 60°C water bath for 15
minutes and was shaken 30 seconds every 2 minutes.
6 mL of 0.01 N H3P04 to the test tube, and the sample was agitated
for 2 minutes on a wrist action shaker.
7-3
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SOg Sampln
1.0mL Baae/Neutral Surrogataa
t.OmL Acid Surrogate*
Sonicate with 250mL
0.5 N, NaOH and 15mL MaCI2
Filter thru Buehniir and
Rlnaa with 0.5 ft NaOH
Extract 3x with MeClj,
In Separatory Funnel
Aquaoua
Organic
Adjuat to pH2 with HCl;
Extract 3x with MeCI2
Flltar with Na2SO4
Add 30mL Cone. H2SO4:
Shaft* 4 mln; Alternate
with 30mL dlatlllad H2O;
Repeat until acid la claar.
Add 10ml. Benzene
Concentrate to 1ml.
Filter with
To 1mL Banzana add:
2.0mt lao octana
2.0mL Aeatonltrll*
30uLPyrldln«
20uL Acatlc Anlydrlda
Add 10mL Haxanaa;
Concantrata to 1mL
Pra-wot Coftimn
wtth aoiiri. Hexanaa
Put In 60 C H^J bath
for 15 minutes. Shaking
3O aaconda avary 2 mlmitao.
Add 6mL of O.01 N
H3PO4; Shaka 2 minutaa.
Chromatography column with:
I.Og Silica
2.0g 33% NaOH Silica
2.0g Silica
But* with 90mL Haxanaa;
Coneantrat* to 1mL
Mini-column with
1.0g Alumina
Eluta with 20mL SO/50
MaCI2/Haxanaa
Add Ouantltatlon Staindarda;
Concantrata to 1inL
6C/MS Analyala
Figure 7-1. Sample Preparation Flow Diagram
for Site ISW-A Precursor Analyses
7-4
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3. The organic layer was removed and the quantitation standard was
added. The sample was concentrated in a Reacti-Vial at room
temperature (using prepurified N2) to 1 ml prior to GC/MS analysis.
Cleanup of the organic (or base/neutrals) layer from the first MeCl2
extraction involved successively washing the extract with concentrated FUSO.
and deionized distilled water. The acid or water was added in a 30 ml portion
and the sample was shaken for two minutes. After the aqueous (or acid) and
organic layers were completely separated, the aqueous (or acid) layer was
discarded. The acid washing procedure was repeated until the acid layer was
colorless. The organic fraction from the final wash was dried with anhydrous
NagSO^, exchanged to hexane and concentrated. Final cleanup of the sample by
column chromatography involved the following procedure.
A glass macro-column, 20 mm o.d. x 230 mm in length, tapered to 6 mm o.d.
on one end was prepared. The column was packed with a plug of silanized glass
wool, followed successively by 1.0 g silica, 2.0 g silica containing 33% (w/w)
1 N NaOH, and 2.0 g silica. After wetting the chromatography column with
hexanes, the concentrated extract was quantitatively transferred to the column
and eluted with 90 ml hexanes. The entire eluate was collected and
concentrated to a volume of 1 ml in a centrifuge tube.
A disposable liquid chromatography mini-column was constructed by cutting
off a 5-mL Pyrex disposable pipette at the 2.0 ml mark and packing the lower
portion of the tube with a small plug of silanized glass wool, followed by 1 g
of Woehlm basic alumina. The alumina had been previously activated for at
least 16 hours at 600°C in a muffle furnace and cooled in a desiccator for 30
minutes just before use. The concentrated eluate from above was
quantitatively transferred onto the liquid chromatography column. The
centrifuge tube was rinsed consecutively with-two 0.3-mL portions of a 3
.percent MeCl2: hexanes solution, and the rinses were transferred to the liquid
chromatography column.
The liquid chromatography column was eluted with 20 ml of a 50 percent
(v/v) MeCl2:hexanes solution, and the eluate was concentrated to a volume of
approximately 1 ml by heating the tubes in a water bath while passing a stream
of prepurified N2 over the solutions. The quantitation standard was added and
the final volume was adjusted to 1.0 ml prior to GC/MS analysis.
7-5
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7.2.1.2 Analysis
Analyses for CP, CB and PCBs present in the feed sample extracts were
performed with a Finnigan Model 5100 mass spectrometer using selected ion
monitoring. A fused silica capillary column was used-for chromatographic
separation of the compounds of interest. Analytical conditions for the GC/MS
ii
analysis are shown in Table 7-1.
Tuning of the 6C/HS was performed daily as specified in the Tier 4 QA
Project Plan. An internal-standard calibration procedure was used for sample
quantitation. Compounds of interest were calibrated against a fixed
concentration of either djg-chrysene (for CB, PCB) or dg-naphthalene (for CP).
Components of the calibration solution are shown in Table 7-2. For
multi-point calibrations, this solution was injected at levels of 10, 50, 100,
and 150 ng/ml.
Compound identification was confirmed by comparison of chromatographic
retention times and mass spectra of unknowns with retention times and mass
spectra of reference compounds. Since the selected ion monitoring technique
was necessary for the samples analyzed, care was taken to monitor a
sufficiently wide mass region to avoid the potential for reporting false
positives.
The instrument detection limit for the analytes of interest (i.e., CP,
CB, and PCB) was estimated to be approximately 500 pg on column. For a 50 g
sample and 100 percent recovery of the analyte, this corresponds to a feed
sample detection limit of 10 ppb.
7.3 TOX ANALYSIS
/
Incinerator feed samples were analyzed for total organic halide (TOX) by
short-column GC and a Hall detector (GC/Hall). Solid samples were extracted
with benzene for at least 16 hours in a Soxhlet apparatus. The extracts were
washed three times with 100 ml portions of reagent-grade water concentrated to
10 ml.
7-6
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TABLE 7-1. ANALYTICAL CONDITIONS FOR THE GC/MS
Parameter
Chi orobenzenes/,-.— —
Polychlorinated biphenyls
Chlorophenols
Column
Injector Temperature
30 m WB DB-5 (1.0 u film
thickness) fused silica
capillary
290°C
Separator Oven Temperature 290°C
same
290°C
290°C
Column Head Pressure
He flow rate
GC program
Emission Current
9 psi
1 mL/min
40(4)-290°C,
min & hold
0.50 mA
9 psi
1 mL/min
40m-290°C,
12°/min & hold
0.50 mA
Electron Energy
Injection Mode
Mode
70 eV
Splitless 0.6 min,
then 10:1 split
Electron ionization,
Selected Ion Monitoring
70 eV
7-7
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TABLE 7-2. COMPONENTS OF THE CALIBRATION SOLUTION
Bass/Neutrals
Acids
4-chlorobiphenyl
3,3 *-dichlorobi phenyl
2,4',5-trichlorobiphenyl
3,3'4,4'-tetrachlorobiphenyl
2,2',6,6'-tetrachlorobiphenyl
2,2,4,5,6-pentachlorobi phenyl
2,2',4,4',5,5'-hexachlorobiphenyl
2,2',3,4,4',5',6-heptachlorobiphenyl
2,2',3,3',4,4',5,5'-octachlorobiphenyl
2,2',3,3',4,4',5,6,6'-nonachlorobiphenyl
decachlorobiphenyl
p-di chlorobenzene
1,2,4-tri chlorobenzene
1,2,3,5-tetrachlorobenzene
pentachlorobenzene
hexachlorobenzene
d4-l,4-dichlorobenzene (SS)
3-bromobiphenyl (SS)
2,2',5,5'-tetrabromobiphenyl (SS)
2,2',4,4',6,6'-hexabromobiphenyl (SS)
2
octachloronaphthalene (QS)
djQ-phenanthrene (QS)
djg-chrysene (QS)
2,5-dichlorophenol
2,3-dichlorophenol
2,6-d.ichlorophenol
3,5-dichlorophenol
3,4-dichlorophenol
2,3,5-trichlorophenol
2,3,6-trichlorophenol
3,4,5-trichlorophenol
2,4,5-trichlorophenol
2,3,4-trichlorophenol
2,3,5,6-tetrachlorophenol
pentachlorophenol
dg-phenol (SS)
d«-2-chlorophenol (SS)
Cg-pentachlorophenol (SS)
dg-naphthalene (QS)
2,4,6-tribromophenol (QS)
djQ-phenanthrene (QS)
d12chrysene (QS)
Surrogate standard.
"Quantitation standard.
7-3
-------
An attempt to use a fused silica capillary column to separate surrogates
from target compounds was unsuccessful due to the complexity of the sample
constituents. Determinations for TOX were therefore performed on samples
without surrogates and no measure of extraction efficiency is available.
Instrument conditions are shown in Table 7-3. Samp!e"quantitation was
based on an average response factor developed from a mixture of chlorinated
benzenes and brominated biphenyls. Individual CP, CB and PCBs were also
injected at various concentrations to develop a calibration curve for
comparison to the mixture response factors.
7.4 TOTAL CHLORINE ANALYSIS
Total chlorine concentrations in feed samples were determined by Parr
bomb combustion followed by ion chromatography (1C). A 0.5g sample was placed
in the Parr bomb with 10 mL of a 50 g/L Na^CO* solution. After combustion of
the samples according to standard procedures (ASTM 2015), the contents of the
bomb were rinsed into a 100 mL flask and diluted to 100 mL. The resulting
solution was analyzed for chloride concentration (Cl~) by 1C using standard
anion conditions. For samples difficult to combust (such as sludges), 25
drops of paraffin oils were added to the bomb prior to combustion.
7-9
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TABLE 7-3. ANALYTICAL CONDITIONS FOR TOX ANALYSIS
Hall Detector Conditions
Reactor temperature - 850°C ;
Solvent - n-propanol
Hydrogen flow rate - 35 mL/min
GC Conditions (Varian 3700)
Injection volume (1 - 5 uL)
Helium carrier gas flow rate - 60 mL/min
Column - 3-ft packed column with 1 in 10% 0V 101
Column temperature - 200°C isothermal
7-10
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8.0 QUALITY ASSURANCE/QUALITY CONTROL (QA/QC)
This section summarizes results of the quality assurance and quality
control (QA/QC) activities for field sampling and laboratory analyses for
Site ISW-A, The flue gas and bottopm ash dioxin/furan data for- Stte .ISW-A
were within the QC specifications outlined in the Tier 4 QAPP. Surrogate
recoveries for all the samples were within the specified limits of 50 to
120 percent for labeled TCDD's and 40 to 120 percent for hepta- and octa-
CDD's. The results of the analysis of the fortified laboratory QC sample were
within 33 percent for all homologues except octa-CDF. Recovery for octa-CDF
was 59 percent, which is just outside the accuracy objective of 60 to 140
percent. Overall the dioxin/furan analysis gave reasonable results.
The dioxin/furan precursor analysis of the feed samples was not as
accurate as the dioxin/furan homologue analysis. In general, the surrogate
recoveries were outside the specified QC limits of 100 ± 50 percent for all
types of feed samples. The low precursor surrogate recoveries resulted from
two difficulties encountered during analysis. Initially, due to the complex
nature of the feed samples extensive clean-up procedures were necessary, which
increased the potential for losses during sample preparation. Secondly,
larger sample sizes were necessary to ensure representative samples; however,
the amount of labeled surrogate was not increased in proportion to sample
size. In spite of the relatively low surrogate recovery values, the resulting
analytical sensitivity for the target analytes was considered acceptable or
the purpose of this study.
The following sections summarize the results of all Site ISW-A QA/QC
activities. Manual gas sampling methods are considered in Section 8.1 and
continuous monitoring and molecular weight determinations are considered in
Section 8.2. The laboratory analysis QA/QC activities are summarized in
Section 8.3.
8.1 MANUAL GAS SAMPLING
Manual gas sampling methods used at Site ISW-A included modified Method 5
(MM5), the HC1 acid train, EPA Methods 1 through 4, and the ambient air/XAD
8-1
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train. These methods are discussed In Section 6.0. Quality assurance and
quality control (QA/QC) activities for the manual methods centered around 1)
equipment calibration, 2} glassware precleaning, 3) procedural QC checks and
4) sample custody procedures. Key activities and QC results in each of these
j-areas are discussed in this section. Also discussed are problems encountered
that may have affected data .quality. - -
Pretest calibrations or inspections were conducted on pitot tubes,
sampling nozzles, temperature sensors and analytical balances. Both pre and
post-test calibrations were also performed on dry gas meters. All of this
equipment met the calibration criteria specified in the QAPP. Differences in
pre- and post-test dry gas meter calibrations were less than 3.4 percent.
An extensive precleaning procedure was implemented for all sample train
glassware and sample containers. This cleaning procedure, which is outlined
in Table 8-1, was implemented to minimize the potential for sample
contamination vrith substances that may have interfered with the analysis for
dioxins and furans. To minimize the potential for contamination in the field,
all sample train glassware was kept capped until use and a dust free
environment was maintained for train assembly and sample recovery.
Procedural QC activities during manual gas sampling focused on:
inspecting equipment visually, j
collecting sampfe train blanks,
ensuring the proper location and number of traverse points,
conducting pre-test, port change and post-test sample train leak
checks,
maintaining proper temperatures at the filter housing, sorbent trap
and impinger train,
maintaining isokinetic sampling rates, and
recording all data on preformatted data sheets.
Results of isokinetic calculations for the MM5 and HC1 test runs are
shown with EPA Method 4 results in Table 8-2. As shown in Table 8-2, the
average isokinetic sampling rate for both the MM5 and HC1 sampling trains
exceeded the QA objective of +10 percent for test runs 3 and 4. The slightly
8-2
-------
TABLE 8-1. GLASSWARE PRECLEANING PROCEDURE
NOTE: USE DISPOSABLE fil.QVES AND ADEQUATE VENTTI ATTOM
1. Soak all glassware in hot soapy water (Alconox) 50°C or higher. .
2. H20 rinse (X3)a.
3. Distilled/deionized H20 rinse (X3).
4. Chromerge rinse, if glass, otherwise skip to 6.
5. High purity liquid chromatography grade H20 rinse (X3).
6. Acetone rinse (X3), (pesticide grade).
7. Hexane rinse (X3), (pesticide grade).
8. Oven dry (110°C - 2 hrs).
9. Cap glassware with clean glass plugs or hexane rinsed aluminum foil
a (X3) =• three times.
8-3
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TABLE 8-2. RESULTS OF ISOKINETIC CALCULATIONS
AND MOISTURE DETERMINATIONS
Run
Number
Modified Method 5
Isokinetics
Moisture
HC1 Acid Train
Isokinetics
Moisture
1
2
3
4
104
104
112
111
7.45
7.62
8.44
7.73
102
101
112
118
6.18
5.51
8.20
7.39
QA objective for isokinetics was 100±10 percent.
8-4
-------
high isokinetics for these test runs Is not expected to have a significant
impact on the dioxin/furan or HC1 emission determinations for these test runs.
The high isokinetics sampling rate would effect only the quantity of
particulate matter collected on the filter. The dioxins/furans (or HC1) of
greatest interest-are expected- to be- in the- vapor phase and the quantity
collected in the sample train would not be effected by isokineticity.
In considering the isokineticity of samples collected from Site ISW-A, it
should also be noted that large fluctuations in stack gas temperature and
velocity occurred periodically throughout all of the MM5 and HC1 test runs.
As discussed in Section 3.0, the induced draft fan downstream of the waste
heat boiler on the incinerator cycled on and off to meet steam demands of the
plant. During periods when the fan cycled/stack gas temperatures varied from
about 300°F when the fan was on to as high as 700 or 800°F when the fan was
off. Corresponding changes in stack gas velocity occurred with these changes
in temperature. Since periods when the fan was off rarely exceeded 30
seconds, the MM5 or HC1 sampling rate could not be adjusted to account for
these periods. Sampling rate adjustments were, therefore, based only on the
instantaneous stack temperature and pitot tube readings taken at set
five-minute intervals.
Limited data collected during one test run show that the fan operated 71
minutes during a 74-minute. period of observation with the fan cycling off and
on 10 times. However, since a number of plant operating conditions affect
steam demand from the waste heat boiler, the period of time that the fan
actually operated during a given test run is unknown.
Initial, final and port change leak checks for the MM5 trains were passed
for all of the test runs. However, the glass probes on the HC1 trains were
found to be broken at the end of test runs 2 and 3. The cause of the breakage
was apparently a tight probe-cyclone bypass-filter holder assembly. The
actual time that the breakage occurred during the sampling run is not known,
but the breakage is most likely to have occurred either during the port change
or when the train was removed from the stack for disassembly. Following a
review of the chloride analysis results, the HC1 data for Run 2 was
invalidated because the HC1 values determined for this run were unreasonably
low compared to those for Runs 1 and 4. Results for Run 3 were very similar
8-5
-------
to those for Runs 1 and 4 and 1t appears likely that this probe was not broken
until after sampling was completed.
Sample custody procedures used during thjs program emphasized careful
documentation of the sample collected and the use of chain-of -custody records
for samples -to be transported Steps taken to identify and document samples
collected included labeling each sample with a unique alphanumeric code and
logging the sample in a master sample logbook* All samples shipped to Troika
or returned to Radian were also logged on chain-of -custody records that were
signed by the sampler at shipment and then by the receiving laboratory when
the samples arrived. Each sample container was also sealed with a
chain-of -custody seal so that the container could not be opened without
tearing the seal.
i
8.2 CONTINUOUS MONITORING/MOLECULAR WEIGHT DETERMINATION
Flue gas parameters monitored continuously during the MM5 test runs
included CO, C02, 02, total hydrocarbons (THC), and NOX. Concentrations of
C0
and N2 were a^so <'eterm''ned
integrated bag samples of stack gas.
Quality control results for these analyses are discussed in this section.
Drift check and quality control standard analysis results for the
continuously monitored flue gas parameters are summarized in Table 8-3. The
acceptance criterion for drift checks was an instrument drift within +10
percent. All data reduction was performed by assuming a linear drift of
instrument response over the test day. The largest calibration drifts were
observed for CO and C02, both of which exceeded acceptance criterion for three
of the four test runs. The instrument showing the smallest drift was the 0?
monitor.
The quality control standards for this program consisted of mid-range
standards that were not used for instrument calibration but were analyzed
immediately after calibration to provide data on day-to-day instrument
variability. The acceptance criterion for each control standards was
agreement within ±10 percent of the running mean value. All of the
instruments met this criterion on each test day except for the CO monitor.
However, failure of the CO monitor to meet the acceptance criterion during
3-6
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8-7
-------
test runs 2, 3, and 4 is not entirely unexpected. The QC standard (2060 ppmv)
was above the calibration range selected for the CO instrument during these
test runs (0 to 520 ppmv) and, the CO instrument shows some non-linearity at
low concentration. The instrument was calibrated at a low range to maximize
instrument accuracy near the CO levels present in the flue gas.
Molecular weight was determined by analyzing integrated bag samples of
stack gas for C02, 02, and N2. Quality control for this analysis involved
duplicate analyses of calibration gases immediately before and after sample
analysis. Analysis of the calibration gases was to be repeated until two
consecutive analyses within +5 percent were obtained. This same criterion of
±5 percent also applied to duplicate analyses required for each sample
quantitation. These criteria were met for all molecular weight
determinations.
8.3 LABORATORY ANALYSES
QA/QC data collected for the various laboratory analyses performed on
Site 02 samples are discussed in this section. Dioxin/furan QC data are
discussed in Section 8.3.1, precursor QC data are discussed in Section 8.3.2,
and total chloride and organic halide data are summarized in Section 8.3.3.
8.3.1 Dioxin/Furan QC Data
Surrogate recoveries for dioxin/furan analyses performed on Site ISW-A
samples are presented in Table 8-4. All of the surrogate recoveries are
within the target ranges of 50 to 120 percent for the labeled TCDD's and 40 to
120 percent for the labeled hepta- and octa-CDD's.
Results for dioxin/furan blank samples arid a QC (fortified spiked) sample
are summarized in Table 8-5. Again surrogate recoveries were all within the
target ranges. The field blank and the laboratory blank were found to be
clean with the exception of 2.9 ng of octa-CDD and 0.2 ng of other TCDF in the
field blank. Comparison of measured and spiked quantities for the QC sample
shows excellent recoveries for the unlabeled PCDD and PCDF, with the exception
of the octa-CDF. Recovery for octa-CDF was 59 percent, which is just outside
the accuracy objective of 60 to 140 percent for this sample.
3-8
-------
TABLE 8-4. SUMMARY OF SURROGATE RECOVERIES FOR DIOXIN/FURAN
ANALYSES ON SITE ISW-A SAMPLES
.
Compound
37C14-TCDD
13C12-TCDD
37Cl4-Hepta-CDD
13r
L12-Octa-CDD
Run 1
MM5
96
98
88
73
Surrogate Recoveries (percent)
Run 2
MM5
94
92
81
68
Run 3
MM5
96
88
98
54
Run 4
MM5
102
82
86
41
Run 1 Run 3 Run 4
Asha Asha Asha
--
99 100 94
--
43 56 69
Only two surrogates were used in the bottom ash samples analysis.
3-9
-------
TABLE 8-5. SUMMARY OF RESULTS FOR DIOXIN/FURAN BLANK
SAMPLES AND FORTIFIED QC SAMPLES
Surrogate Recoveries,
Percent
Field Laboratory Fortified
Compound Blank Blank QC Sample
Hcld-TCDDa 96
r _ Tf*nn^ QC
07^*1 0 ' v*U« L OO
f,CTf Hepta-CDDD 79
"Cjg Octa-CDDD 60
96 102
110 108
57 64
56 57
Amount detected, ng (Amount spiked on fortified sample, ng)
Dioxins
2378 TCDD NDC
Other TCDD ND
Penta CDD ND
Hexa CDD ND
Hepta CDD ND
Octa CDD 2.9
Furans
2378 TCDF ND
Other TCDF 0.2
Penta CDF ND
Hexa CDF ND
Hepta CDF ND
Octa CDF ND
ND 0.4 (0.4)
ND ND (0)
ND ND (0)
ND 1.6 (1.6)
ND 2.6 (2.4)
ND 3.3 (3.2)
NO 0.3 (0.4)
ND ND (0)
ND 0.7 (0.8)
ND 1.7 (1.6)
ND 2.3 (2.4)
ND 1.9 (3.2)
a Spiked at 5 ng in each sample.
ND =* not detected. Detection limit ranged from 0.01 to 0.19 ng.
8-10
-------
8.3.2 Precursor PC Data
Surrogate recovery efficiencies for six labeled compounds spiked into
incinerator feed samples are presented in Table 8-6. The recoveries vary
considerably depending on sample type and the particular surrogate.
Recoveries for wood/plastic cutoffs ranged from 0 to 46 percent.
Cardboard/paper/wood ranged from 0 to 362 percent and paint sludges ranged
from 0 to 75 percent. With the exception of bromobiphenyl in one
cardboard/paper/wood sample, the surrogate recoveries are generally below the
50 percent objective stated in the Tier 4 QA Project Plan and are below those
generally considered achievable when analyzing for similar compounds in water
or from MM5 train components. There are no directly comparable surrogate
recovery values reported in the literature for samples similar to those
analyzed for Site ISW-A. The high recovery for bromobiphenyl in the one
sample may be due to native compound present in the sample.
There are several reasons for the comparatively low precursor surrogate
recoveries reported in the Tier 4 study for samples such as Site ISW-A feed
samples. First, the complex nature of the samples required extensive clean-up
procedures prior to GC/MS analysis, which increased the potential for losses
of the surrogate compounds (and analytes) during sample preparation. Second,
large sample sizes (25 to 50 g) were required to increase method sensitivity
for the target analytes and to ensure that representative portions of the
samples were analyzed. Due to the high cost of labeled surrogates, it was not
desirable to spike the large sample sizes with surrogates in proportion to
that normally used for smaller samples. Supplemental in-house laboratory
studies showed that when sample size was restricted to 1 g and the amount of
surrogate spiked was held fixed, surrogate recoveries improved and were
directly comparable to.those obtained by Tiernan and co-workers for municipal
incinerator feed materials. Surrogate recoveries for Tier 4 samples and the
results for small sample sizes are further discussed in the Tier 4 Engineering
Analysis Report.
In spite of the relatively low surrogate recovery values for some of the
feed samples, the resulting analytical sensitivity for the target analytes was
considered acceptable for the purpose of this study. The instrumental
8-11
-------
TABLE 8-6. ' SUMMARY OF SURROGATE RECOVERIES FOR DIOXIN PRECURSOR ANALYSES
Precursor Surrogate Recoveries (percent)4
Sample Type
Test Run Compound
2 d4-Dichlorobenzene
Bromobiphenyl
Tetrabromobi phenyl
dg - Phenol
d^ - Chlorophenol
Cg - Pentachlorophenol
3 d^-Dichlorobenzene
Bromobiphenyl
Tetrabromobi phenyl
dg - Phenol
d^ - Chlorophenol
Cg - Pentachlorophenol
4 d^-Dichlorobenzene
Bromobiphenyl
Tetrabromobi phenyl
dg - Phenol
d^ - Chlorophenol
13
Cg - Pentachlorophenol
Surrogates spiked at 200 ng each
Wood/
Plastic
Cutoff
13
19
22
18
30
36
ND
ND
ND
5
6
46
ND
ND
ND
5
9
25
in 50 g
8-12
Cardboard/
; Paper/
Wood
65
362
78
! 14
1
22
20
I
i
i
1
i
I
-
: 6
i
20
i 14
6
10
i 3
sampl e .
i
i
I
Hytest
Paint
SI udge
ND
2
ND .
27
9
ND
ND
ND
ND
11
12
6
ND
3
ND
120
23
14
Latex
Paint
Sludge
ND
8
ND
23
27
23
ND
1
ND
47
37
31
ND
ND
ND
75
ND
8
-------
detection limit ranged from about 100 to 500 picograms on-column for the 1
micro!iter of final extract injected into the GC/MS. At a method recovery
efficiency of 100 percent for a 50 gram solid sample cleaned up to a final
extract volume of 1 milliliter, the overall analytical sensitivity would be
approximately 2 tq.lQ. ppb in the solid sample. For samples such as the paint
sludge with surrogate recoveries as low as 1 percent, the overall analytical
sensitivity of the method would still be 200 to 1000 ppb, or 0.2 to 1.0 ppm.
Thus, even in a worst-case situation the analytical procedures used provide
information on the precursor content of the feed samples down to the ppm
1 eve!.
A single matrix spike was analyzed for the Site ISW-A feed samples. This
sample showed 6 to 9 percent recovery for spiked chlorobenzenes and 8 to 11
percent for spiked chlorinated biphenyls in a wood/plastic cutoff sample.
Chlorinated phenols were not spiked in this sample. Results of laboratory
blanks for the precursor analyses all showed no detectable levels of the
target compounds.
8.3.3 Chloride and Organic Halide QC Datg
Chloride analyses were performed by Radian laboratories on HC1 acid train
samples. Results for two audit samples submitted with the HC1 train samples
showed -3.6 percent error at 27.6 mg/L chloride and 13 percent error at 8.1
mg/L. These results are considered acceptable, although one of the errors
exceeds the 7 percent accuracy objective in the Tier 4 QA plan.
Total chloride analyses were performed by Research Triangle Institute on
one composite feed sample and three fuel oil samples. Blank analysis values
obtained for the Parr bomb combustion/ion chromatography technique were 36, 0,
56, and 18 ppm chloride. Data presented in Section 5 were blank corrected. A
LECO coal sample containing 2600 ppm chloride was analyzed as a daily QC
standard. Reported values were 2500, 2500, 2500, and 2400 ppm.
Quality control for the total organic halide (TOX) data consisted of a
single QC sample analysis. The sample contained 2-chlorophenol and
pentachlorophenol at a TOX level of 376 ppm. The total TOX measured for the
sample was 251 ppm, showing 67 percent recovery.
8-13
-------
-------
APPENDIX A
FIELD RESULTS
A-l
-------
-------
APPENDIX A-l
MODIFIED METHOD 5 and
EPA METHODS 1-4 FIELD RESULTS
A-3
-------
-------
I <=%rsj SOLJFtCE:
METHOD 2 —
TEST
PLANT
PLANT SITE
SAMPLING LOCATION
INCINERATOR (NORTH UNIT
TEST #
DATE
TEST PERIOD
DIOXIN SITE #O2
EXHAUST
Q2-MM5-01
11/07/84
1O47-1545
(1047-1247 / 1345-1545)
PARAMETER
VALUE
Sampling time (min.)
Barometric Pressure (in.Hg)
Sampling nozzle diameter (in.)
Meter Volume (cu.-ft.)
Meter Pressure (in.H20)
Meter Temperature (F)
Stack dimension (sq.in.)
Stack Static Pressure (in.H20)
Stack Moisture Collected (gm)
Absolute stack pressure(in Hg)
Average stack temperature (F)
Percent CO2
Percent O2
Percent N2
Delps Subroutine result
DGM Factor
Pi tot Constant
240
29. 19
.302
181.776
1.937708
87.4
962.115
-.33
292.7
29.16206
286.7917
4.84
17.58
77.58
13.87255
.9973
.84
A-5
-------
I <=»N SOURCE
METHODS S —I
PLANT
PLANT SITE
SAMPLING LOCATION
INCINERATOR (NORTH UNIT
TEST #
DATE
TEST PERIOD
DIOXIN SITE #O2
EXHAUST
O2-MM5-01
11/O7/S4
1047-1545
(1047-1247 / 1345-1545)
PARAMETER
RESULT
Vm(dsc-f)
Vm(dscm)
Vw gas(scf)
Vw gas (scm)
7. moisture
Md
MWd
MW
Vs(-fpm)
Vs (mpm)
Flow (ac-f m)
Flow(acmm)
Flow(dscfm)
Flow(dscmm)
% I
'/. EA
171.4268
4.8548O6
13.8OO81
. 39O£3388
7.45O73
.9254927
29.4776
28.62244
2068., 901
630.7626
13823.06
391.4691
8815.; 934
249.6672
1O4.0O99
6O5.9727
Program Revision:1/16/84
A-6
-------
I *=*|N| SOURCE
METHOD S —
TEST
PLANT
PLANT SITE
SAMPLING LOCATION
INCINERATOR (NORTH UNIT
TEST #
DATE
TEST PERIOD
DIOXIN SITE #02
EXHAUST
02-MM5-O2
ll/B/84
-2023 (1255-1345/1503-1613/1905-1917/1940-2023)
PARAMETER
VALUE
Sampling time
-------
METHODS s—s
F=-I ixl*=»L_ RESULTS
PLANT DIOXIN SITE! #02
PLANT SITE
SAMPLING LOCATION
INCINERATOR (NORTH UNIT EXHAUST
TEST # O2-MM5-Q2
DATE ll/S/84 I
TEST PERIOD
;55-2O23 (1255-1345/15O3-1613/19O5-1917/194O-2O23)
PARAMETER
RESULT
VrnCdsc-f)
Vm(dscm)
Vw gas
Flow(dscmm)
7. I
'/. EA
13O.9752
3.709216
10.79735
.30-5781
7.615969
.92384O4
29.342
28.4782
2296.759
700.2315
15345.46
434.5835
9412.269
266.5555
1O3.S584
759.7911
Program Revision:1/16/S4
A-8
-------
I *=»r*4 SOLJIROE
METHOO 2 —
PLANT
PLANT SITE
SAMPLING LOCATION
INCINERATOR (NORTH UNIT
TEST #
DATE
TEST PERIOD
DIOXIN SITE #02
EXHAUST
02-MM5-03
11/09/84
L857 (1102-1132/1141-1311/1424-1444/1627-1647/1737-1857)
PARAMETER-
VALUE
Sampling time (min.)
Barometric Pressure (in.Hg)
Sampling nozzle diameter (in.)
Meter Volume (cu.-ft.)
Meter Pressure (in.H2O)
Meter Temperature (F)
Stack dimension (sq.in.)
Stack Static Pressure (in.H20)
Stack Moisture Collected (gm)
Absolute stack pressure(in Hg)
Average stack temperature (F)
Percent CO2
Percent 02
Percent N2
Delps Subroutine result
DBM Factor
Pi tot Constant
24O
29. IS
-3O9
173.2OS
1.792O83
72.89585
962.115
-.38
327.6
29.15206
368.7083
4.96
16.58
78.46
14.10O55
.9973
.84
A-9
-------
METHODS: S — 5
PLANT DIOXIN SITE #O2
PLANT SITE I
SAMPLING LOCATION |
INCINERATOR (NORTH UNIT EXHAUST
TEST # O2-MM5-O3
DATE 11/O9/84
TEST PERIOD
">2-lB57 CU02-1132/1141-131I/1424-1444/1627-1647/1737-1857)
PARAMETER
RESULT
Vm(dsc-F)
Vm(dscm)
Vw gas(sc-f)
Vw gas (scm)
'/. moisture
Md
MWd
MW
Vs(-fpm)
Vs (mpm)
Flow (ac-f m)
Flow(acmm)
Flow(dsc-fm)
Flow(dscmm)
% I
7. EA
167.674
4.748528
15.44634
.4374404
8.435076
.9156492
29.4568
28.49O41
21O8.133
642.7233
14085.IS
398.8923
80O6.293
226.7382
112.O2O8
4O1.1187
Program Revision:1/16/84
-------
I *=*I-"4 SOURCE!
METHOD S —!
:ST
PLANT
PLANT SITE
SAMPLING LOCATION
INCINERATOR (NORTH UNIT
TEST #
DATE
TEST PERIOD
DIOXIN SITE #02
EXHAUST
02-MM5-04
11/12/84
1021-1503 (1021-1221 / 13O3-15O3)
PARAMETER
VALUE
Sampling time (min.)
Barometric Pressure (in.Hg)
Sampling nozzle diameter (in.)
Meter Volume (cu.-ft.)
Meter Pressure (in.H20)
Meter Temperature (F)
Stack dimension (sq.in.)
Stack Static Pressure (in.H20)
Stack Moisture Collected (gm)
Absolute stack pressure(in Hg)
Average stack temperature (F)
Percent C02
Percent 02
Percent N2
Delps Subroutine result
DGM Factor
Pi tot Constant
24O
29.65
.309
176.435
1.S9
71.16666
962.115
-.38
3O9.5
29.622O6
350.25
4.4
18.2
77.4
14.19743
.9973
.84
A-ll
-------
R.P»:D I
PLANT
PLANT SITE
SAMPLING LOCATION
INCINERATOR (NORTH UNIT
TEST #
DATE
TEST PERIOD
DIOXIN SITE #02
EXHAUST
02-MM5-04
11/12/S4
1021-1503 (1021-122.1- / 1303-1503)
PARAMETER
RESULT
Vm(dsc-f)
Vm(dscm)
Vw gas(scf)
Vw gas (scm)
7. moisture
Md
MWd
MW
Vs(-Fpm)
Vs (mpm)
Flow (ac-f m)
Flow(acmm)
Flow(dsc-fm)
Flow(dscmm)
% I
7. EA
174.193
4.933145
14.59293
.4132716
7.; 729881
.9227012
29.432
28.54832
2:LO3.573
641.3333
14O54.72
398.0296
8366.653
236.9436
111.3636
814.8286
Program Revision:1/16/34
A-12
-------
APPENDIX A-2
CONTINUOUS EMISSION MONITORING RESULTS
A-13
-------
-------
CEM Data at 3% 0,
Site ISW-A Test 1
TIME
NO.
1045
1050
1055
1100
1105
1110
1115
1120
1125
1130
1135
1140
1145
1150
1155
1200
1205
1210
1215
1220
1225
1230
1235
1240
1245
1250
1340
1345
1350
1355
1400
1405
1410
1415
1420
1425
1430
1435
1440
1445
1450
1455
1500
1505
1510
1515
1520
1525
1530
1535
1540
1545
1550
PTS.
MEAN
STD
. DEV.
02
(SV)
9.7
8.8
10.5
7.9
9.0
11.2
12.7
13.6
9.9
9.4
9.9
7.4
9.7
9.9
10.1
10.1
8.8
10.4
9.5
10.1
10.8
10.0
9.0
10.6
10.5
10.3
10.1
11.2
11.2
9.4
9.5
9.5
10.1
9.7
10.7
11.6
9.9
11.5
10.1
10.7
10.8
11.9
13.1
14.0
11.4
11.5
10.4
12.1
12.4
11.7
10.2
11.6
9.6
53
10.5
1.3
CO
(PPMV)
496.5
474.7
572.8
499.6
457.5
659.4
640.6
636.2
537.1
538.3
468.3
553.6
570.8
525.9
638.9
649.6
586.8
494.2
469.6
513.2
742.8
484.7
420.3
777.4
713.7
691.8
683.1
1059.0
748.0
545.6
806.0
645.3
636.5
466.7
684.7
738.8
612.5
670.4
561.2
696.7
600.8
691.1
900.8
1041.7
937.4
736.9
692.7
707.0
872.2
713.7
644.4
682.6
610.4
53
645.3
140.0
CO 2
CSV)
15.3
15.1
14.1
15.9
14.4
14.4
16.1
16.2
14.6
15.4-
16.2
12.5
16.6
13.6
17.1
14.4
14.7
16.2
15.7
14.9
16.2
16.6
15.9
16.5
13.8
13.7
16.1
16.2
16.7
19.1
17.1
18.9
15.2
17.7
17.3
15.4
16.3
14.7
15.8
15.0
18.1
17.7
15.3
18.6
16.8
16.7
17.9
16.0
15.9
16.0
18.4
12.9
16.3
53
15.9
1.4
NOX
(PPMV)
SB3 = 3JSSST
214.2
224.4
184.9
213.6
188.7
155.1
137.7
137.2
124.1
122.8
145.0
125.5
151.7
129.5
133.5
132.4
124.4
140.1
136.0
133.8
129.9
144.0
120.7
123.2
116.3
122.4
165.2
134.0
145.2
140.3
107.4
133.1
116.1
118.9
126.3
136.0
130.5
118.5
127.7
104.7
104.6
98.8
97.0
99.3
145.1
109.7
131.5
101.3
93.6
91.9
97.7
89.1
90.9
53
131.4
29.8
A-15
-------
CEM Data at 3% Oc
Site ISW-A Test 2
NO.
TIKE
1300
1305
1310
1315
1320
1325
1330
1335
1340
1345
1500
1505
1510
1515
1520
1525
1530
1535
1540
1545
1550
1555
1600
1605
1610
1615
1905
1910
1915
1920
1940
1945
1950
1955
2000
2005
2010
2015
2020
2025
2030
PTS.
MEAN
STD
. OEV.
02
(SV)
9.0
10.3
12.4
11.5
11.2
11.3
8.9
9.6
11.9
11.0
10.1
10.9
10.0
12.1
12.2
11.9
13.8
13.0
11.7
12.5
11.1
13.1
10.5
9.7
10.2
10.7
12.0
12.2
13.9
15.0
12.6
15.3
14.0
12.2
9.2
11.3
11.0
12. .8
14.1
14.6
14.9
41
11.8
1.7
CO
(PPMV)
315.9
242.3
401.5
395.9
134.8
458.2
294.6
264.5
328.0
264.2
111.9
198.0
79.0
302.3
228.9
308.4
400.6
313.4
242.2
172.0
202.8
248.2
207.8
114.3
244.5
186.7
222.7
100.5
97.3
137.0
232.0
344.1
49.6
63.1
188.1
52.2
166.5
405.8
460.7
500.9
472.7
41
247.7
121.5
C02
?5SV)
14.1
12.8
14.9
18.3
17.6
21.2
12.9
16.2
14.9
17.15
17.1
16.1
14.7
15.3
15. «
15. <>
17. Ji
17. (5
14.9
17.0
20.
17.4
17. «
14.1
17.0-
18. 0
17.01
19.1
15.4
16.5
14.1
14.3
17.3
16.3
41
16.4
1.8
NOX
(PFMV)
112.0
112.8
107.4
116.4
111.0
148.5
90.2
92.3
108.2
104.9
164.8
148.4
102.4
99.9
98.7
235.7-
171.6
141.0
114.4
131.9
183.2
118.1
155.2
211.0
177.1
149.5
148.8
112.9
114.4
113.2
132.5
136.1
142.4
124.0
122.9
131.7
118.7
112.3
109.8
105.9
102.1
41
130.1
31.2
THC
(PPMV)
SS33SSS3
14.7
15.3
17.4
14.0
18.9
15.8
5.9
5.9
13 .0
14.4
9.0
9.8
9.6
11.7
12.4
11.0
15.1
10.9
9.2
12.1
9.8
11.2
8.5
7.3
8.8
8.7
10.6
11.3
18.3
10.8
14.9
11.5
10.4
6.2
11.1
7.8
11.4
18.4
18.7
18.0
40
12.0
3.6
A-16
-------
CEM Data 3% 0'
Site ISW-A Test 3
TIME
NO.
MEAN
STD.
1105
1110
1115
1120
1200
1205
1210
1215
1220
1225
1230
1235
1240
1245
1250
1255
1300
1305
1310
1315
1420
1425
1430
1435
1440
1445
1625
1630
1635
1640
1645
1650
1735
1740
1745
1750
1755
1800
1805
1810
1815
1820
1825
1830
1835
1840
1845
1850
1855
PTS.
OEV.
02
(JSV)
11.4
12.2
14.1
14.3
9.0
9.2
9.6
9.9
9.9
9.7
10.0
10.2
12.2
8.9
9.9
12.4
10.1
12.4
13.9
10.2
10.1
10.8
10.9
10.9
11.6
13.3
13.6
12.6
10.7
12.1
10.3
11.0
11.8
10.5
12.6
12.1
11.3
13.3
10.1
11.8
11.5
12.6
13.7
11.9
14.0
12.4
12.4
14.8
15.3
49
11.6
1.6
CO
(PPMV)
248.1
319.8
382.2
572.3
185.9
322.8
358.9
308.9
326.5
266.7
181.3
159.9
166.1
255.9
335.3
173.2
235.1
364.4
415.0
436.8
158.1
516.1
271.6
400.9
52.3
158.8
695.7
119.0
26.9
189.4
168.0
133.8
129.8
410.0
105.9
255.5
49.8
58.9
564.8
432.7
505.7
368.3
409.6
696.6
503.4
45
297.7
166.1
C02
(SV)
15.2
16.3
17.3
15.4
13.2
16.2
14.9
16.6
16.6
16.0
15.0
15.6
13.3
14.3
14.9
14.6
16.1
16.8
17.1
14.5
14.6
15.7
IS. 2
14.8
14.3
16.7
15.1
16.8
18.3
15.1
16.1
16.8
18.5
14.5
17.0
15.7
14.6
18.1
21.0
17.3
17.2
14.2
17.0
17.2
19.6
16.1
17.4
19.5
21.1
49
16.2
1.7
NOX
(PPMV)
113.8
167.1
195.8
131.2
146.7
135.2
131.9
143.6
142.3
165.7
165.5
155.6
145.6
155.6
142.2
186.1
170.1
169.0
170.4
124.8
133.2
134.4
138.8
139.5
137.8
104.8
113.7
152.9
143.1
147.7
123.2
110.. 6
111.4
118.9
119.6
135.3
123.1
207.2
114.8
114.2
100.1
109.6
176.0
125.3
116.0
107.5
104.7
107.3
48
138.1
25.3
THC
(PPMV)
7.1
6.7
12.7
4.3
4.3
5.0
4.9
4.7
4.5
5.2
5.0
6.1
4.5
4.5
7.1
5.0
5.8
6.0
4.0
4.2
3.9
3.5
3.5
3.9
6.2
7.8
6.7
4.7
5.5
4.2
3.9
4.2
4.1
7.9
5.8
5.1
7.6
3.3
3.8"
3.8
4.8
6.1
4.3
7.9
44
5.3
1.7
A-17
-------
CEM Data at 3% Q<:
Site ISW-A Test 4
TIKE
1030
1035
1040
1045
1050
1055
1100
1105
1110
1115
1120
1125
1130
1135
1140
1145
1150
1155
1200
1205
1210
1215
1305
1310
1315
1320
1325
1330
1335
1340
1345
1350
1355
1400
1405
1410
1415
1420
1425
1430
1435
1440
1445
1450
1455
1500
NO. PTS.
MEAN
02
(55V)
11.1
12.3
9.8
8.7
9.0
10.5
10.6
11.7
9.2
11.8
8.7
11.9
13.2
12.0
14.3
10.6
11.6
9.6
11.3
11.9
11.7
10.0
12.4
13.9
13.0
12.2
11.4
13.1
10.5
13.4
11.4
9.9
10.9
12.0
13.6
12.9
14.5
11.8
12.0
13.3
11.9
13.9
11.5
12.3
11.6
12.6
46
11.7
CO
(PPMV)
264.4
360.5
92.0
274.6
225.6
404.3
324.5
356.1
219.3
279. S
289.5
409.6
415.6
414.1
277.1
222.8
220.8
257.1
200.8
411.7
275.2
463.3
361.4
318.1
225.5
180.6
198.3
249.8
219.0
271.2
115.9
327.9
409.9
423.6
286.8
146.2
118.4
150.3
547.2
258.2
256.8
480.5
468.4
233.1
80.0
45
288.6
Gw2
C5V;>
18.3
15.4
17.0
12.7
16.9
15.0
15.3
13.6
15.1
15.7
17.7
11.4
15.2
15.1
14.6
15.13
13.9
14.0
17.2
15.4
16.4
14.1
13. «
15. 5
14. 9
20.7
15. 1
15.0
15, S
15.6
14.3
13.7
15.4
14.6
15.6
15. 9
14.0
13.6
16.11
17.0"
14.8
15.0
13.1
14.7
17.0
13.3
46
15.2
• KOX
(PPMV)
= S5J5 = = = SS
157.0
112.2
185.8
104.7
115.3
122.2
109.4
106.1
116.0
109.5
127.8
131.1
122.2
112.3
117.4
111.2
112.2
147.7
126.3
114.0
119.0
110.5
109.6
102.3
90.2
138.1
127.9
93.3
106.3
115.0
111.9
108.1
151.8
107.6
106.5
107.8
95.7
88". 3
85.7
84.2
92.5
81.0
74.1
123.1
125.3
110.7
46
113.6
THC
(PFMV)
= = :: = = = 3
13 .0
.8.3
6.4
4.7
7.3
6.2
4.7
4.7
3.3
4.1
2.7
2.9
4.0
3.3
4.7
3.5
3.9
3.1
3.6
4.0
4.1
3.5
3.9
5.2
10.0
4.0
3.4
4.6
3.0
3.7
2.9
2.3
2.4
3.1
3.2
2.9
3.7
2.7
2.7
3.7
4.7
4.9
3.7
4.9
4.2
4.5
46
4.3
STO. OEV.
1.4
109.2
1.6
20.2
2.0
A-18
-------
APPENDIX A-3
HC1 ACID TRAIN RESULTS
A-19
-------
-------
RAD
EPA
IAN
M E
8
T H
0 U R C E
0 D 2 -
TEST
DATA)
(RAW
PLANT
PLANT SITE
SAMPLING LOCATION
PLANT WASTE INCINERATOR (NORTH UNIT) EXHAUST
TEST *
DATE
TEST PERIOD
DIOXIN SITE #02
02-HCL-01
11/07/84
1104-1552 (1104-1252 / 1412-1552)
PARAMETER
VALUE
Sampling time (min.) 208
Barometric Pressure (in.Hg) 29.19
Sampling nozzle diameter (in.) .302
Meter Volume (cu.ft.) 144.181
Meter Pressure (in.H20) 1.8
Meter Temperature (F) 80.18
Stack dimension (sq.in.) 962.115
Stack Static Pressure (in.H20) -.38
Stack Moisture Collected (gm) 191.83
Absolute stack pressure(in Hg) 29.16206
Average stack temperature (F) 290.3637
Percent C02 4.84
Percent 02 17.58
P.ercent N2 77.58
Delps Subroutine result 13.56493
DGM Factor .9945
Pitot Constant .84
A-21
-------
RADIAN S
EPA M E T H
FINAL RE
PLANT
PLANT SITE
SAMPLING LOCATION
PLANT WASTE INCINERATOR (NORTH UNIT)
• -TEST #
DATE
TEST PERIOD
OURCE TEST
0 D S 2-5
S U L T S
DIOXIN SITE #02
EXHAUST
02-HCL-01
11/07/84
1104-1552 (1104-1252 / 1412-1552)
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vv gas(ncf)
Vv gas (scm)
% moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flow(dscfm)
Flow(dacmm)
I I
Z EA
137.3553
3.889903
9.044784
.2561483
6.178128
.9382187
29.4776
28.7685
2017.882
615.2078
13482.18
381.8154
8675.269
245.6836
102.3005
605.9727
A-22
Program Revision:I/16/
-------
RADIAN S
EPA M E T H
PARTICDLATE
PLANT
PLANT SITE
SAMPLING LOCATION
PLANT WASTE INCINERATOR (NORTH UNIT
TEST t
DATE
TEST PERIOD
OURCE TEST
0 D 5
LOADING
DIOXIN SITE #02
EXHAUST
02-HCL-01
11/07/84
1104-1552 (1104-1252 / 1412-1552)
PARAMETER
FRONT-HALF
BACK HALF
Total Grams
Grams/dscf
Grams/acf
Grains/dscf
Grains/acf
Grams/dscm
Grams/acm
Pounds/dscf
Pounds/acf
Pounds/Hr
Kilograms/Hr
0.1225000
0.0008918
0005739
0137612
0088548
0314911
0202633
0000020
0000013
0236070
4643052
5.,713 9000
0.0415994
0.0267676
0.6418789
0.4130246
1.4688750
0.9451652
0.0000917
0.0000590
47.7452300
21.6570900
Program Revision:I/16/84
A-23
-------
EPA METHOD 2-5
(RAW DATA)
PLANT DIOXIN SITE #02
PLANT SITE
SAMPLING LOCATION
PLANT WASTE INCINERATOR (NORTH UNIT EXHAUST
TEST.*
DATE
TEST PERIOD
02-HCL--03
11-09-84
1104-1859 (1104-1310/1328-1346/1629-1649/1739-1859)
PARAMETER
VALUE
Sampling time (min.) 244
Barometric Pressure (in.Hg) 29.18
Sampling nozzle diameter (in.) .302
Heter Volume (cu.ft.) 171.4041
Meter Pressure (in.H20) 1.8
Meter Temperature (F) 64.875
Stack dimension (sq.in.) 962.115
Stack Static Pressure (in.H20) -.38
Stack Moisture Collected (gm) 318.27
Absolute stack pressuredn Hg) 29.15206
Average stack temperature (F) 351.25
Percent C02 4.96
P.ercent 02 16.58
Percent N2 78.46
Delps Subroutine result 14.24123
DGM Factor .9945
Pitot Constant .84
A-24
-------
RADIAN S
EPA M E T H
FINAL RE
PLANT
PLANT SITE
SAMPLING LOCATION
»LANT WASTE INCINERATOR (NORTH UNIT
TEST #
DATE
TEST PERIOD
.104-1859 (1104-1310/1328-1346/1629-1649/1739-1859)
0 U R C E T
O D S 2-5
S U L T S
DIOXIN SITE
EXHAUST
02-HCL-03
11-09-84
E S T
#02
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vw gas(scf)
Vw gas (scm)
% moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flow(dscfm)
Flow(dscmm)
% I
% EA
167.9938
4.757583
15.00643
.4249821
8.200228
.9179977
29.4568
28.51732
2128.162
648.8297
14219
402.6821
8277.468
234.4179
111.7852
401.1187
Program Revision:1/16/84
A-25
-------
RADIAN SOURCE TEST
EPA METHOD 5
PARTICDLATE LOADING
PLANT DIOXIN SITE #02
PLANT SITE
SAMPLING LOCATION
PLANT WASTE INCINERATOR (NORTH UNIT EXHAUST
TEST * 02-HCL-03
DATE 11-09-184
TEST PERIOD
1104-1859 (1104-1310/1328-1346/1629-1649/1739-1859)
PARAMETER
Total Grams
Grams/dscf
Graras/acf
Grains/dscf
Grains/acf
Grams/dscm
Grams/acm
Pounds/dscf
Pounds/acf
Pounds/Hr
Kilograms/Hr
FRONT-HALF
BACK HALF
.2424000
.0014429
.0008400
.0222641
.0129609
.0509492
.0296596
.0000032
.0000019
.5801450
0.7167489
11.8580000
0.0705860
0.0410910
1.0891410
0.6340342
2.4923900
1.4509240
0.0001556
0.0000906
77.2993200
35.0627400
Program Revision:I/16/i
A-26
-------
KAD1AM SUUKO& i fc a
EPA METHOD 2-5
(RAW DATA)
PLANT DIOXIN SITE #02
PLANT SITE
SAMPLING LOCATION
PLANT WASTE INCINERATOR (NORTH UNIT EXHAUST
TEST #
DATE
TEST PERIOD
02-HCL-04
11/12/84
1023-1500 (1023-1218 / 1305-1500)
PARAMETER
VALUE
Sampling time (min.) 220
Barometric Pressure (in.Hg) 29.65
Sampling nozzle diameter (in.) .302
Meter Volume (cu.ft.) 163.672
Meter Pressure (in.H20) 1.8
Meter Temperature (F) 63.96
Stack dimension (sq.in.) 962.115
Stack Static Pressure (in.H20) -.38
Stack Moisture Collected (gm) 276.4
Absolute stack pressure(in Hg) 29.62206
Average stack temperature (F) 346.1667
Percent C02 4.4
Percent 02 18.2
Percent N2 77.4
D'elps Subroutine result 14.19654
DGM Factor .9945
Pitot Constant .84
A-27
-------
RADIAN SOURCE TEST
EPA METHODS 2-5
FINAL RESULTS
PLANT DIOXIN SITE #02
PLANT SITE
SAMPLING LOCATION
PLANT WASTE INCINERATOR (NORTH UNIT EXHAUST
TEST #
DATE
TEST PERIOD
02-HCL-04
11/12/84
1023-1500 (1023-1218 / 1305-1500)
PARAMETER
RESULT
Vm(dacf)
Vm(dacm)
Vv gas(ncf)
Vw gas (scm)
Z moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flov(dscfm)
Flow(dscmm)
Z I
Z EA
163.2722
4.623869
13.03226
.3690736
7.391906
.9260809
29.432
28.58696
2102.02
640 .-8596
14044.34
397.7356
8433.599
238.8395
118.2647
814.8286
Program Revision:I/16/
A-28
-------
RADIAN SOURCE TEST
EPA METHOD 5
PARTICULATE LOADING
PLANT DIOXIN SITE #02
PLANT SITE
SAMPLING LOCATION
»LANT WASTE INCINERATOR (NORTH UNIT EXHAUST
TEST #
DATE
TEST PERIOD
02-HCL-04
11/12/84
1023-1500 (1023-1218. / 1305-1500)
PARAMETER
FRONT-HALF
BACK HALF
Total Grams
Grams/dscf
Grams/acf
Grains/dscf
Grains/acf
Grams/dscm
Grama/acm
Pounds/dscf
Pounds/acf
Pounds/Hr
Kilograms/Hr
.0471000
.0002885
.0001732
.0044512
.0026729
.0101861
.0061167
.0000006
.0000004
0.3218706
0.1459996
8.6726000
0.0531174
0.0318969
0.8196019
0.4921694
1.8755760
1.1262800
0.0001171
0.0000703
59.2665700
26.8831400
Program Revision:1/16/84
A-29
-------
-------
APPENDIX A-4
AMBIENT AIR-XAD TRAIN FIELD RESULTS
A-31
-------
-------
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
I ftlNj SOURCE
METHOD 3: — 3
DIOXIN SITE #02
ROOF TOP NEXT TO AMBIENT AIR DAMPER
TOTAL AMBIENT RUN 4 DAYS TOTAL
11/7-B-9-12/S4
METER VOLUME FOR THE AMBIENT SAMPLE
PARAMETER
VALUE
Sampling time
-------
I
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
I i=Hx| SOURCE TE
METHODS S—S
RESUL-TS
DIOXIN SITE #02
ROOF TOP NEXT TO AMBIENT AIR DAMPER
TOTAL AMBIENT RUN 4 DAYS TOTAL
11/7-S-9-12/S4
METER VOLUME FCjR THE AMBIENT SAMPLE
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vw gas(sc-f)
Vw gas (scm)
% moisture
Md
MWd
MW
Vs(-fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flow(dsc-fm)
Flow(dscmm)
% I
% EA
473-1892
13.40072
.99534S5
28. 84
28.789
Program Revision:1/16/84
A-34
-------
APPENDIX A-5
EPA METHOD 3 FIXED GAS FIELD RESULTS
A-35
-------
-------
Fixed .Gas Analysis Results for ISW-A£
Run
Number
Sample
Number
1
2
3
4
5
6
7
Average
1
2
3
Average
1
2
3
4
5
6
Average
1
2
3
4
5
6
Average
Fixed Gas Concentrations(
0,
16.58
17.90
CO,
4.
4.
4.
5.
5.
4.
4,
00
36
26
44
95
4.81
5.09
4.84
4.96
19
30
4.77
5,
5.
3.
01
11
24
4.44
77.27
Total
Percentages
b Analysis by gas chromatograph/thermal conductivity detector.
Represents tedlar bags of flue gas collected according to EPA Method 3
Concentrations presented represent average values from duplicate sample
.analyses.
Sum of fixed gas concentrations.
analytical error.
Differences from 100 percent are due to
A-37
-------
-------
APPENDIX A-6
MODIFIED METHOD 5 AND
EPA METHODS 1-4 SAMPLE CALCULATIONS
A-39
-------
-------
RADIAN SOURCE TEST
EPA METHOD 2-5
SAMPLE CALCULATION
PLANT
PLANT SITE
SAMPLING LOCATION
NCINERATOR (NORTH UNIT
TEST g
DATE
TEST PERIOD
DIOX1N SITE #02
EXHAUST
02-MM5-01
11/07/84
1047-1545 (1047-1247 / 1345-1545)
1) Volume of dry gas sampled at standard conditions (68 deg-F ,29.92 in. Hg)'
Y x Vm x CT(std) t 460] x l~Pb t(Pm/13.6)D
Vm(std) = . —
P(std) x (Tm + 460)
.9973 x 181.776 x 528 x [ 29.19 t ( 1.937708 /13.6)H
Vm(std) = .
29.92 x ( 87.4 -t- 460)
Vm(std) = 171.427dscf
2) Volume of water vapor at standard conditions:
Vw(gas) = 0.04715 cf/gm x W(|) gm
Vw(gas) a 0.04715 x .292.7 = 13.801 scf
3) Percent Moisture in stack gas :
100 x Vw(gas)
Vj M — ™"""«»"»«»«^»«»«««»»«M^«.»»^^
Vm(std) + Vw(gas)
100 x 13.801
JM = • — 7.45 %
171 .427 -H 13.801
4) Mole fraction of dry stack gas :
100 - $M 100 - 7.45
Md = = = .9254927
100 100
A-41
-------
SAMPLE CALCULATION
PAGE TWO
5)Average Molecular Weight of DRY stack gas :
HWd » (.44 x 2C02) + (.32 x 302) + (.28 x ?>N2)
i
MWd = (.44 x 4.84 ) + (.32 x 17.58 ) + (.28 x 77.58 ) = 29.4776
6)Average Molecular IVelght of wet stack gas :
MW « MWd x Md + 18(1 - Md)
MW » 29.4776 x ,9254927 + 18(1 «• .9254927 ) = 28.62244
7) Stack gas velocity In feet-pei—minute (fpm) at stack conditions :
Vs « KpxCp x CSQRT '(dP)I]§avet x SQRT L~Ts §avgt] x SQRT Cl/(PsxMW)] x 60sec/ini
Vs » '85.49 x .84 x 60 x 13.87255 x SQRTp/( 29.16206 X 28.62244 )]
Vs * 2068.901 FPM ,
8) Average stack gas dry volumetric flow rate (DSCFM) :
I
Vs x As x Md x T(std) x Ps
144 cu. In./cu.ft. x (Ts +460) x P(std)
2068.901 x 962.115 x .9254927 x528x 29.16206
144 x 746.7917 x 29.92
Qsd » 8815.934 dscfm
Qsd »
Psd
A-42
-------
SAMPLE CALCULATION
PAGE THREE
)lsoklnetlc sampling rate (%) %
Dimensional Constant C = K4 x 60 x 144 x L~1 / (Pi /4)3
K4 = .0945 FOR ENGLISH UNITS . ...
I el -
I f> -
C x Vm(std) x (Ts + 460)
Vs x Tt x Ps x Md x (Dn)°2
1039.574 x 171.4268 x 746.7917
2068.901 x 240 x 29.16206 x .9254927 x( .309 )°2
\% = 104.0099
0) Excess air (%) :
100 x !?02 100 x 17.58
•««•«»"•*"»«••« — —• — — 3 •«•«»•«««••»•««•«•«••«
(.264 x $N2) - $02 (.264 x 77.58 ) - 17.58
EA = 605.97
1) Particulate Concentration :
Cs = ( grams part.) / Vm(std) = 0 / 171.4268
EA =
Cs =
Ca =
Ca =
Ca =
LBS/HR =
LBS/HR =
LBS/HR = 0
0.0000000 Grams/DSCF
T(std) x Md x Ps x Cs
P(std) x Ts
528 x .9254927 x 29.16206 x 0.0000000
29.92 x 746.7917
0.0000000 Grams/ACF
Cs x 0.002205 x Qsd x 60
O.OOOOOOOx 0.002205 x 8815.9 x 60
Program Revision:1/16/34
A-43
-------
R A
E P
D E
PARAMETER
TtCmFn.)
Dn( In.)
Ps( ln.H20)
Vm(cu.ft.)
Vw(gm. )
Pm( In.H20)
Tm(F)
Pb( In.Hg.)
3 C02
% 02
f, N2
SQR(DELPS)
As(sq. In. )
Ts(F)
Vm(dscf )
Vm(dscm)
Vw gas(scf)
% moisture
Md
MWd
MW
Vs(fpm)
F 1 ow (acf m)
F low(acmm)
F I ow( dscf m)
F low(dscmm)
% 1
% EA
DGH
Y
PS
Cp
dH
dP
*** EPA
STANDARD
CONDITIONS
DIAN SOURCE1 TEST ;
A METHODS 2:-5
FINITION OF TERMS ;
DEFINITION
TOTAL SAMPLING TIME
SAMPLING NOZZLE DIAMETER
ABSOLUTE STACK STATIC GAS PRESSURE
ABSOLUTE VOLUME OF GAS SAMPLE MEASURED BY DGM
TOTAL STACK MOISTURE COLLECTED
AVERAGE STATIC PRESSURE OF DGM
AVERAGE TEMPERATURE OF DGM
BAROMETRIC PRESSURE '
CARBON DIOXIDE CONTENT OF STACK GAS
OXYGEN CONTENT OF STACK GAS
NITROGEN CONTENT OF STACK GAS
AVE. SO. ROOT OF S-PIITOT DIFF, PRESSURE-TEMP, PRODUCT
CROSS-SECTIONAL AREA OF STACK(DUCT)
TEMPERATURE OF STACK
STANDARD VOLUME OF GAS SAMPLED ,Vm(std),AS DRY STD . C
STANDARD VOLUME OF GAS SAMPLED, Vm( std ), AS DRY STD. CM
VOLUME OF WATER VAPOR IN GAS SAMPLE, STD
WATER VAPOR COMPOS IT I1 ON OF STACK GAS
PROPORTION, BY VOLUME, OF DRY GAS IN GAS SAMPLE
MOLECULAR WEIGHT OF STACK GAS, DRY BASIS LB/LB-MOLE
MOLECULAR WEIGHT OF STACK GAS, WET BASIC LB/L3-MOLE
AVERAGE STACK GAS VELOCITY
AVERAGE STACK GAS FLOW RATE( ACTUAL STACK COND.)
AVERAGE STACK GAS FLOW RATE(ACTUAL STACK COND.)
AVERAGE STACK GAS VOLUMETRIC FLOW RATE(DRY BASIS)
AVERAGE STACK GAS VOLUMETRIC FLOW RATE (DRY BASIS)
PERCENT ISOKINETIC
PERCENT EXCESS AIR IN STACK GAS
DRY GAS METER
DRY GAS METER CORRECTION FACTOR
STACK STATIC GAS PRESSURE
PI TOT COEFFICIENT
ORIFICE PLATE DIFF. PRESS. VALUE
PITOT DIFF. PRESS. VALUE
Temperature = 68 deg«F (528 deg-R) j
Pressure = 29.92 In, Hg.
A-44
-------
APPENDIX B
PROCESS MONITORING DATA
B-l
-------
-------
APPENDIX B
CODE TO PROCESS DATA TABLES
(1) Feed weights in units of pounds.
(2) Feed type are as follows:
1 a Crate wood, paper, cardboard
2 » Treated wood
3 = Painted wood
4 » Wood/plastic cutoffs
5 « Hytest paint sludge
6 = Latex paint sludge
(3) Temperatures in units of °F.
(4) Water rates in units of
gpm.
(5) Boiler rate in units of Ib/hr steam.
(6) Boiler pressure in units of psig.
(7) Oil usage in units of gallons.
B-3
-------
-------
date
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
U784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
tile
936
936
937
937
939
948
955
955
1001
1005
1009
1012
1018
1018
1020
1024
1027
1029
1032
1036
1040
1044
1047
1052
1052
1056
1122
1125
1140
1142
1148
1158
1158
1158
1207
1207
1213
1217
1222
1226
1230
1233
1233
1241
1247
1247
1255
1257
1257
1315
feed
Height
207
153
140
163
405
353
70
309
156
194
164
201
116
238
265
138
195
58
237
118
39
224
188
120
29
768
745
154
148
156
430
283
34
400
150
340
148
155
114
320
.
185
284
395
55
46
186
104
28
300
feed
type
2
1
3
1
1
1
1
2
1
1
1
1
1
3
1
1
1
1
3
1
3
3
1
1
5
3
1
1
1
1
1
1
5
4
1
4
1
1
1
1
.
1
2
1
1
6
1
1
6
2
•ain
teip
.
t
.
f
.
.
.
,
.
1400
1400
1350
a
,
m
m
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1200
B
.
1200
a
.
1200
,
a
1550
9
1300
.
1200
1200
,
•
.
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9
t
1300
.
m
-a
1200
f
t
a
1300
,
.
stack
teip
a
t
m
f
t
,
,
,
(
1150
1400
1300
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m
B
t
a
1650
a
t
1650
.
,
1600
a
t
1400
m
1700
,
1650
1750
B
t
,
m
1650
t
.
1650
.
.
.
1700
,
.
g
1750
.
,
•ain stack boiler boiler
nater water rate pressure
« • t >
t
• • • •
•
• a a •
* • a a
" a a a
» • « a
« « a a
m
50 5
40 5
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•
• • • •
• « t i
40 5 8000 12
• » a i
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40 5 . 12
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40 5 11
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40 5 .
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a a a •
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a a i t
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40 5
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•
45 5
6600 12.5
.
« • • a
40 5
* • a a
• • a a
40 5
a a a a
B-5
-------
r
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11784
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
1335
1340
1342
1349
1354
• 1354
1358
1405
1413
1413
1424
1428
1431
1438
1504
1506
1511
1513
1521
1526
1532
1535
1542
1545
1133
1143
1146
1146
1151
1151
1158
1201
1204
1206
1210
1214
1219
1224
1227
1235
1242
1246
1251
1258
1309
1312
1317
1320
1324
1329
1329
1334
1340
1345
1349
1355
349
49
348
422
35
78
291
293
146
367
.
156
173
647
133
303
121
250
82
77
316
314
460
533.5
269
199
226
110
71
230
395
178
172
139
209
176
184
205
225
210
210
226
338
622
,
222
237
81
240
107
373
69
243
583
151
169
3 1650 1200
1
1 1450 1550
1
1
2
1 1300 1700
1
1 1300 1600
4
1450 1580
1
1
1
1
3
1
1 1550 1500
1
1 1450 1500
1
1 1450 1750
1 1400 1700
1
1 1200 300
1
2
1
4
3
1
1 1550 750
1
1
1
1
1
1
1
1 1600 1050
1
1
1
2
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1 1430 1420
1
1
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1
4
1
1
2
1 1250 1650
1
40 ! 5
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.
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.
40 I 5
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.
.
.
m
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35 4.5
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33 5
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f
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50 5
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.
47 5
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.
•
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f
.
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:
5200
12.5
B-6
-------
PLANT THO DATA
11384
11984
11384
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
11884
'11884
11884
11884
11384
11884
11884
11884
11884
11884
11884
11884
11884
11884
11384
11884
11884
11884
11884
11884
11884
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
1355
1359
1439
1443
1446
1455
1455
1510
1517
1523
1529
1535
1539
1542
1546
1550
1559
1559
1603
1610
1800
1807
1813
1826
1832
1836
1845
1853
1855
1355
1902
1904
1904
1915
1939
1943
1943
1949
1959
2005
2017
925
925
940
947
950
956
958
1002
1004
1004
1012
1014
1019
1024
1026
66
176
310
432
627
295
180
247
93
151
• 378
125
359
28
148
30
440
35
435
230
700
700
325
325
707
230.5
327
.
34
37.5
174
308
34.5
.
112
783
829
333
330
202
.
245
186
255
242
312
68
723
466
278
211
254
270
207
271
.
5
1
3
3
3
3
2
1
1
1
1
1
1
1
1
1
3
5
3
1
3
3
1
1
1
1
4
,
1
5
1
1
5
,
1
1
3
4
1
4
.
1
3
1
1
1
1
3
1
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1
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3
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1
.
,
,
1600
.
1450
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.
1600
.
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1730
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.
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9
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,
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,
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.
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1000
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1800
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1100
1060
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1520
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9
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60 3.5
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m
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.
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10 5
4500
11
B-7
-------
CLANI (NO
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
• 11984
• 11984
• 11984 .
• 11984
• 11984
• 11984
• 11984
• 11984
• 11984
• 11984
• 11984
• 11984
• 11984
• 11984
DATA
1031
1038
1041
1048
1050
1052
1054
1059
1102
1107
1111
1117
1118
1122
1127
1129
1131
1133
1136
1137
1142
1147
1157
1158
1158
1202
1206
1207
1211
1213
1220
1225
1225
1229
1231
1231
1237
1241
1244
1255
1256
1255
1309
1310
- 1315
1320
1330
1337
1337
1337
1342
1354
1355
1403
1409
1409
172
330
108
79
298
194
274-
.
.
.
.
.
376
230
278
i
397
.
590
t
878
601
.
376
394
•
,
.
312
.
271
85
208
.
315
112
.
24
365
.
349
90
.
200
211
297
.
188
240
392
52
704
.
364
101
303
1
1
1
1
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t
2
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1
.
3
1
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1
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1
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1
3
4
5
1
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1
2
.
.
1300
.
.
1300
1200
.
1280
1500
1610
,
9
1400
1300
.
.
.
1260
1280
,
1140
.
,
1100
1180
.
.
1130
.
.
.
1140
a
.
1230
m
m
1270
.
.
1300
.
.
.
1220
*
a
.
.
1175
1200
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.
.
• ' • • . .
. . . . .
i
• . . . .
1400 50 5
• a a a a
a a a ' ' * a a
1440 50 5 i
1620 50 5
8000 10.5
1310 50 5
1300 ....
1040 ....
a a a a a
t a i a a 'a
1050 60 5 . '• -
1280 ....
a a , a a a
7600 9 '
• • , a a • i
1570 ....
1350 60 5
a a 1 a a a
1750 ....
• a a a a
a a a a a
1820 65.. ',
1700 . . 7400 13 ;
7400 13
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1770 65
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1710 65..
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1680 65.. :
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1440 60 5
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1720 95
1800 ....
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B-8
-------
PLANT THO
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
'11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
DATA
1419
1425
1427
1428
1431
1433
1437
1441
1448
1553
1557
1602
1603
1607
1610
1610
1616
1619
1623"
1630
1633
1634
1641
1643
1643
1648
1715
1718
1723
1726
1730
1736
1741
1741
1742
1748
1749
1750
1753
1754
1755
1755
1803
1807
1807
1813
1816
1817
1817
1322
1822
1826
1828
1832
1838
1840
251
c
105
184
,
*
.
.
.
201
200
182
50
.
514
243
.
.
528
.
519
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366
308
304
265
.
175
482
.
t
348
55
.
*
154
.
.
45
255
133
*
416
29
. .
.
67
33
224
47
,
.
103
.
307
1
*
1
1
.
,
.
.
.
1
1
1
1
,
3
1
.
.
1
.
3
.
.
4
1
2
1
,
1
1
.
t
4
1
*
.
1
*
,
1
3
1
.
4
6
,
.
1
6
3
1
t
.
1
a
4
1400
,
1400
.
1400
1360
1420
1500
1870
1500
1750
1710
1710
,
1600
1550
1570
1650
1700
1800
1500
1430
B
a
t
9
1700
1730
t
1390
1340
m
t
1340
1350
.
1340
*
a
1300
,
1350
m
9
1390
1390
g
a
,
9
1330
1420
a
1450
,
.....
1650 ....
.
1630 - 60 5
7200 13
1720 60 5 ...
1620 ....
1550 60 5
1260 ....
630 60 ...
870 . ..... . ,- : -
1000 ....
1070 60 5
1000 ....
•
1270 60 5
1310 ....
1220 ....
1200 ....
1200 ....
1130 60 5
1570 ....
1350 ....
.
•
1
.
1000 ! '. \
1180 ....
• • t • .
1640 60 5
1350 ....
.
!
1500 60 5
1500 60 5
• « *
1440 .
7000 13
m
1650
^
1620 ...'.'
•
-
1470
1520 ....
•
.....
.....
•
1340 !
1480 ....
•
1400 '. !
B-9
-------
PUNT TWO
11984
11984
11984
11984
11984
111284
111284
111284
111284
111284
111284
111284
111284
111284
111234
111284
111284'
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284,
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
DATA
1840
1843
1848
1853
1856
946
956
1003
" 1015
1020
1022
1022
1024
1029
1035
1036
1040
1042
1042
1045
1050
1053
1059
1101
1103
1107
1108
1108
1110
1113
1117
1122
1131
1140
1140
1142
1143
1145
1147
1150
1155
1155
1200
1200
1202
1207
1209
1214
1214
1223
1225
1300
1302
1307
1310
1313
92
•
119
90
t
302
•
410
260
288
270
740
,
165
201
•
•
593
95
401
614
•
*
*
•
*
265
36
•
•
239
98
V
445
30
321
.
•
•
.
303
35
167
313
V
,
536
250
394
•
.
490
•
115
•
743
1
•
1
1
•
1
•
1
1
1
1
3
•
1
1
t
•
3
1
4
1
t
•
.
*
•
1
5
•
•
1
1
•
1
5
1
•
t
•
•
4
6
1
4
•
•
1
1
4
•
•
1
•
1
•
1
1410
1420
1340
•
•
1410
•
•
.
•
•
1590
a
•
1400
1500
*
t
1230
•
1230
1190
1200
1230
1230
1220
•
1190
1220
1250
•
1250
1320
•
.
1250
1250
1240
,
•
•
.
•
1300
1270
•
*
1290
1250
•
•
1420
•
1600
1590
;
1160 .
1130 . .
940 .
4000 12
• • ' • • . •
1120 . .
» • • • o
• • • i i
• • • • i
• « • » •
• « • • •
1300 . .
• * • • «
• i ; • • •
1280 ....
1300 56 ...
• • • • •
« • • • «
1650 ....
8000 12
1610
1600 6
1530 ....
1390 . .
1310 .
1750 . . .
• «...
1710 .
1500 .
1300 ....
» « • • •
1300 58
1150 58 6
t * • • •
* • • « i
1200 ....
1590 58 6
1510 58 6
7800 12
• • • • «
• • * • •
• • • • •
• • • • t
1450 . . " .
1400 .
• • • • •
• • • • •
1610 . . . . .
1800 ....
8000 12.6
• • • • •
1510 . . . .
t t • « •
1120 ....
1270 . . .
B-10
-------
PLANT THO DATA
111284
111284
111284
111284
111284
111284
111284
111284
111234
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111234
111284 •
111234
111284
111284
111284
111284
111284
111284
111284
111234
111284
1315
1315
1318
1330
1335
1342
1342
1342
1347
1350
1353
1354
1359
1405
1407
1407
1408
1415
1421
1421
1426
1426
1426
1435
1440
1444
1447
1448
1450
1500
1501
1505
403
28
a
192
,
903
24
116
295
.
114
.
,
.
563
29
55
517
750
29
31
105
432
.
.
.
,
t
,
. .
.
.
1
6'
.
1
,
1
5
4
3
.
1.
.
,
•
1 '
6
1
1
1
5
6
1
3
.
.
.
.
,
•
,
,
•
,
1700
.
.
.
1520
.
.
1450
.
1270
1300
1420
.
.
,
1450
1420
,
,
.
,
1400
1320
1400
1400
1370
1260
.
1150
1170
a • a a a
1270 ....
> , > , . . .
80000 12
» « a a a
1350 60 ...
• • • a a
a a a i a
1550 60 . .
• • • a •
1790 ....
1600 ....
1300 . . 7800 12.2
« « a • ,
• • a a •
" • « a «
1400 ....
1370 60 . t .
• • • a
.
« « t • a
• a • a a
1400 ....
1400 ....
1000 ....
1250 ....
1250 ....
1370 ....
7700 11
1400 ....
1300 ....
B-ll
-------
plant tuo oil usage data
date
11884
11884
11884
11384
11884
11884
11884
11884
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
11984
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
111284
beginning
tiie
1319
1720
1742
1803
1853
1858
1934
1955
1005
1035
1100
1109
1118
1130
1141
1200
1217
1256
1311
1331
1427
1451
1609
1717
1738
1808
1823
1021
1032
1045
1058
1111
1124
1137
1146
1158
1210
1223
1305
1320
1331
1346
1400
1415
1428
1442
ending
tiie
1720
1742
1803
1853
1858
1934
1955
2020
1035
1100
1109
1118
1130
1141
1200
1217
1256
1311
1331
1427
1451
1609
1717
1738
1808
1823
1849
1032
1045
1058
1111
1124
1137
1146
1158
1210
1223
1305
1320
1331
1346
1400
1415
1428
1442
1501
oil
usage
31.1
3.2
3.4
,6.3
1.3
5.5
3.5
3.6
4.4
3.9
1.5
1.6
1.9
1.3
1.4
0
2
1.7
0
6.3
2.2
13.2
10.9
3.8
3.5
2.1
2.8
2.4
2.1
1.7
1.6
2.3
2.3
1.3
1.6
2.2
1.8
8.5
2.6
2.2
2.7
1.3
2.6
2.6
2.5
3.1
B-12
-------
APPENDIX C
SAMPLE SHIPMENT LETTER
C-l
-------
-------
AD I AN
orporation
afcubei—25-, 1934
S. EPA Toxicant Analysis Center
uilding 1105
ay St. Louis, MS 39529.
ttention: Danny McDaniel
abject: Tier 4 - Analysis Instructions
ear Sir:
The objective of this letter is to clarify instructions and prior-
itiiss for individual samples from specific Tier 4 combustion sites
rus instruction letter is No. 2 and pertains to EPA Site No O? at
aypart;, MN. ~~
, Then!!P**°de No- is '2493> and SCC numbers assigned to this site were
umbers DQ0002O1 through DQOOO224.
SCC numbers DQOOO201 through DQOOO206 have been assigned to Troika
or internal QA/QC purposes. All remaining numbers have been assigned
o samples as described below.
The sample shipment for EPA Site No. O2 consists of 3 bo-=s
=n raining JX samples.
Please note that the container numbering scheme used for the
iified Method 5 (MM5) samples for EPA site 02 is different than that
se- for EPA site Ol. The change in the numbering scheme for EPA sit=
- resulted from two individual interpretations of the ASTM protocol
-id was not noticed in sufficient time to re-label all of the MM5
amplas. The scheme used at EPA site O2 will be used at all future
isr 4 test sites.
Instructions for extraction and analysis follow.
The following samples require IMMEDIATE EXTRACTION and analvsis
-------
U. S. EPA ECC Toxicdant Analysis Center
two
1934
Radian Run # O2-MM5-02
(Total of 6 train components)
SCC
DQOOO211
DQ000211
DQO00211
DQ000211
DG000211
DQ000211
Container
2
X J
srv
Fraction
Filter
XAD Module
Probe Rinse ;
Back Half /
Coil Rinse
Condensats
Impinger Solution
Radian Run # O2-MM5-Blank
(Total o-f 6 train components)
SCC
Container
Fraction
DQ000212
DQOOO212
DQ000212
DQOOO212
DQ000212
DQO00212
1
6
4
5
Filter
XAD Module :
Probe Rinse
Back Half /
Coil Rinse
Condensate
Impinger Solution
Radian Run # O2-MM5-O3
(Total o-f X* train components)
SCC # Container
Fraction
DQ000219
DQOOO219
DQ000219
DQ000219
DQ000219
DQ000219
DQ000219
1
1
6
2
4
5
Filter A
Filter B
XAD Module
Probe Rinse
Back Half /
Coil Rinse
Condensate
Impinger Solution
C-4
-------
S. EPA ECC Toxicant Analysis Center
ge three
4..-, ha.- "?«=: 1984
Radian Run # 02-MM5-04
(Total of 6 train components)
SCC #
Container
Fracti on
DQ000213
DQOOO213
DQOOO213
DQ000213
DQOOO213
DQ000213
1
6
Filter
XAD Module
Probe Rinse
Back Hal-F /
Coil Rinse
Condensate
Impinger Solution
Bottom Ash
SCC #
Process Sample
Samp11
DQ00021O
DQO00222
DQOOO224
DQ000217
DQOOO213
Ash
Ash
Ash
Ash
Ash
The following Priority 2# samples should be held for analysis pending
the results o-f Priority #1 analysis.
SCC #
DQOOO214
DQOOO214
DQ000214
Container
1
2
3
Fraction
======;==
Probe Rinse
XAD Module
Condensate
C-5
-------
•J. S. EPA ECC Toxicant Analysis Center
= age -four
•Z,l.~IJL!i 20, 1984
All Remaining Priority #2 and all Priority #3 samples for this sits
will be archived at Radian pending the results of Priority #2
analyses. These include the following:
SCC #
Sample
DQ000203
DQ000215
DQOOO22O
DQ000209
DQOOO221
DQ000223
DQOOO216
Waste feed composite
Waste feed composite
Waste feed composite
Fuel oil
Fuel oil
Fuel oil
Soi 1 s
If there are any questions concerning thfs sample shipment, please
:ntact either Gary Henry, Mike Palaazolo, or Andrew Miles at Radian
:rporation (919) 541-910O,
Sincerely,
TEST TEAM LEADER
C-6
-------
APPENDIX D
DIOXIN/FURAN ANALYTICAL DATA FOR GASEOUS SAMPLES
D-l
-------
-------
TABLE D-l. DIOXIN/FURAN ANALYTICAL DATA FOR MM5 TRAINS
Isomer/Homologue
Amount Detected, Picograms per Sample Train
Run 01 Run 02 Run 03 Run 04
Dioxins
2378 TCDD
Other TCDD
Penta CDD
Hexa CDD
Hepta CDD
Octa CDD
Total PCDD
Furans
2378 TCDF
Other TCDF
Penta CDF
Hexa CDF
Hepta CDF
Octa CDF
Total PCDF
2,000
33,000
50,000
98,000
117,000
48,000
348,000
11,000
337,000
351,000
560,000
390,000
53,000
1,702,000
2,000
38,000
55,000
81,000
98,000
43,000
317,000
9,600
309,400
288,000
207,000
215,000
39,000
1,068,000
7,000
124,000
155,000
187,000
239,000
84,000
796,000
31,000
692,000
681,000
629,000
426,000
87,000
2,546,000
5,000
83,000
113,000
152,000
312,000
56,000
721,000
22,000
670,000
739,000
696,000
597,000
61,000
2,785,000
0-3
-------
-------
APPENDIX E
RUN-SPECIFIC DIOXIN/FURAN EMISSIONS DATA
E-l
-------
-------
E-l
Run-Specific Dioxin/Furan Emissions Data
(As-measured Concentrations)
E-3
-------
-------
TABLE E-l. DIOXIN/FURAN EMISSIONS DATA FOR RUN 1, SITE ISW-A
Dioxin/Furan
Isoraer
Isomer Concentration
In Flue Gas
(ng/dscra)
Isomer Concentration
In Flue Gas
(ppt)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
4.12E-01
6.80E+00
1.03E+01
2.02E+01
2.41E+01
9.90E+00
N/A ) 3.08E-02( N/A )
N/A
N/A
N/A
N/A
5.08E-01(
6.97E-OH
1.24E+OOI
N/A )
N/A )
N/A )
1.37E+00( N/A )
N/A ) 5.18E-01{ N/A )
7.18E+01 4.36E+00
2.27E+00( N/A ) 1.78E-01( N/A )
6.95E+01
7.24E+01
1.15E+02
6.37E+01
1.09E+01
N/A ) 5.46E+00
N/A
N/A
N/A
N/A
5.12E+00
7.41E+00
3.75E+00
5.92E-01
3.34E+02 2.25E+01
N/A )
N/A )
N/A )
N/A )
N/A )
6.18E+00
1.02E+02
1.54E+02
3.03E+02
3.61E+02
1.48E+02
1.07E+03
3.40E+01
1.04E+03
1.08E+03
1.73E+03
9.54E+02
1.64E+02
5.01E+03
NOTE: Isomer concentrations shown are at as-measured oxygen conditions.
N/A - detection limits not applicable. QA samples indicate method
capability and detection limits.
ng = 1.0E-09g
ug = 1.0E-06g
ppt parts per trillion, dry volume basis
2200 operating hours per year
E-5
-------
TABLE E-2.DIOXIN/FURAN EMISSIONS DATA FOR RUN 2, SITE 2
Dioxin/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscm)
Isomer Concentration
In Flue Gas
(Ppt)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF .
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
5.39E-01(
1.02E+01(
1.48E+01(
2.18E+01(
2.64E+01(
1.16E+01(
8.54E+01
2.59E+00(
8.34E+01(
7.76E+01(
5.58E+01(
5.80E+01(
1.05E+01(
2.88E+02
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
j
)
)
)
,
)
)
)
)
4.03E-OZ(
7.65E-Oi(
1.00E+00(
1.34E+00(
1.50E+00(
6.06E-01(
5.25E+00
2.03E-01(
6.56E+00(
5.49E+00(
3.58E+00(
3.41E+OQ(
5.70E-01(
1.98E+01
N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
8.62E+00 i
1.64E+02 ,
2.37E+02
3.49E+02
4.23E+02
1.85E+02
1.37E+03
4.14E+01
1.33E+03 ;
1.24E+03 i
8.92E+02
9.27E+02 ''-
1.68E+02
1
4.60E+03
NOTE: Isomer concentrations shown are at as-measured oxygen conditions.
N/A - detection limits not applicable. QA samples indicate method
capability and detection limits.
ng » 1.0E-09g
ug - 1.0E-06g
ppt parts per trillion, dry volume basis
2200 operating hours per year
E-6
-------
TABLE E-3. DIOXIN/FURAN EMISSIONS DATA FOR RUN 3, SITE ISW-A
Dioxin/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscra)
Isomer Concentration
In Flue Gas
(ppt)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
1.47E+00( N/A )
2.61E+OK N/A ]
3.26E+OH N/A ]
3.94E+OH N/A
S.03E+01( N/A ;
1.77E+01( N/A ]
1.68E+02
6.53E+00
1.46E+02
1.43E+02
1.32E+02
8.97E+01
1.83E+01
5.36E+02
N/A J
N/A ;
N/A ;
N/A !
N/A
N/A ]
1.10E-01
1.95E-:-00
2.21E+00
2.42E+00
2.85E-:-00
N/A ;
N/A
N/A
N/A
N/A
9.25E-01( N/A
1.05E+01
5.13E-01
1.15E+01
1.01E+01
8.49E+00
N/A
N/A
N/A
N/A
5.27E+00( N/A
I 9.92E-01( N/A
3.69E+01
> 2.00E+01
3.55E+02
4.44E+02
5.36E+02
6.85E+02
2.41E+02
2.28E+03
) 8.88E+01
1 1.98E+03
1 1.95E+03
1 1.80E+03
1 1.22E+03
) 2.49E+02
7.29E+03
NOTE: Isomer concentrations shown are at as-measured oxygen conditions.
N/A - detection limits not applicable. QA samples indicate method
capability and detection limits.
ng = 1.0E-09g
ug » 1.0E-06g
ppt parts per trillion, dry volume basis
2200 operating hours per year
E-7
-------
TABLE E-4. DIOXIN/FURAN EMISSIONS DATA FOR RUN 4, SITE ISW-A
D1ox1n/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscm)
Isomer Concentration
In Flue Gas
(ppt)
Isomer Hourly
Emissions Rate
(ug/hr) '
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
1.01E+00(
1.68E+01(
2.29E+01
3.08E+01
6.33E+01
1.14E+01
1.46E+02
4.46E+00(
1.36E+02(
1.50E+02
1.41E+02?
1.21E+02(
1.24E+01(
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
7.
1,
58E-02
26E+OG
1.55E+00
.90E+00
58E+00
5.94E-01
8.96E+00
3.51E-OK
1.07E+01(
1.06E+01
9.0SE+00(
,12E+00(
.70E-01(
7.
6.
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
5.65E+02
3.85E+01
1.44E+01
2.39E+02
3.26E+02
4.38E+02
9.00E+02
1.61E+02
2.08E+03
6.34E+01
1.93E+03
2.13E+03
2.01E+03
1.72E+03
1.76E+02
3.03E+03
NOTE: Isomer concentrations shown are at as-measured oxygen conditions.
N/A - detection limits not applicable. QA samples indicate method
capability and detection limits.
ng - 1.0E-09g
ug » 1.0E-06g
ppt parts per trillion, dry volume basis
2200 operating hours per year
E-8
-------
E-2
Run-Specific Dioxin/Furan Emissions Data
(Concentrations Corrected to 3 Percent Oxygen)
E-9
-------
-------
TABLE E-5. DIOXIN/FURAN EMISSIONS DATA FOR RUN
Concentrations Corrected to 3% Oxygen
1, SITE ISW-A
D1oxin/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscm @ 3% oxygen)
Isomer Concentration
In Flue Gas
(ppt @ 3% oxygen)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-COF
Octa-CDF
Total PCDF
. ...
2.17E+00(
3.58E+01
5.43E+01
1.06E+02
1.27E+02
5.21E+01
3.78E+02
1.19E+01
3.66E+02
3.81E+02
6.08E+02
3.35E+02
5.75E+01
1.76E+03
N/A )
N/A
N/A
N/A
N/A
; N/A
( N/A
N/A
N/A
; N/A
; N/A
( N/A
1.62E-01(
2.68E+OOI
3.67E+OOI
6.54E+OOI
7.19E+OOI
2.72E+00!
2.30E+01
.
) 9.38E-01
2.87E+01
2.69E+01
3.90E+01
1.97E+01
3.12E+OOI
1.18E+02
N/A )
N/A ]
N/A ;
N/A ;
N/A ;
N/A ]
N/A ]
N/A
N/A !
N/A
N/A
[ N/A
6.18E+00
1.02E+02
1.54E+02
3.03E+02
3.61E+02
1.48E+02
1..07E+03
1 3.40E+01
I 1.04E+03
1.08E+03
1.73E+03
9.54E+02
1.64E+02
5.01E+03
NOTE: Isomer concentrations shown are corrected to 3% oxygen.
N/A - detection limits not applicable. QA samples indicate method
capability and detection limits.
ng » 1.0E-09g
ug = 1.0E-06g
ppt parts per trillion, dry volume basis
2200 operating hours per year
E-ll
-------
TABLE E-d DIOXIN/FURAN EMISSIONS DATA FOR RUN 2, SITE
Concentrations Corrected to 3% Oxygen
Dioxin/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscm @ 3% oxygen)
Isomer Concentration
I in Flue Gas
(ppt @ 3% oxygen)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
3.45E+00(
6.56E+01I
9.50E+01I
1.40E+02I
1.69E+02!
7.42E+01I
5.47E+02
1.66E+01
5.34E+02
4.97E+02
3.57E+02
3.71E+02
6.73E+01
1.84E+03
N/A )
N/A ]
N/A ;
N/A ;
N/A ;
N/A J
„
N/A
N/A
N/A
N/A
N/A
[ N/A
2.58E-01(
4.90E+OOI
6.42E+OOI
8.60E+00
9.58E+00
3.88E+00
3.36E+01
1.30E+00
4.20E+01
3.52E+01
2.29E+01
2.18E+01
3.65E+00
1.27E+02
N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
[ N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
8.62E+00
1.64E-HD2
2.37E+02
3.49E+02
4.23E+02
1.85E+02
1.37E4-03
4.14E+01
1.33E+03
1.24E+03
8.92E+02
9.27E+02
1.68E+02
4.60E+03
NOTE: Isomer concentrations shown are corrected to 3% oxygen.
N/A - detection limits not applicable. QA samples indicate method
capability and detection limits.
ng - 1.0E-09g
ug - 1.0E-06g
ppt parts per trillion, dry volume basis
2200 operating hours per year
E-12
-------
TABLE E-7. DIOXIN/FURAN EMISSIONS DATA FOR RUN
Concentrations Corrected to 3% Oxygen
3, SITE ISW-A
D1oxin/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscm @ 3% oxygen)
Isomer Concentration
In Flue Gas
(ppt (3 3% oxygen)
Isomer Hourly
Emissions Rate
(ug/hr)
OIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
4.89E+00(
8.67E+01?
1.08E+02(
1.31E+02(
1.67E+02<
5.87E+01I
5.57E+02
2.17E+01
4.84E+02
4.76E+02
4.40E+02
2.98E+02
6.08E+01
1.78E+03
•
N/A
N/A
N/A
N/A
N/A :
N/A ;
N/A
N/A
N/A
N/A
N/A
N/A
3.66E-OK
6.48E+00
7.32E+OOi
8.04E+OOI
I 9.46E+OOI
3.07E+OOI
3.47E+01
1.70E+00
3.80E+01
3.37E+01
) 2.82E+01
) 1.75E+01
) 3.30E+00
1.22E+02
N/A
N/A
N/A
k N/A
k N/A
, N/A
( N/A
; N/A
! N/A
N/A
N/A
N/A
)
j
)
Z.OOE+01
3.55E+02
4.44E+02
5.36E+02
6.85E+02
2.41E+02
2.28E+03
8.88E+01
1.98E+03
1.95E+03
1.80E+03
1.22E+03
2.49E+02
7.29E+03
NOTE: Isomer concentrations shown are corrected to 3% oxygen.
N/A => detection limits not applicable. QA samples indicate method
capability and detection limits.
ng - 1.0E-09g
ug - 1.0E-06g
ppt parts per trillion, dry volume basis
2200 operating hours per year
E-13
-------
TABLE E-8. DIOXIN/FURAN EMISSIONS DATA FOR RUN
Concentrations Corrected to 3% Oxygen
4, SITE ISW-A
Dioxln/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscm @ 3% oxygen)
Isomer Concentration
In Flue Gas
(ppt @ 3% oxygen)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
'Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
*
6.52E+00(
1.08E+02
1.47E+02
1.98E+02
4.07E+02
7.30E+01
N/A
N/A
N/A
N/A
N/A
N/A ]
9.40E+02
2.87E+01I
8.74E+02
9.64E+02
9.08E+02
7.78E+02
7.95E+01
[ N/A
N/A
N/A
N/A
N/A
N/A
3.63E+03
4.87E-01
8.09E+00
9.96E+00
1.22E+01
2.30E+01
1 3.82E+00
N/A )
N/A )
N/A
N/A )
k N/A )
L N/A )
5.76E401
) 2.26E+00
6.87E+01
6.82E+01
1 5.82E+01
4.58E+01
4.31E+00
N/A )
N/A )
N/A
N/A )
N/A )
N/A )
2.47EH-02
1.44E+01
2.39E+02
3.26E+02
4.38E+02
9.00E+02
1.61E+02
2.08E+03
6.34E+01
1.93E+03
2.13E+03
2.01E+03
1.72E+03
1.76E+02
8.03E+03
NOTE: Isomer concentrations shown are corrected to 3% oxygen.
N/A - detection limits not applicable. QA samples indicate method
capability and detection limits.
ng - 1.0E-09g
ug « 1.0E-06g
ppt parts per trillion, dry volume basis
2200 operating hours per year
E-14
-------
APPENDIX F
RUN-SPECIFIC RISK MODELING INPUT DATA
F-l
-------
-------
TABLE F-l. RISK MODELING PARAMETERS FOR RUN 1, SITE ISW-A
Latitude - 45 Degrees, 01 Minutes, 28 Seconds
Longitude * 92 Degrees, 46 Minutes, 40 Seconds
Stack Height (From Grade Level) - 36.6 m .
Stack Diameter (ID) - 0.91 m
Flue Gas Flow Rate (Dry Standard) - 249.7 dscmm
Flue Gas Exit Temperature - 414.7 Degrees K
Flue Gas Exit Velocity (Actual) - 631 mpm
Dioxin/Furan
Isomer
2378 TCDD
Other TCDD
2378 TCDF
Other TCDF
Penta-CDD
Penta-CDF
Hexa-CDD
Hexa-CDF
Hepta-CDD
Hepta-CDF
Octa-CDD
Octa-CDF
Isomer
Concentration
In Flue Gas
(ng/dscm)
4.12E-01
6.80E+00
2.27E+00
6.95E+01
1.03E+01
7.24E+01
2.02E+01
1.15E+02
2.41E+01
6.37E+01
9.90E+00
1.09E+01
Isomer Hourly
Emissions
Rate
(ug/hr)
6.18E+00
1.02E+02
3.40E+01
1.04E+03
1.54E+02
1.08E+03
3.03E+02
1.73E+03
3.61E+02
9.54E+02
1.48E+02
1.64E+02
Relative
Potency
Factor
1.000
.010
.100
.001
.500
.100
.040
.010
.001
.001
.000
.000
2,3,7,8 - TCDD
Equivalent
Emissions
(mg/yr)
1.36E+01
2.24E+00
7.47E+00
2.29E+00
1.70E+02
2.39E+02
2.66E+01
. 3.81E+01
7.95E-01
2.10E+00
.OOE+00
.OOE+00
Net 2378 TCDD Equivalent Atmospheric Loading
5.02E+02
NO
N/A
ng
ug
mg
not detected (detection limit in parentheses)
detection limit not available
1.0E-09g
1.0E-06g
1.0E-03g
Standard conditions: 293 K (20 C) temperature and 1 atmosphere pressure.
2200 operating hours per year
F-3
-------
TABLE P-2RISK MODELING PARAMETERS FOR RUN 2, SITE 2
Latitude - 45 01 28
Longitude - 92 46 40
Stack Height (From Grade Level) = 36.6 m
Stack Diameter (ID) - 0.91 m
Flue Gas Flow Rate (Dry Standard) = 266.60 dscmm
Flue Gas Exit Temperature =» 431 K •
Flue Gas Exit Velocity (Actual) =• 700.2 mpm
Dioxin/Furan
Isomer
Isomer
Concentration
In Flue Gas
(ng/dscm)
Isomer Hourly
Emissions
Rate
(ug/hr)
Relative
Potency
Factor
2,3,7,8 - TCDD
Equivalent
Emissions
(mg/yr)
2378 TCDD
Other TCDD
2378 TCDF
Other TCDF
Penta-CDD
Penta-CDF
Hexa-CDD
Hexa-CDF
Hepta-CDD
Hepta-CDF
Octa-CDD
Octa-CDF
5.39E-01
1.02E+01
2.59E+00
8.34E+01
1.48E+01
7.76E+01
2.18E+01
5.58E+01
2.64E+01
5.80E+01
1.16E+01
1.05E+01
8.62E+00
1.64E+02
4.14E+01
1.33E+03
2.37E+02
1.24E+03
3.49E+02
8.92E+02
4.23E+02
9.27E+02
1.85E+02
1.68E+02
1
Net 2378 TCDD Equivalent Atmospheric Loading
.000
.010
.100
.001
.500
.100
.040
.010
.001
.001
.000
.000
1.90E+01
3.
9.
2.
.60E+00
,11E+00
.93E+00
2.61E+02
2.73E+02
3.07E+01
1.96E+01
9.30E-01
2.04E+00
.OOE+00
.OOE+00
6.22E+02
NO » not detected (detection limit in parentheses).
N/A - detection limit not available
ng •* 1.0E-09g
ug - 1.0E-06g
mg - 1.0E-03g
Standard conditions: 293 1C (20 C) temperature and 1 atmosphere pressure.
2200 operating hours per year
F-4
-------
TABLE F-3-. RISK MODELING PARAMETERS FOR RUN 3, SITE ISW-A
Latitude > 45 Degrees, 01 Minutes, 28 Seconds
Longitude - 92 Degrees, 46 Minutes, 40 Seconds
Stack Height (From Grade Level) - 36.6 m
Stack Diameter (ID) - 0.91 m
Flue Gas Flow Rate (Dry Standard)-- 226.7
Flue Gas Exit Temperature - 460.2 Degrees K
Flue Gas Exit Velocity (Actual) - 643 mpm
Dioxin/Furan
Isomer
2378 TCDD
Other TCDD
2378 TCDF
Other TCDF
Penta-CDD
Penta-CDF
Hexa-CDD
Hexa-CDF
Hepta-CDD
Hepta-CDF
Octa-CDD
Octa-CDF
Isomer
Concentration
In Flue Gas
(ng/dscm)
1.47E+00
2.61E+01
6.53E+00
1.46E+02
3.26E+01
1.43E+02
3.94E+01
1.32E+02
5.03E+01
8.97E+01
1.77E+01
1.83E+01
Isomer Hourly
Emissions
Rate
(ug/hr)
2.00E+01
3.55E+02
8.88E+01
1.98E+03
4.44E+02
1.95E+03
5.36E+02
1.80E+03
6.85E+02
1.22E+03
2.41E+02
2.49E+02
Relative
Potency
Factor
1.000
.010
.100
.001
.500
.100
.040
.010
.001
.001
.000
.000
2,3,7,8 - TCDD
Equivalent
Emissions
(mg/yr)
4.41E+01
7.81E+00
1.95E+01
4.36E+00
4.88E+02
4.29E+02
4.71E+01
3.96E+01
1.51E+00
2.68E+00
.OOE+00
.OOE+00
Net 2378 TCDD Equivalent Atmospheric Loading
1.08E+03
NO - not detected (detection limit In parentheses).
N/A - detection limit not available
ng - 1.0E-09g
ug - 1.0E-06g
mg a 1.0E-03g
Standard conditions: 293 K (20 C) temperature and 1 atmosphere pressure.
2200 operating hours per year
F-5
-------
TABLE F-4. RISK MODELING PARAMETERS FOR RUN 4, SITE ISW-A
Latitude - 45 Degrees, 01 Minutes, 28 Seconds
Longitude - 92 Degrees, 46 Minutes, 40 Seconds
Stack Height (From Grade Level) - 36.6 m
Stack Diameter (ID) » 0.91 m
Flue Gas Flow Rate (Dry Standard) - 236.9 dscmm
Flue Gas Exit Temperature - 450.0 Degrees K
Flue Gas Exit Velocity (Actual) - 641 mpm
Dioxin/Furan
Isomer
Isomer
Concentration
In Flue Gas
(ng/dscm)
Isomer Hourly
Emissions
Rate
(ug/hr)
Relative
Potency
Factor
2,3,7,8 - TCDD
Equivalent
Emissions
(mg/yr)
2378 TCDD
Other TCDD
2378 TCDF
Other TCDF
Penta-CDD
Penta-CDF
Hexa-CDD
Hexa-CDF
Hepta-CDD
Hepta-CDF
Octa-CDD
Octa-CDF
1.01E+00
1.68E+01
4.46E+00
1.36E+02
2.29E+01
50E+02
08E+01
1.41E+02
6.33E+01
1.21E+02
1.14E+01
1.24E+01
1,
3.
1.44E+01
2.39E+02
6.34E+01
1.93E+03
26E+02
13E+03
1
3,
2.
4.38E+02
2.01E+03
9.00E+02
1.72E+03
1.61E+02
1.76E+02
Net 2378 TCDD Equivalent Atmospheric Loading
.000
.010
.100
.001
.500
.100
.040
.010
.001
.001
.000
.000
17E+01
27E+00
40E+01
25E+00
58E+02
69E+02
86E+01
4.42E+01
1.98E+00
3.79E+00
.OOE+00
.OOE+00
9.71E+02
ND
N/A
ng
ug
mg
not detected (detection limit in parentheses)
detection limit not available
1.0E-09g
1.0E-06g
1.0E-03g
Standard conditions: 293 K (20 C) temperature and 1 atmosphere pressure.
2200 operating hours per year
F-6
-------
APPENDIX G
RESEARCH TRIANGLE INSTITUTE (RTI)
SITE ISW-A SYSTEMS AUDIT
G-l
-------
-------
QUALITY ASSURANCE AUDIT FOR TIER 4 OF THE
NATIONAL DIOXIN STUDY:
INDUSTRIAL INCINERATOR SITE ISW-A
by
Richard V. Crume
EP'A Contract No. 68-02-3149
Work Assignment 10-1
RTI Project No. 472^2500-48
EPA Technical Project Monitor
Robert Olexsey
Prepared for
William B. Kuykendal, Air Management Technology Branch
Monitoring and Data Analysis Division
Office of Air Quality Planning and Standards
Environmental Protection Agency
Research Triangle Park, NC 27711
February 1985
-------
-------
TABLE OF CONTENTS
Chapter
1.0
2.0
3.0
4.0
5.0
6.0
Page
Summary ^
Introduction 5
2.1 Process Description 6
2.2 Test Program Design 7
2.3 Audit Objectives '.'.'.'. 8
Comments and Recommendations 13
3.1 Introduction . 13
3.2 'Process Operation 13
3.3 Modified Method 5 Sampling Train .... 14
3.4 Blank MM5 Sampling Train .' 15
3.5 Ambient MM5 Sampling Train 16
3.6 HC1 Sampling Train . . .* 16
3.7 Continuous Emission Monitors 17
3.8 Process Samples [."!." 18
3.9 Sample Handling, Transportation, and Storage ... 18
3.10 Soil Sampling 19
Conclusions 20
References. 21
Appendix ^ 22
6.1 Audit Checklists 22
-------
-------
TABLES
Number
1 List of Persons Present During RTI Audit
2 Summary of Recommendations .......
3
4
Critical Quality Assurance Elements
Reference Materials Used to Evaluate the Radian
Test Program .....
Page
2
3
9
12
-------
-------
1.0 SUMMARY
On November 8, 1984, Research Triangle Institute (RTI) performed a
quality assurance (QA) audit of an emission test program underway at an
industrial incinerator located at site designation "ISW-A." The emission
test program was one of a series of tests performed by Radian Corporation
for the U.S, Environmental Protection Agency (EPA). The data collected
during these tests will be added to the data base supporting Tier 4 of
EPA's National Dioxin Study. ("Tier 4" refers to those combustion sources
having the potential to emit significant concentrations of a dioxin compound
known as 2,3,7,8-tetrachlorodibenzo-p-dioxin, or 2,3,7,8-TCDD. 2,3,7,8-TCDD
is a potential human carcinogen.) The audit was performed by Richard
Crume, an environmental engineer with RTI. The EPA Project Officer is
William Kuykendal, of the Office of Air Quality Planning and Standards,
Research Triangle Park, North Carolina. A list of persons present during
the audit is presented in Table 1.
The goals of the audit were to: (1) evaluate Radian Corporation's
adherence to the test program's test plan and QA plan; (2) document the
test procedures used; and (3) make any recommendations that could improve
the quality of data collected during future tests. Overall, RTI was
impressed with the test team and the quality of their work. Although on
the day of the audit several process disruptions occurred, these problems
were beyond the control of the Radian test team. RTI is satisfied that the
data generated by the test program will be of sufficient quality to achieve
the objectives of the study, provided that: (1) the analytical procedures,
which will be evaluated under a separate audit, are performed correctly;
and (2) the sampling procedures continue to be performed with the same
level of care exhibited during the Site ISW-A tests.
RTI's audit recommendations are summarized in Table 2. These recom-
mendations address problems which are not serious enough to invalidate the
test results. However, the implementation is crucial for two reasons:
-------
TABLE 1. LIST OF PERSONS PRESENT DURING RTI AUDIT
Name
Affiliation
Mike Palazzolo
Dave Dayton
Lee Garcia
Gary Henry
Jim McReynolds
Dave Savia
Bob Mournigham
Richard Crume
Radian (Test Team Leader)
Radian
Rad i an
Radian
Radian
Radian
EPA (Cincinnati)
Research Triangle Institute
-------
TABLE 2. SUMMARY OF RECOMMENDATIONS
Modified Method 5 (MM5) Sampling Train
Radian should mount the MM5 sampling train's XAD-condenser in a
vertical position during future tests. Alternatively; R«dian —-
should explain in each test report: (1) why the condenser mount-
ing position differs from the test protocol; and (2) what effect
this is likely to have on the outcome of that particular series
of tests (e.g., was all moisture observed to be carried forward
into the resin).
Blank MM5 Sampling Train
The front and back ends of the blank MM5 train should remain
sealed throughout each test. The probe should be sealed with
hexane-rinsed aluminum foil and the last impinger with a ground
glass cap.
Ambient XAD Sampling Train
Ordinarily the XAD resin trap associated with the ambient sam-
pling train is kept in place between the 4-hour test runs and is
not removed until the final test run at a given site is complete.
The resin trap should be cooled between test runs as well as
during the runs. This iis especially important whenever the train
is located in hot or variable-temperature environments.
HC1 Sampling Train
During the audit the HC1 sampling probe broke, thereby invali-
dating the HC1 results. More care should be taken in the future
to avoid breakage of equipment.
Continuous Emission Monitors
Calibration and quality control gases for the continuous emission
monitors should test the entire sampling interface, beginning at
the stack.
Once the span check of a continuous monitor has been completed
the monitor's reading should be allowed to return to zero before
challenging the meter with a quality control gas.
If possible, Radian's continuous monitor data acquisition system
should incorporate a time constant to average out positive and
negative noise peaks in the monitor signal.
(continued)
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TABLE 2 (continued)
Temperature variations within the continuous monitor trailer
should be minimized so that continuous monitor stability will be
improved.
r Continuous monitor strip charts should be offset a positive 10%
from zero to avoid negative drift.
Sample Handling, Transportation, and Storage
The liquid level on all sample collection bottles should be
marked at the time of collection.
Soil Sampling
Soil sampling should be conducted over a wide area where potential
dioxln contamination is most likely.,
• • Soil samples should be composited using an appropriate tool, such
as a hexane-rinsed garden trowel.
All debris (e.g., leaves and dead grass) should be cleaned from
the ground before soil sampling is begun.
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(1) the recommendations will help prevent potential problems from developing
.in the future; and (2) the recommendations will bring all test procedures
into agreement with the written protocols.
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2.0 INTRODUCTION
2.1 PROCESS DESCRIPTION
The process unit under study during the Site ISW-A incinerator test
program was a Kelley Model 2500 waste incinerator rated at 18 MMBtu/h.
This unit consists of primary and secondary combustion chambers, a waste
heat boiler, and a steam turbine. Various waste materials are burned,
including:
Paint filters and dry paint,
Paint sludge,
Wood/plastic cutoffs,
Wooden crate parts,
Paper'and cardboard, and
Office and cafeteria Waste.
No. 2 fuel oil is burned to help sustain combustion. Additionally, the in-
cinerator is fed about every 10 minutes on a batch basis so that a total of
approximately 1 ton of waste material is burned each hour. Emissions are
ducted to a stack that stands about 30 feet above the roof of the two-story
building housing the incinerator.
Four aspects of the incinerator design must be carefully considered in
designing a successful emission test program. These aspects are summarized
below:
Ambient Air Damper: This damper, which is about 30 feet from the
top of the stack, opens or closes as required to maintain a
design draft in the secondary chamber. The amount of dilution
air introduced by this damper must be considered when deciding
upon the stack sampling time required to obtain a detectable
concentration of the desired pollutant.
Exhaust Fan: The ID fan, located upstream of the boiler, cuts en
and off according to the demand for steam and the associated
bypass of gases past the boiler. The periodic switching on and
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off of this fan requires that stack isokinetic sampling rates be
watched carefully. :
Ash Pushing: Several times each daiy ash is pushed from the
bottom of the incinerator into disposal carts, causina large
clouds of dust to be carried up the stack. The selection of the
testing period must take into account the ash pushing schedule so
that a representative number of pushes can be included in the
test.
Batch Loading of Wastes: Waste materials are loaded into the
incinerator on a batch basis. This has the potential to cause
variations in stack exhaust rates, making careful control of
isokinetic sampling rates important.
More details concerning the incinerator design can be found in Radian
Corporation's Test Plan.1
2.2 TEST PROGRAM DESIGN
The test program can be divided into the following categories:
Process monitoring,
Modified Method 5 (MM5) sampling train,
Blank MM5 sampling train.,
Ambient MM5 sampling train,
HC1 sampling train,
Continuous emission monitors,
Process samples,
Sample handling, transportation, and storage, and
Soil sampling.
Details concerning these systems can be found in Radian Corporation's Test
Plan,1 Quality Assurance Plan,2 and Sampling Procedures Document.3
The most important aspect of the test program concerns the sampling of
organic compounds (including any dioxins present in the gas stream) using
a MM5 sampling train. The MM5 train is similar to the EPA Method 5 train,
except that a sorbent trap for the collection of vapor phase organics is
included. The trap consists of separate sections for cooling the gas ;
stream and for adsoroing the organic compounds onto Amberlite XAD-2 resin.
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The setup and operation of the MM5 train are described in detail in the
"ASME MM5 Sampling Methodology for Chlorinated Organics" contained in
Radian's Test Plan.1 Three test runs, each of approximately 4 hours'
duration, were to be conducted at the test site.
2.3 AUDIT OBJECTIVES
The goals of the audit were to evaluate the quality of work performed
by Radian Corporation, to document the test procedures used, and to make
any recommendations that could improve the quality of data collected during
future tests. These goals were achieved by performing two types of audit
activities: systems audits and performance audits.
A systems audit consists of an onsite inspection and review of the
test procedures (including any QA activities) associated with test program
measurements. RTI's systems audit of the Radian test began with an evalua-
tion of Radian's QA project plan.2 This plan was evaluated according to
the criteria presented in EPA's QAMS-005/80 guideline document and summarized
in Table 3.4 Radian's test plan was similarly evaluated, although adherence
to the QAMS-005/80 criteria was not required. RTI's comments on the Radian
QA and Test Plans were previously submitted.5 6 The systems audit continued
with an onsite inspection of the Radian test program and the preparation of
this report. (An onsite systems audit of Radian's analytical laboratory
will also be performed in early 1985. The results of the laboratory audit
will be presented in a separate report.)
The objectives of a performance audit are similar to those of a systems
audit (i.e., to evaluate the quality of data likely to be generated by the
test or experimental program). The performance audit differs from the
systems audit in-that it involves the actual measurement of critical test
program parameters using standardized reference materials. RTI's perform-
ance audit of the Radian test program utilized the materials listed in
Table 4. Radian, its subcontractor, and EPA's Troika Laboratories will
analyze these materials and return the results to RTI for evaluation. The
results, which will be useful in assessing the accuracy and precision of
the measurement systems, will be discussed by RTI in a separate report."
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TABLE 3. CRITICAL QUALITY ASSURANCE ELEMENTS
Project Description
Project description
Experimental design
Intended use of acquired data
Start and completion dates
Appropriate diagrams, tables, and figures
Project Organization and Responsibility
Organization of project
Line of authority
Key individuals (including quality assurance official)
Quality Assurance Objectives for Measurement Data
Precision
Accuracy
Completeness
Represents ti veness
Comparability
Sampling Procedures
Sampling site selection
Sampling procedures i
Description of containers for sample collection, preservation,
transport, and storage
Procedures to avoid sample contamination
Sample preservation methods and holding times
Procedures for recording sample history, sampling conditions, and
analyses to be performed
Sample Custody Records
Preparation of reagents or supplies associated with sample
Location and conditions where sample was taken
Sample preservation methods
Labeling
Field tracking forms
Field and laboratory sample custodians
Laboratory custody log
Laboratory handling, storage, and dispersement procedures
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Table 3. Continued
Calibration Procedures
Description of,' or reference to, calibration procedure
Frequency of calibration
Calibration standards, including sources and traceability
procedures
Analytical Procedures
Analytical procedure
Appropriateness of method
Data Reduction, Validation, and Reporting
Data reduction scheme
Equations to be used
Validation procedures
Identification and treatment of outliers
Internal Quality Control Checks
Replicates
Spiked samples
Split samples
Control charts
Blanks
Internal standards
Performance and Systems Audits
Schedule for conducting audits
Systems to be audited
Sources of audit materials
Zero and span gases
Quality control samples
Surrogate samples
Reagent checks
Calibration standards and devices
Procedures to Assess Data Precision, Accuracy, and Completeness
Central tendency and dispersion
Measures of variability
Significance test
Confidence limits
Testing for outliers
Preventive Maintenance
Schedule of maintenance tasks
List of critical spare parts on hand
10
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Table 3. Continued
Corrective Action
Predetermined limits for data acceptability
Procedures for corrective action
Responsible individuals
Quality Assurance Reports to Management
Frequency of reporting
Responsible individuals
Significant problems and recommended solutions
11
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TABLE 4. REFERENCE MATERIALS USED TO EVALUATE
THE RADIAN TEST PROGRAM
Material
Description
1. Fuel oil
2. Fuel oil
3. Fuel oil
4. HC1 impinger solution
5. HC1 impinger solution
6. Dust sample
7. Particulate sample
8. Computer data
9. Calibrated orifice
Fuel oil spiked with known chloride
concentration.
Similar to Material No. 1.
Similar tor Material No. 1.
HC1 train impinger solution having
verified chloride concentration.
Similar to Material No. 4.
Dust sample having known 2,3,7,8-TCDD
concentration.
Particulate sample having known
2,3,7,8-TCDD concentration.
Data to be fed into Radian's computer
to examine the accuracy of the computer
calculations.
Used to evaluate the sampling trains'
dry gas meter calibrations.
12
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3.0 COMMENTS AND RECOMMENDATIONS
3.1 INTRODUCTION
Observations made during the audit are recorded on the checklists
contained in the Appendix. These checklists were used during the audit to
document the procedures used by Radian and to help identify any problem
areas. RTI's observations and recommendations are discussed further in the
sections below. Additionally, RTI's recommendations are summarized in
Table 2 of Chapter 1.0.
3.2 PROCESS OPERATION
On the day the audit took place the sampling was interrupted several
times because the incinerator was shut down. Since the shutdowns were
unannounced and unexpected, the test team was unable to simultaneously
cease their sampling activities. Consequently, the trains sampled a gas
stream that may have been somewhat nonrepresentative of normal operation.
Although the shutdowns were largely due to equipment malfunction (I.e., a
broken fuel oil line and turbine blade), it appeared that a lack of diligence
on the part of the incinerator operator was also a factor. One operator in
particular was less diligent and less cooperative with the test team than
other operators encountered during the testing.
Another process variable that presented a problem to the test team was
the stack exhaust fan, which cut on and off according to steam demand. The
fan presented a challenge to the sample train operators in maintaining
isokinetic sampling rates.
A third process variable of concern to the test team was the ambient
air intake damper, located about 30 feet from the top of the stack. The
damper position, which did not vary substantially during the test run,
resulted in dilution of the stack gases by roughly 50 percent. The effect
of the dilution was to double (from 80 to 160 minutes) the sampling time
required to detect a minimum of 1.0 ppt dioxin in the stack gases.2 (Since
13
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the total sampling time exceeded 160 minutes, the dilution of stack gases
did not present a problem in achieving the 1.0 ppt minimum detection limit
goal.) Additionally, there is some risk that the gases sucked into the
stack gas stream though the intake damper may have contaminated the gas i
stream with dioxins or other chlorinated organic compounds. However, this
seems unlikely because no other organics emission sources were believed to
be in the vicinity of the intake damper. (Any contaminants would be
detected by the ambient MM5 sampling train, which was located close to the
intake damper.)
A final troublesome process variable was the frequency at which ash
was pushed from the incinerator bottom into disposal carts. Since this
frequency varied with the operator, the test team had difficulty determining
how many pushes represented normal operation.
The net effect of the problems noted above was to shorten the sampling
period to less than the 4-hour goal and to raise questions concerning the
representativeness of samples obtained.
As a result of these problems and their potential adverse effects on
sample representativeness and data quality, Radian decided to extend the ;
test program at this industrial site from three to four tests. The fourth
test was intended to provide an extra set of data in the event that the
data set produced by test No. 2 (i.e., the test audited by RTI) is judged
in the future to be unacceptable or of poor quality. Fortunately, the (
problems which occurred during the RTI audit were reported to be much less
significant during the other three tests at this site. ;
The Radian test team handled the problems discussed above in a respon-
sible manner. Furthermore, Radian was very conscientious about taking feed
material weights-and recording all pertinent process operating parameters.
3.3 MODIFIED METHOD 5 SAMPLING TRAIN
The MM5 sampling train appeared to be set up and operated according to
the ASME MM5 sampling methodology specified in Radian's Test Plan, with one
exception: the position of the XAD trap condenser. Radian mounted the
condenser in a horizontal position, although the ASME method specifies that
the condenser shall be oriented vertically. The mounting of the condenser
in a horizontal position is not a problem provided that all condensed !
14
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liquids are carried forward into the resin by the gas stream. Although
this appeared to be the case during the audit, there is no guarantee that
this will always be the case during future tests. Furthermore, test results
carry more credibility when the test procedure is strictly adhered to.
Otherwise, all MM5 procedures specified in the Test Plan appeared to be
implemented correctly.
It is'recommended that Radian mount the MM5 XAD-condenser in a vertical
position during future tests. Alternatively, Radian should explain in each
test report: (1) why the condenser mounting position differs from the test
protocol; and (2) what effect this is likely to have on the outcome of that
particular series of tests (e.g., was all moisture observed to be carried
forward into the resin).
3.4 BLANK MM5 SAMPLING TRAIN
The blank MM5 sampling train was located at the base of the sample
train scaffolding and consisted of most of the essential elements of a
standard MM5 train (i.e., the probe filter box, XAD cartridge, and 1m-
pingers). The probe inlet and the final impinger outlet were capped with
hexane-rinsed aluminum foil. The main discrepancy between Radian's pro-
cedure and the test protocol involved the period of time during which the
train ends were capped. The test protocol implies that the train ends are
to remain capped throughout the test; however, Radian was observed to
remove the caps during part of the test.
An additional discrepancy between Radian's procedure and the test pro-
tocol involves the type of cap used to seal the last impinger. The test
protocol specifies that a ground glass cap shall be used, whereas Radian
was observed to use hexane-rinsed aluminum foil. (Radian may have intended
to remove the caps during periods coinciding with the movement of the stack
MM5 train from one point or one port to another point or port. Nevertheless,
the procedure specified in the test protocol appears to be more appropriate.)
It is recommended that Radian allow the front and back ends of the
blank MM5 train to remain sealed throughout future tests. The probe should
be sealed with hexane-rinsed aluminum foil and the last impinger with a
ground glass cap.
15
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3.5 AMBIENT MM5 SAMPLING TRAIN
The ambient MM5 sampling train was located on the roof of the plant
beside the sampling train scaffolding. The train was set up according to
the description presented in Radian's test plan. Since three runs were to:
be composited into a single sample, the train was not disassembled between
runs.
On the day of the audit, the XAD resin organic trap was not continuously
cooled between runs. Since the trap was located out-of-doors and was
subject to relatively cool ambient temperatures, continuous cooling of the
resin was probably not crucial. Nevertheless, the adsorption of organic
gases into XAD is somewhat sensitive to temperature, and continuous cooling
between runs should be incorporated into future tests where possible.
(EPA's Level 2 guidelines note that a 10 °C change in the sorbent module
temperature will result in a factor-of-two change in the volumetric capacity
of the resin for a particular compound.7)
• The ambient train was located beside the stack near the ambient air
intake damper. Although the train would ordinarily be located near the
combustion air intake, the ambient air intake damper site was approved by
EPA prior to the test. This site allowed the test team to determine whether
any chlorinated organic compounds measured in the stack by the MM5 sampling
train were contributed by gases sucked in through the ambient air damper. ;
It is recommended that the ambient XAD resin trap be cooled on a
continuous basis between runs (as well as during runs) whenever the train
is located in a hot or variable-temperature environment.
3.6 HC1 SAMPLING TRAIN
The HC1 train was operated in an acceptable manner, except that a
break was discovered in the probe at the end of the test. Often these
types of problems occur no matter how much care is exercised, although just
as often the problem can be avoided through more careful handling of equip-
ment.
It is recommended that Radian take precautions as necessary to avoid
any future breakage of equipment, as occurred with the HC1 sampling probe
on the day of the audit. ;
16
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,3.7 CONTINUOUS EMISSION MONITORS
The continuous emission monitoring system consisted of a coarse fil-
ter, sampling probe, heated sampling line, moisture removal system, moni-
toring units, strip charts, and an automated data acquisition system.
(Gases sent to the hydrocarbon monitor bypass.ed the moisture removal sys-
tem.) A separate bag sample was periodically taken at a point above the
ambient air intake damper to determine the extent of dilution at the damper.
Strip charts were carefully marked and all calibration data were recorded.
Three-point calibrations were performed at the beginning of the test pro-
gram, and two-point calibrations were performed at the beginning and end of
each test run. Calibration and quality control gases were introduced at
the end of the sample line near the moisture removal system. Thus, the
entire sampling interface was not tested by these gases. (Radian indicated
that the entire interface would be tested during future tests.)
Separate gas cylinders were used for calibration and quality control.
The quality control gases were used before each run, immediately following
the span check. The monitor meter should be allowed to return to zero
before the monitor is challenged with the quality control gas; however,
this was not done. (By allowing the monitor to return to zero, the quality
control check becomes truly independent of the span check.) The quality
control gases were calibrated by the vendor against NBS standards, and none
of the cylinders were allowed to fall below 200 Ib pressure. The cylinders
are returned to the vendor for reverification at the end of each test
series.
Data were collected by the data acquisition system at 5-minute inter-
vals, and corrections for drift were made at the end of the test run. This
procedure worked nicely, except that the data acquisition system did not
incorporate a time constant to average out noise peaks in the monitor
signal. (However, since readings were taken so frequently, positive peaks
were probably balanced by negative peaks such that the net effect was
little or no bias.) Monitor drift was not bad, except for the NO monitor
during significant temperature variations inside the continuous monitor
trailer. (Radian indicated that this problem would be solved once their
new trailer is outfitted and put in service.) Finally, strip charts were
offset 5 percent rather than the recommended 10 percent.8
17
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We have the following recommendations for the continuous emission
monitoring system: (1) calibration and quality control gases for the
continuous emission monitors should test the entire sampling interface; (2)
continuous monitor meter readings should be allowed to return to zero
before challenging the"meter with a quality control gas; (3) if possible,
the continuous monitor data acquisition system should incorporate a time \
constant to average out peaks in the monitor signal; (4) temperature vari-
ations within the continuous monitor trailer should be minimized; and (5)
continuous monitor strip charts should be offset 10 percent.
3.8 PROCESS SAMPLES
The process sample collection activities involved the collection of '
representative samples of waste feed, No. 2 fuel oil, and incinerator
bottom ash. The waste feed samples consisted of paint sludge, wood and
plastic cutoffs, crate parts, paper, and cardboard. Representative samples
of waste feed were very difficult to obtain due to the bulkiness of some
materials and the thick consistency of the paint sludge. The test team i
worked hard to homogenize the waste sludges; however, their attempts were
largely unsuccessful.
3.9 SAMPLE HANDLING, TRANSPORTATION, AND STORAGE
Radian reported that during earlier dioxin testing, several"bottles
broke during shipment. This problem is now avoided by sealing the bottles
inside two insulated plastic bags separated by packing material. Under
these conditions future breakage seems unlikely.
While the Radian test was in progress it was observed that the liquid
level was not marked on the sample collection bottles. Instead, bottle
weights were recorded before and after the bottles were filled. Radian's
procedure is certainly more accurate than the procedure of marking liquid
levels directly on the bottle. However, their procedure has a problem
in that there is no quick and convenient way to determine whether any
liquid loss has occurred. (According to Radian, the bottle weights are not
checked back at the laboratory unless the physical appearance of the bottle
indicates that some leakage may have occurred.)
It is recommended that Radian mark the liquid level on all sample
collection bottles.
18
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3.10 SOIL SAMPLING :
The soil sampling activities appeared generally to follow the procedures
specified in the Jest Plan. (More details concerning these procedures'are
presented in the appendix to this report.) However, there are three aspects
of these activities that could be improved. First, site selection was a
problem at this test site due to the small amount of open land available in
the vicinity of the incinerator. The site selected was probably the most
logical one under the circumstances. However, if one objective of the
sampling of soils is to search for dioxins deposited by stack emissions,
the location selected may have been too close to the stack to permit effec-
tive downwash to occur.
Another concern about the soil sampling program is the proximity of
the soil samples to one another. Ideally, the samples should cover a wide
area of the grounds surrounding the plant. However, at the incinerator
test site the 10 samples were taken within a rectangle of approximately 3
by 9 feet. (This area was selected because of the scarcity of suitable
land for sampling near the plant.) The consequence of taking closely
spaced samples is to provide data that represent only a very small segment
of the land surrounding the plant.
An additional concern is the manner in which the soil samples were
composited. During the audit there seemed to be some confusion about
whether the compositing should be performed by hand or by using a tool such
as a garden trowel. Use of a hexane-rinsed garden trowel is preferable.
A final comment concerns the cleaning of surface debris (e.g., leaves
and dead grass) from the soil sampling area before sample collection is
performed. Radian did not implement this procedure, although little signif-
icant debris was present. ,
RTI has the following soil sampling recommendations: (1) in the
future Radian should conduct soil sampling over a wide area where potential
dioxin contamination is most likely; (2) soil samples should be composited
using an appropriate tool, such as a hexane-rinsed garden trowel; and
(3) all debris (e.g., leaves and dead grass) should be cleaned from the
ground before soil sampling is begun.
19
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4.0 CONCLUSIONS
Overall, RTI was impressed with the Radian test team and the quality
of their work. Although on the day of the audit testing was interrupted
several times due to process disruptions, these problems were beyond the
control of the test team. RTI is satisfied that the data generated by the
test program will be of sufficient quality to achieve the objectives of the
study, provided that: (1) the analytical procedures, which will be evaluated
under a separate audit, are performed correctly; and (2) the sampling
procedures continue to be performed .with the same level of care exhibited
during the Site ISW-A incinerator tests. However, the quality of data could
be further improved if the recommendations contained in this report are
implemented. These recommendations are summarized in Table 2.
20
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5.0 REFERENCES
1.
2.
3.
4.
5.
6.
7.
8.
M. A Palazzolo, Radian Corporation. "Site Specific Test Plan, Indus-
trial Solid Waste, Test Number Two, Site ISW-A, National Dioxin Study
Tier 4: Combustion Sources." DCN No. 84-231-056-12-05. Research
Triangle Park, North Carolina. November 1, 1984.
M. A. Palazzolo, R. F. Jongleux, and L. E. Keller. "National Dioxin
Study Tier 4, Combustion Sources, Quality Assurance Project Plan "
DCN No. 84-231-056-12-03. Research Triangle Park, North Carolina
September 21, 1984.
Radian Corporation. "Draft Report, National Dioxin Study Tier 4
Combustion Sources, Sampling Procedures." DCN No. 84-240-016-51-09
Research Triangle Park, North Carolina. October 17, 1984.
U.S. Environmental Protection Agency. "Interim Guidelines and Spe-
cifications for Preparing Quality Assurance Project Plans " OAMS-
005/80. December 29, 1980.
Richard V. Crume, Research Triangle Institute. Letter to Mr Bill
Kuykendal, Office of Air Quality Planning and Standards, U.S. Environ-
mental Protection Agency. October 23, 1984.
Richard V. Crume, Research Triangle Institute. Letter to Mr Bill
Kuykendal, Office of Air Quality Planning and Standards, U.S. Environ-
mental Protection Agency. November 8, 1984.
U.S. Environmental Protection Agency. "EPA/IERL-RTP Procedures for
Level 2 Sampling and Analysis of Organic Materials." EPA-600/7-79-
033. February 1979.
U.S. Environmental Protection Agency.
Pollution Source Monitoring Systems."
"Handbook: Continuous Air
EPA-625/6-79-005. June 1979.
21
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6.0 APPENDIX
6.1 AUDIT CHECKLISTS
Detailed information concerning the Site ISW-A industrial incinerator
audit is presented in the following audit checklists.
22
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