EPA-600/2-76-047
March 1976
Environmental Protection Technology Series
MOLECULAR SIEVE TESTS FOR CONTROL OF
SULFURIC ACID PLANT EMISSIONS
Industrial Environmental Research Laboratory
Office of Research and Development
U.S. Environmental Protection Agency
Research Triangle Park, North Carolina 27711
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RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into five series. These five broad
categories were established to facilitate further development and application of
environmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The five series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
This report has been assigned to the ENVIRONMENTAL PROTECTION
TECHNOLOGY series. This series describes research performed to develop and
demonstrate instrumentation, equipment, and methodology to repair or prevent
environmental degradation from point and non-point sources of pollution. This
work provides the new or improved technology required for the control and
treatment of pollution sources to meet environmental quality standards.
EPA REVIEW NOTICE
This report has been reviewed by the U.S. Environmental
Protection Agency, and approved for publication. Approval
does not signify that the contents necessarily reflect the
views and policy of the Agency, nor does mention of trade
names or commercial products constitute endorsement or
recommendation for use.
This document is available to the public through the National Technical Informa-
tion Service. Springfield, Virginia 22161.
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EPA-600/2-76-047
March 1976
MOLECULAR SIEVE TESTS FOR
*»
CONTROL OF SULFURIC ACID PLANT EMISSIONS
by
Karl R. Boldt and Richard F. Timmons
York Research Corporation
One Research Drive
Stamford, Connecticut 06906
Contract No. 68-02-1401, Task 2
ROAP No. 21ADH-006
Program Element No. 1AB014
EPA Project Officer: E. J. Wooldridge
Industrial Environmental Research Laboratory
Office of Energy, Minerals, and Industry
Research Triangle Park, NC 27711
Prepared for
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Washington, DC 20460
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PAGE i
ABSTRACT
A molecular sieve control system for sulfur dioxide from sulfuric
acid plant tail gas was tested by York Research Corporation.
The system, the PuraSiv S, was developed by Union Carbide Corpora-
tion, Linde Division, and is currently operating at the Coulton
Chemical Corporation in Oregon, Ohio. The PuraSiv S utilizes
a molecular sieve adsorbent material which releases SC>2 upon
the application of heat. The S02 is then recycled for an additional
2 to 3 percent production of acid.
This report is an evaluation of the PuraSiv S based upon data
gathered during a 4-week test program. Sulfur dioxide concentra-
tions were continuously measured and recorded by a DuPont 460/1
photometric gas analyzer at both the inlet and outlet gas streams.
Average removal efficiency was 98.0 percent. Average SO2
emissions from adsorbers during testing was less than 100 ppm.
This report was submitted in fulfillment of contract number
68-02-1401, Task Number 2 by York Research Corporation under
the sponsorship of the Environmental Protection Agency. Work
was completed as of March 4, 1975.
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PAGE 11
TABLE OF CONTENTS
ABSTRACT
LIST OF FIGURES
LIST OF GRAPHS
LIST OF TABLES
LIST OF APPENDICES
LIST OF APPENDIX FIGURES
ACKNOWLEDGMENT
I. INTRODUCTION
II. SUMMARY
III. PROCESS DESCRIPTION AND OPERATION
IV. SAMPLING AND ANALYTICAL PROCEDURES
A. Location of Sampling Ports
B. Sampling Procedures
C. Analytical Procedures
V. DISCUSSION OF TEST RESULTS
APPENDICES
Page
i
iii
iv
v
vi
vii
viii
1
2
4
10
11
11
15
17
45
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PAGE .i:Li
LIST OF FIGURES
FIGURE PAGE
1 Flow Diagram Showing B-Plant, Coulton 5
Chemical Corporation
2 Flow Diagram of PuraSiv S (showing Al 8
Absorbing and A2 regenerating)
3 Location of Inlet Sample Point and Detail 12
of Probe .(not to scale)
4 Location of Outlet Sample Point 13
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PAGE iv
LIST OF GRAPHS
GRAPH PAGE
1 Typical Cycle During Normal Operation - 26
Adsorber Al
2 Typical Cycle During Normal Operation - 27
Adsorber A2
3 Adsorber Efficiency Versus Time for Typical 28
Cycle During Normal Operation
4 Process Upset - High Converter Exit 29
Temperature
5 Process Upset - Malfunction of Condenser 30
Controller Causing Erratic Converter
Temperature
6 Process Upset - "Slug" of Sulfur Dumped 31
into Burner
7 Plant Shutdown with PuraSiv Off-Line 32
8 Plant Shutdown with PuraSiv On-Line 33
9 Plant Startup 34
10 Plant Startup 35
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PAGE v
LIST OF TABLES
TABLE PAGE
1 S02 Test Summary 19
2 List of S02 Test Cycles 20
3 DuPont S02 Accuracy Calculations 36
4 Sulfuric Acid Mist Emission Results 37
5 Total Acid Emission Results 38
6 Chloride Emission Results 39
7 Sulfide Emission Results 40
8 Hydrocarbon Emission Results 41
9 Oxides of Nitrogen Emission Results 42
10 Moisture Results 43
11 Orsat Readings 44
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PAGE vi
LIST OF APPENDICES
PAGE
APPENDIX A Installation and Operation of Continuous 45
Monitoring System
APPENDIX B Calculation of S02 Mass Emission Rate 47
APPENDIX C Wet Chemical Test Methods 49
APPENDIX D Example Calculations for Wet Tests gg
APPENDIX E S02 Data Summary (English Units) 61
APPENDIX F S02 Data Summary (Metric Units) 67
APPENDIX G Strip Chart 73
APPENDIX H Raw Data Sheets - Wet Tests 201
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PAGE vii
LIST OF APPENDIX FIGURES
FIGURE PAGE
Al S02 Sampling Train 50
A2 Diagram of a Heated Midget Sample Train 52
and Probe
A3 Sampling Train 54
A4 Hydrocarbon Sampling 56
, A5 NOX Sampling Train 57
A6 Flue Gas Collection by Leveling Bottle 59
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PAGE viii
ACKNOWLEDGMENT
York Research would like to express its appreciation to the
staff of Coulton Chemical Corporation for the courtesy extended
during the performance of this test series. Particular thanks
are extended to Messrs. Dave Lovell, Leonard Stonestreet and
Connelly Neal for the technical knowledge and assistance both
in the preparation of test sites and during the actual testing.
We would also like to thank Messrs. Lou Fornoff of Union Carbide
and Ed Wooldridge of the Environmental Protection Agency for
their invaluable assistance throughout the project.
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PAGE 1
I. INTRODUCTION
York Research Corporation, under contract to the Environmental
Protection Agency/ Office of Research and Development, Industrial
Environmental Research Laboratory, tested a sulfur dioxide
control system designed and manufactured by the Union Carbide
Corporation, Linde Division, and installed at the Coulton Chemical
Corporation in Oregon, Ohio. Designated the PuraSiv S* process,
the unit utilizes a molecular sieve adsorbent material which
has an affinity for polar compounds. It is being used to remove
sulfur dioxide from the tail gas stream of a contact sulfuric
acid plant.
The PursaSiv S utilizes two adsorbing beds, one of which is
"on-line" and one of which is being "regenerated" at any particular
time. Normal cycle time is 4 hours; however, the cycle time
can be increased or decreased from the norm as conditions dictate.
The system has been operating at Coulton Chemical Corporation's
B-Plant since February 4, 1973, although the adsorbing beds
were replaced in November of that year. A second-generation,
more durable sieve material was installed at that time. Actual
usage of the new beds was about 11 months, since the plant ex-
perienced several shutdowns.
The B-Plant was rated at 200 tons of sulfuric acid per day;
however, operational problems had reduced the production rate
to 160 tons per day. The plant operators successfully increased
the S02 loading to the PuraSiv S in excess of maximum design
loading for the test.
The specific task assignment entailed the continuous measurement
of sulfur dioxide in order to perform a technical evaluation
of the tail gas control system. Sampling sites were at the
outlet of the adsorption bed prior to the inlet to the stack
and at the inlet of the adsorbers following the Brink demister.
A total of 118 cycles, 59 for each adsorber, were monitored
between February 4, 1975 and March 4, 1975. Instrumentation
used was a DuPont 460/1 photometric gas analyzer with a two-
point sampling system and dual range capability. In order to
determine baseline tail gas component concentrations, wet tests
were performed for the following: sulfuric acid mist, total
acid, nitrogen oxides, hydrocarbons, chloride, sulfides, carbon
dioxide, oxygen, and moisture.
*Union Carbide trade name.
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PAGE 2
II. SUMMARY
Sulfur dioxide concentrations were measured at the outlet and
inlet of the PuraSiv S unit at the Coulton Chemical Corporation
in Oregon, Ohio. The plant is a typical contact sulfuric acid
plant with a rated capacity of 200 tons per day. The PuraSiv
S has a maximum design loading of 2800 ppm S02 at 10,500 SCFM.
The objectives of the test program were (a) to establish S02
emission levels at maximum design loadings, (b) to document
S02 emission levels when a process upset caused inlet concentra-
tions to go out of control, and (c) to determine the effect
of tail gas impurities on the performance of the sieve. Objectives
(a) and (b) were successfully obtained and can be found in detail
in Section V of this report. Objective (c) was not obtained
since the test program was far too short to complete a definitive
study on tail gas impurities. However, baseline determinations
of the following tail gas components were obtained and can be
found in Section V: sulfuric acid mist, total acid, nitrogen
oxides, hydrocarbons, chloride, sulfides, carbon dioxide, oxygen,
and moisture.
Due to an operational difficulty with the plant during the test
period, production rate was down to 160 tons per day with an
accompanying drop in tail gas flow rate to 7500 SCFM. The plant
operators, however, were able to increase the S02 loading
to the PuraSiv S without endangering the equilibrium balance
of the plant. This was accomplished by routing the recycled
SO2 directly to the combustion air inlet from the regenerating
adsorber and bypassing the primary stripper.
The PuraSiv S unit is comprised of two adsorbing vessels which
alternate functions at 4- or 5-hour intervals - i.e., at any
particular time one vessel is adsorbing and the other is regenera-
ting. During regeneration the desorbed S02 is piped to the
combustion air inlet and recycled through the plant for an addi-
tional 2 to 3 percent production of sulfuric acid. The major
portion (75 percent) of the stream leaving the adsorber is ex-
hausted through the main tail gas stack, while a slipstream
is taken from the outlet duct and used to regenerate the air
dryer beds.
The S02 concentrations were measured at the adsorber inlet and
in the outlet duct just prior to entering the main stack. Sulfur
dioxide concentrations were printed on a strip chart, permitting
instantaneous results and documentation of trends and patterns.
Inlet values averaged from 2335 to 4800 ppm over individual
cycles of operation. When inlet concentration is plotted versus
time for a single cycle, the curve is characterized by a constant
value during the first hour. The next 1% hours give a rise
of 500 ppm above the concentration seen during the first hour,
followed by a drop to 100 ppm below the concentration seen the
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PAGE 3
first hour. The last hour is characterized by a return to the
same value experienced during the first hour. The rise is caused
by a "slug" of desorbed 862 from the regenerating adsorber which
has been recycled through the plant. Since the desorption is
followed by a flush of clean air through the bed, the slug of
SC>2 is followed by a slug of clean air, accounting for a dilution
of tail gas that shows up as a drop in inlet S02 concentration.
The pattern of outlet concentrations over a single cycle typically
started at 15 to 50 ppm during the first hour, rising to 80
to 100 ppm during the second hour and continuing to a maximum
of 120 to 180 ppm at the end of the cycle. Several process
upsets were documented and two shutdowns were experienced; however,
at no time was "breakthrough" noted. (Breakthrough is the point
at which emissions increase sharply due to bed saturation.)
The emissions exceeded the EPA limit of 4 pounds S02 per ton
of acid (300 ppm) only during startup. The average emissions
from A2 were 0.804 pounds SO? per ton of acid as measured over
the entire range of test conditions.
Sixty percent of the test period saw loadings to the PuraSiv
S in the range of 75 percent of maximum. Emissions, when averaged
over separate cycles, were 62 ppm for adsorber A2 and 73 ppm
for adsorber Al. At 100 percent of maximum design loading,
which was experienced over 35 percent of the test period, emissions
averaged 82 ppm for adsorber A2 and 111 ppm for adsorber Al.
Five percent of the test period saw loadings of 100 percent
of maximum design. Emissions during these cycles averaged 99
ppm for adsorber A2 and 107 ppm for adsorber Al. A short
time before the test program, a problem with adsorber Al was
discovered. The bed support had broken and an unknown quantity
of molecular sieve had been lost. The problem had not yet been
corrected at the time of testing and, therefore, slightly
lower efficiency was experienced from that unit.
The emissions from adsorber A2 were below 100 ppm, as emissions
were averaged over several cycles. When averaged over individual
cycles, however, emissions were as high as 118 ppm. Union Carbide
has claimed that the emissions from the PuraSiv S average less
than 100 ppm* per cycle, and this level was exceeded in 13 percent
of the total number of cycles measured.
Average efficiency of S02 removal by adsorber A2 was 98.05 percent
for S02 loadings up to 100 percent of design, while efficiency
was 97.9 percent for loadings up to 110 percent of design.
*Union Carbide Corporation, "PuraSiv S Systems for Sulfuric
Acid Plants - Technical Pact Sheet."
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PAGE 4
III. PROCESS DESCRIPTION AND OPERATION
The PuraSiv S system has been in operation at the B-Plant of
Coulton Chemical Corporation since February 4, 1973. In November
of that year the molecular sieve adsorbent material in the beds
was replaced with a more durable second-generation sieve packing.
The new adsorbent was claimed to have a useful life in excess
of 3 years. At the onset of testing, the age of the new sieve
was 15 months, although the actual usage had been approximately
11 months.
The B-Plant was designed to produce 200 tons per day of concen-
trated sulfuric acid. However, problems had been experienced
with an electrical transformer on the electrostatic precipitator.
This problem forced the use of a smaller standby transformer,
which restricted the daily production to 160 tons.
The plant is a single adsorption contact plant, where combustion
of sulfur-bearing feed produces a gas stream high in S02, which
is then exposed to several sequential processes before the final
product of sulfuric acid is realized. The feed is composed
of molten sulfur, H2S off-gas, and spent sulfuric acid waste
from a nearby petroleum refinery. The tail gas from the adsorp-
tion process is the major source of emissions at the plant.
Other emission sources include fuel combustion units for air
heating. The tail gas flow rate fluctuates with production
rate and ranges up to 10,500 SCFM, with an average S02 concentra-
tion ranging between 2500 and 5000 ppm. At design loading to
the PuraSiv S, 1300 +100 pounds of S02 are adsorbed over a
4-hour period.
Although the plant was operating at reduced capacity, a condition
was induced during the test period whereby the weight of S02
adsorbed on the PuraSiv S beds equalled or exceeded the design
loading. The regeneration gas returning to the plant was piped
directly to the combustion air inlet, bypassing the S02 stripper,
and increasing the S02 concentration in the gas stream through
the plant. Combined with the lengthening of the adsorption
cycle beyond 4 hours, the resulting effect was to increase the
loading to as much as 1560 pounds of S02 absorbed per cycle.
Figure 1 is a schematic diagram which shows the basic flow pattern
of the B-Plant. Two combustion chambers are utilized for the
production of S02; one of which is fed molten sulfur, and the
other hydrogen sulfide and alkylation spent acid supplied by
the petroleum refinery. The combustion takes place at a high
enough temperature to dissociate the spent acid and hydrogen
sulfide into S02 and water vapor. The gas stream is humidified
prior to the removal of dust and S03/acid mist in a lead-lined
electrostatic precipitator. During normal equilibrium conditions
virtually no S03/acid mist is formed at this wtaqc- of the
However, during startup and shutdown procedures, and any other
process imbalance which results in temperature fluctuations,
-------
Spent
Acid
H2S
Weak
Acid
Air
Molten
Sulfur
tion
$
i
MMMMM
1
Furnace
y
[
^
i
Humidi-
fying
Tower
1
Strong
Acid
Mist
Preci-
pitator
Drying
Tower
Impure
Acid
Sulfur Burner
Blower
S02 = 9.5%
Weak
Acid
Process Gas Stream
800°F 860°F 990°F
L
1060°F
Jl
Jl
810°F
810°FJ 850°Fl 1
150°F
90°F
Tail Gas
to Pura
Siv
Brink
Demister
Absorbinc
Tower
480°F
Strong
Acid
o
Acid Flow
Gas Flow
FIGURE 1
Flow Diagram Showing B-Plant, Coulton
Chemical Corporation
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PAGE 6
SO 3 and acid mist may form in considerable quantities.
The next stage of the process involves the removal of water
vapor from the stream in order to prevent acid formation in
the piping. This is accomplished by exposing the stream to
circulating concentrated sulfuric acid in a drying tower. The
temperature of the stream is then reduced to approximately 825°
F in a heat-exchange system prior to entering the first stage
of the four-stage converter. At this point in the system the
gas stream contains 9 to 10 percent S02 with smaller amounts
of C02 and 62; the balance being nitrogen. The S02 oxidation
reaction is exothermic; thus, the temperature of the gas stream
rises appreciably when passing through the converter. Heat
exchangers are utilized between stages to cool the gas stream
back to approximately 825°F before it enters the next stage
of the converter. The practical upper limit of conversion for
single absorption plants is about 98 percent. This appears
to be the level at which the S02 is in an equilibrium state
with S03 and although oxygen is available for the reaction,
further oxidation will not take place unless partial removal
of 303 takes place. The remaining S03 passes through the system
unchanged.
The process stream leaves the conversion area at about 800°F
but is cooled to 480°F prior to absorption. The absorption
tower is similar in construction and operation to the drying
tower. The gas is exposed to a circulating stream of 98 to
99 percent sulfuric acid, where the sulfur trioxide combines'
with the water in the acid and increases the strength to between
99.1 and 99.3 percent. Virtually 100 percent of the S02 is
absorbed while the unconverted 503 (0.2 to 0.5 percent) passes
through unabsorbed. A Brink demister is utilized at the tail
end of the base plant to remove any acid mist carry-over from
the absorber. Temperature at this point is about 90°F.
The tail gas stream is piped via a 24-inch diameter steel duct
to the PuraSiv S unit where it is routed to one of two adsorbing
vessels. The system is flexible in that cycle time can be in-
creased or decreased from the 4-hour standard, depending on
the S02 load from the plant. During any particular cycle, one
vessel is adsorbing and one vessel is being regenerated, thus
returning the desorbed SO2 to the combustion air inlet.
The first hour of regeneration is spent flushing the bed with
hot, dry air in order to bring the bed up to an optimum tempera-
ture. The bulk of SO2 desorption takes place during the second
hour after the bed has reached the desired temperature. The
increase of SO2 in the process gas stream during the second
hour of regeneration is demonstrated by a 500 ppm increase in
the S02 concentration in the tail gas and by a boost of acid
strength in the absorber amounting to 0.002 percent. The last
2 hours of the regeneration cycle consist of bringing the bed
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PAGE 7
back to operating temperature by purging it with dry, ambient
air.
The adsorbent in the PuraSiv S has a strong affinity for polar
compounds, and since water is highly polar, water vapor will
actually displace S02 from the bed. This causes no problem
with plant tail gas as moisture is removed from the stream
prior to conversion. The concentration of moisture in the PuraSiv
S inlet stream was only 20 ppm.
Since ambient air is used for regeneration, it is imperative
to remove moisture from the regeneration air, and this is accom-
plished with the use of two similar (although smaller) adsorp-
tion beds. These air dryers normally operate on 4-hour cycles.
Adsorber regeneration air is drawn by fan F-l through one air
dryer at a constant 4625 SCFM and heated prior to introducing
it into the regenerating adsorbers. The heater exhaust gases
do not mix with the regeneration air. At the end of the initial
2 hours of the cycle, the heater cuts off and fan F-l continues
to flush the bed with dry air. Simultaneously, the alternate
dryer is being regenerated with a slipstream of treated tail
gas. Fan F-2 pulls this slipstream at a constant 2000 SCFM.
Two hours of heating and 2 hours of cooling are required for
regeneration of the air dryers. This process of adsorption/
regeneration is illustrated schematically in Figure 2, which
shows adsorber Al adsorbing and adsorber A2 regenerating while
air dryer A4 is drying and A3 is regenerating.
It is obvious from Figure 2 that there are two S02 emission
points from the PuraSiv S: the main tail gas stack and the
air dryer stack. The concentration of S02 in the main stack
is equal to the S02 concentration of the gas entering the air
dryer. Some SO2 may adsorb on the air dryer bed during the
last 2 hours of regeneration; however, this S02 will desorb
upon the application of heat during the following regeneration
cycle. Therefore, the weight rate of S02 leaving the adsorber
will equal the weight rate of SO2 emitted to the atmosphere
from both stacks when averaged over an 8-hour period. For cal-
culating the outlet S02 weight rate, the PuraSiv S was treated
as a single emission source, using S02 concentration at the
base of the stack and flow rate at the inlet to the adsorber.
An attempt was made to measure the inlet flow rate by traversing
the duct with an S-type pitot tube, but the attempt had to be
aborted before completion due to hazardous working conditions.
The high S02 concentration and high internal duct pressure
(2 inches of mercury) made it impossible to work without a sealed
test port. A standard-type, fixed-point pitot tube had been
installed at the inlet site for a previous test. Since the
duct was sufficiently large in diameter for the unmeasured areas
to have a significant effect upon the calculation of flow rate,
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Plant Tail Gas Inlet^Sanr
Q=7500SCF" L
-t*
Regeneration Gas
to Base Pla
Q=4625
SCFM
Bypass to Stack (Closed)
Heater
Absorber
Al
Absorber
A2
Outlet
Sample
Main Tail
Gas Stack
Q=5500 SCFM
i\
Q=2000SCfM
1
FIGURE 2 Flow Diagram of PuraSiv S
(Showing Al Absorbing and A2 Regenerating)
2
o
00
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PAGE 9
the pitot reading was used only to monitor fluctuations. Flow
rate was measured periodically by Coulton personnel. A
determination was made by traversing the blower inlet and
calculating a sulfur balance on the entire plant. During the test
period, flow rate ranged from 7440 to 7670 SCFM, while the acid
production rate, measured simultaneously with flow rate, remained
constant at 160 tons per day.
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PAGE 10
IV. SAMPLING AND ANALYTICAL PROCEDURES
At the initial coordination meeting between the representatives
of Coulton Chemical, Union Carbide, the Environmental Protection
Agency, and York Research Corporation, York Research proposed
to perform a continuous monitoring study of the PuraSiv S process.
The Environmental Protection Agency agreed to sponsor the study,
provided that wet tests were performed using an acceptable method
to verify the results of the gas analyzer. Following a long
preparation period, during which several types of analyzers
were discussed, the decision was made to use a DuPont 460/1
photometric gas analyzer equipped with a two-point sampling
system. This instrument has a precision of 2 percent.*
Teflon sample lines with a %-inch outside diameter were connected
to the inlet and outlet of the absorber. A compressed air line
was also connected to the instrument from the plant compressor
station. The DuPont 460/1 utilizes a switching system powered
by pneumatic valves and an air-powered arrangement is used to
move the sample. The dual sample-point arrangement consists
of twin aspirators and switching capability to operate the in-
strument in any one of four sampling modes. The first mode
is a flush of instrument air through the sampling interface,
through the sample handling system, and through one of the sample
lines to the probe. During this flush of clean air, the instru-
ment automatically sets the readout at zero. The second mode
is a sample mode, during which some stack gas is extracted and
concentration is measured at the sampling interface. The next
step is a flush of clean air through the sampling system and
back down the second sample line. Following this is a sample
extraction and measurement from the second sampling location.
Each step is automatically and sequentially controlled by a
control station that can be programmed. In addition, a manual
override is included so that any particular sample mode can
be eliminated or held for an indefinite period of time. Normal
cycle times are 30 seconds for each flush sequence and 90 seconds
for each sample sequence.
Since the instrument had only one sampling interface, the calibra-
tion and range adjustment could not be made separately for each
sample location. A high SO 2 removal efficiency characteristic
of the PuraSiv S necessitated that a modification be made to
the instrument that would permit an independent range and calibra-
tion adjustment for each sample location. This was accomplished
by the inclusion of a separate 20 K potentiometer and solenoid
switching arrangement that was actuated automatically whenever
the sample position switched. The result was a separate calibra-
tion and range adjustment that showed no appreciable drift.
*As claimed by the manufacturer.
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PAGE 11
A. Location of Sampling Ports
The inlet sampling location was chosen by the existence of a
maintenance platform and sample port utilized by plant personnel
for taking their own samples. The inlet duct was approximately
25 feet above grade, circular (with a 24-inch diameter), and
ran horizontally from the demister outlet to the PuraSiv S inlet.
The sample port was located 30 feet downstream of the demister
outlet and 8 feet upstream of the adsorber inlet. This port
location is schematically illustrated in Figure 3. The instrument
probe consisted of a piece of stainless steel tubing fitted
through a tee, as illustrated in the lower right area of Figure
3. One leg of the tee was fitted with another length of tubing,
which was connected to a sample line running to the plant control
room. The sample probes were arranged so that the backflush
of air from the DuPont instrument would not affect the sample
taken by the control room personnel.
A special port coupling was designed so that the high S02 concen-
tration and high internal duct pressure would not pose a hazard
to the test crew when the wet tests were performed. The coupling
is shown at the lower left of Figure 3. it was designed so
that the probe could be sealed in place for testing but could
be removed for cleanup. The major component was a 4-inch gate
valve capped with a reducer down to 1-inch pipe thread. A 1-
inch Swagelok fitting was threaded into the reducer and was
used to seal the probe in place. The probe was glass heated
by nichrome windings and sheathed in stainless steel.
It was originally intended to extract the PuraSiv S outlet sample
from a port in the main tail gas stack approximately 25 feet
above grade. This location, however, was immediately above
the adsorber bypass inlet and a small amount of leakage around
the closed bypass valve caused erroneous readings. The sample
probe was then moved to an existing sample tap located in the
outlet duct between the fan F-2 take-off and the inlet to the
stack. This sample location, which was accessible at ground
level, is schematically illustrated in Figure 4. The duct was
horizontal and had a 36-inch diameter. The analyzer probe con-
sisted of a piece of stainless steel tubing fitted into a 1-inch
pipe coupling with a Swagelok reducing fitting. A 3-inch pipe
coupling welded onto the duct at 90° to the analyzer probe served
as the wet test sample port.
B. Sampling Procedures
Wet tests were performed at the inlet and outlet of the PuraSiv
S for sulfuric acid mist, sulfur dioxide, sulfur trioxide, total
acid, chloride, sulfides, oxides of nitrogen, hydrocarbons,
oxygen, and carbon dioxide. With the exception of the acid
mist tests, which were performed isokinetically using a button-
hook-type nozzle on the probe, all wet tests were performed
at a proportional sample rate with a plain probe.
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PAGE 12
From Brink
Demister
24" Inlet Duct
To Absorbers
Bypass to
Stack
Heated Glass-
Lined Probe
4" Gate Valve
4" Flange
4" to 1" Reducer
Sample Line
to Control
Room
1" Swagelok Fitting
Teflon Sample
Line to Analyzer
FIGURE 3 Location of Inlet Sample Point and Detail of Probe
Not to scale
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PAGE 13
F-2 Fan
Main
Tail Gas
Stack
Outlet Sample
Point
F-2 Fan
Take-off
Top View
Teflon Sample
Line To Analyzer
4, ^4^_ 4.
Probe- V OD SS
Tubing
Front View
Figure 4 Location of Outlet Sample Point
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PAGE 14
The acid mist tests were performed isokinetically at a single
point just before the center line of the duct, using a modifica-
tion of EPA Method 8. The single-point test was justified by
the fact that acid mist particles leaving a demister are believed
to be less than 5 microns in size,* and in this range particles
tend to be evenly dispersed throughout the duct. Velocity measure-
ments at the inlet were made with a standard-type pitot tube,
and at the outlet they were made with an S-type pitot tube.
The detailed test method can be found in Appendix C.
The mist tests were performed during the first week of the test
period. However, the purge of the train had been accomplished
without the filter in place. Since the S02 which was absorbed
by the filter was not removed during the purge, the results
were erroneously high and are not presented in this report.
The tests were repeated later in the test program.
The tests for nitrogen oxides, using EPA Method 7, were performed
during the first and last week of the test period. Total acid/
chloride tests were also performed during the first and last
week of the test period. The sample gas was bubbled through
Greenburg-Smith-type impingers containing 100 ml each of dis-
tilled water. Sample aliquots were then analyzed for total
acid and chloride. Hydrocarbon sampling was performed during
the first week, whereas the testing had to be aborted during
the last week when the heating element used to heat the grab
flasks malfunctioned. Sulfides were analyzed from the sample
catch in the iospropyl alcohol bubbler which is incorporated
into the S02 and sulfuric acid mist sample trains. These tests
were performed in the period between the first and last weeks
of testing. Oxygen and carbon dioxide samples were taken during
the first and last weeks of the test program and analysis was
performed on-site using an Orsat analyzer. Moisture content
of the inlet and outlet gas streams was determined during the
middle of the program using the instrumentation method detailed
in Appendix C.
Sample recovery and train preparation were undertaken in an
enclosed trailer parked at the plant site in close proximity
to the sampling locations. The sample recovery consisted of
probe and glassware rinses with either distilled water or isopropyl
alcohol. In the case of sulfuric acid mist tests, the filters
were removed and placed in plastic petri dishes and sealed in
plastic bags. With the exception of Orsat analysis and the
S02 samples, which were analyzed on-site, all samples were trans-
ported in sealed containers to York Research Corporation's labora-
tory in Stamford, Connecticut, for final analysis.
*U.S. Environmental Protection Agency "Compilation of Air Pollu-
tant Emission Factors," February 1972.
-------
PAGE 15
C. Analytical Procedures
Sulfur dioxide samples were analyzed on-site in a section of
the plant laboratory. The samples were stored in Nalgene 4-ounce
plastic sample bottles prior to analysis. Each sample was trans-
ferred to a 250-ml volumetric flask and diluted to that volume
with distilled water. An aliquot was taken from this flask
and placed in a 250-ml Erlenmeyer flask. The aliquot volume
of straight isopropyl alcohol was added four times and the aliquot
was then diluted to 80 ml with 80 percent isopropyl alcohol.
A few drops of thorin indicator were added and the solution
titrated to a pink end point with a standardized solution of
0.01 N barium chloride. Agitation was provided by a magnetic
stirrer. Blanks of all solutions were analyzed on-site.
The acid mist samples were collected on Fiberglas filter discs,
placed in plastic petri dishes, and sealed in plastic bags for
transportation to York Research's laboratory. The first step
in the analytical procedure was to macerate the filters indivi-
dually in an aqueous medium in order to remove all sulfuric
acid from each filter. The acid solution was then combined
with an excess of sodium carbonate to form sodium sulfate in
an alkaline medium. The solution was treated with barium chloride
in order to precipitate barium sulfate out of solution; however,
because this reaction takes place more readily in an acid medium,
a quantity of hydrochloric acid was added prior to the addition
of barium chloride. The resulting solution of sodium chloride
with a barium sulfate precipitate has a turbidity which is
proportional to the concentration of the sulfate. This turbidity
was measured with a visible spectrophotometer at 450 nm and
sulfate concentration was obtained from a standard curve.
Sulfur trioxide samples were stored in 4-ounce plastic sample
bottles and transported to York Research's laboratory for analysis
by titration with barium chloride. The samples were transferred
to a 100-ml volumetric flask and diluted to that volume with
distilled water. An aliquot was taken and transferred to a
250-ml Erlenmeyer flask prior to the addition of four times
the aliquot volume of straight isopropyl alcohol.
A few drops of thorin indicator were added and the solution
was titrated to a pink end point with a 0.01 N solution of barium
chloride.
Determinations of total acid were performed in order to demonstrate
the existence of other acids in addition to sulfuric acid.
The samples were placed in glass jars and transported to York
Research Corporation's laboratory for analysis. An aliquot
of the sample was taken and placed in a 250-ml Erlenmeyer flask.
The flask was placed on a magnetic stirrer and titrated with
a standardized solution of sodium hydroxide to a phenolphthalein
end point. The resulting volume of base necessary to neutralize
the sample was then converted to milliequivalents of total acid.
-------
PAGE 16
Chloride analysis was performed on an aliquot from the same
sample which was analyzed for total acids. A chloride selection
ion electrode combined with a Corning Model 610 research pH
meter was used to measure chloride concentration in the aliquot.
The concentration multiplied by total volume of the sample re-
sulted in chloride content of the sample.
Sulfide samples were obtained in solutions of 80 percent isopropyl
alcohol and sealed in Nalgene 4-ounce plastic sample bottles
for transportation to the Stamford laboratory. A sufficient
amount of ammonium hydroxide was added to the samples to make
the solution alkaline, after which the sulfide was combined
with lead acetate in order to form a lead/sulfide precipitate.
The amount of lead sulfide was determined colorimetrically by
matching the color of the precipitate visually to known concen-
tration standards.
Hydrocarbon samples were obtained in 500-ml glass grab flasks
and transported to the Stamford laboratory in a foam-lined wooden
packing crate. The samples were displaced from the flasks by
injection of liquid mercury, thereby causing the sample to flow
out of the flask and into a Perkin-Elmer Model 881 gas chromatograph
(GC) utilizing a flame ionization detector. The GC was stan-
dardized with a known mixture of hexane and nitrogen, and an
empty column was used so that separation of hydrocarbons did
not occur. The chromatograms were then read as total hydrocarbons.
Analysis of nitrogen oxide samples was performed in the Stamford
laboratory using a phenoldisulfonic acid method. The samples,
which contained 0.1 normal sulfuric acid and absorbed nitrogen
oxides, were transported to the laboratory in Nalgene 4-ounce
plastic sample bottles. The acid was neutralized with sodium
hydroxide and the solution was evaporated to dryness over moderate
heat to avoid spattering. The residue was dissolved in 2 ml
of phenoldisulfonic acid with constant stirring. Twenty milliliters
of water were added to complete the dissolution of undissolved
salts. Upon the addition of 10 ml of concentrated ammonia,
a trialkali salt of 6 nitro-l-phenol-2-4 disulfonic acid was
formed, with a distinct yellow color which is proportional to
the concentration. The color was read with a Bausch & Lomb
Spectronic-20 visible spectrophotometer at 420 nm wave length,
and the NO2 concentration was obtained from a calibration curve
made specifically for that purpose.
Analysis of carbon dioxide and oxygen was performed on-site
using an Orsat analyzer. This is a standard apparatus which
volumetrically measures gaseous components by absorption into
a specific fluid. The samples were taken simultaneously at
the inlet and outlet using leveling bottles with a solution
of dilute sulfuric acid and methyl red.
-------
PAGE 17
V. DISCUSSION OF TEST RESULTS
In order to assess the efficiency of the PuraSiv S process,
a 1-month source sampling and continuous monitoring program
was undertaken. During this period 118 absorption cycles and a
variety of transient conditions were measured. Thus, the test data
obtained allowed for a complete mapping of system performance.
Copies of the original recorded strip charts can be found in Appen-
dix C. Listings of SO2 mass emission rate for each cycle are tabu-
lated in Appendices E and F. Typical cycles for adsorbers Al
and A2 are shown in Graphs 1 and 2, respectively; Graphs 4 through
10 depict various process unbalances and upsets.
The results of the continuous monitoring study were recorded on
a parts per million by a volume basis. The analyzer utilizes
a dual-range capability which permits the recorder to switch from
the 0 to 5000 ppm inlet scale to the outlet 0 to 300 ppm scale.
Example calculations demonstrating the technique used to arrive
at the SO2 mass emission rates are shown in Appendix B. The tail
gas flow rate was calculated by Coulton Chemical personnel and
then corrected to standard conditions (70°F and 29.92 inches Hg).
In determining the outlet mass emission rates, the inlet flow
rate was used. This results in an average emission rate equal
to the total of the main stack S02 emission rate plus the air
dryer stack emission rate, thus showing the PuraSiv S system to
be the single source of S02 emissions at the Coulton B-Plant.
This is justified by the fact that both the Federal and state
of Ohio Environmental Protection Agencies limit total emissions
of acid plant tail gas rather than emissions from individual points
within the plant.
A. Normal Operation
An unusually wide range of S02 inlet concentrations to the PuraSiv
S were experienced over the 4-week period, varying from a minimum
average of 2335 ppm to a maximum of 4800 ppm per cycle, with peaks
exceeding 5000 ppm during the recycle stages. The lower readings
were recorded during the first 2 days of testing and were due
in part to an improperly marked high-range calibration gas cylinder.
The cylinder was recalibrated using the procedure outlined in
the September 11, 1974 Federal Register.
After recalibration of the cylinders, correlation with wet tests
was within 5 percent. The readings obtained during the first
2 days are listed in the mass emission tables in Appendix B, but
they have been omitted from the summaries in Tables 1 and 2.
Since the plant was operating under the restriction of an undersized
electrical transformer, neither acid production nor tail gas flow
rate could be altered without imposing a serious equilibrium im-
-------
PAGE 18
balance on the plant. However, a simulation of variations in
loadings to the PuraSiv S was performed by increasing the time
of adsorption cycle and the S02 concentration to the adsorber.
Thus, we were able to exceed the maximum design loading conditions
to the PuraSiv unit. These results are tabulated by categorization
of:
(a) adsorber vessel.
(b) inlet concentration.
(c) length of cycle.
In addition, Table 1 summarizes the results of average mass emission
rates as a function of each of the above.
Inlet concentrations averaged less than 4000 ppm during 60 percent
of the test period, while the outlet emissions averaged 62 ppm
from adsorber A2 and 73 ppm from adsorber Al. The discrepancy
is due to a problem with an adsorbent bed support in adsorber
Al. The range of inlet concentrations, which represents maximum
capacity of the beds at a flow rate of 7500 SCFM, is 4000 to 4500
ppm. These inlet concentrations were experienced over 35 percent
of the test period, while the outlet of adsorber A2 averaged 82
ppm and adsorber Al 111 ppm. For the remaining periods (approxi-
mately 5 percent) the inlet concentrations of SO2 to the PuraSiv
exceeded 4500 ppm. At this time the concentration leaving adsorber
Al averaged 107 ppm and 99 ppm for A2.
Adsorbing vessels Al and A2 were designed to be identical in func-
tion and performance. Prior to testing, Al was found to have
a defective bed support, which caused a quantity of molecular
sieve to be lost from the system. As well as reducing the capacity
of that bed, the loss of some adsorbent altered the flow distribu-
tion through the vessel, which resulted in slightly less efficiency
for that unit.
Union Carbide Corporation guarantees that the PuraSiv S system
is capable of reducing the average S02 emission level to less
than 100 ppm* over a single cycle. A realistic evaluation, taking
the bed support problem of Al into consideration, shows that the
PuraSiv S emissions exceed this level in 13 percent of the total
number of cycles measured. The highest S02 emission level from
A2, averaged over a single cycle, was 118 ppm.
Graphs 1 and 2 represent typical cycles of normal operation for
adsorbers Al and A2, respectively. The adsorbers have similar
curves with the exception of slightly higher emission concentration
*Union Carbide Corporation "PuraSiv S Systems for Sulfuric Acid
Plants - Technical Fact Sheet."
-------
Cycle
Length
4:00-4:20
4:21-4:40
>4:41
4:00-4:20
4:21-4:40
4:40-4:21
4:00-4:20
4:21-4:40
>4:41
4:00-4:20
4:21-4:40
4:00-4:20
>4:41
Unit
Al
Al
Al
Al
Al
Al
A2
A2
A2
A2
A2
A2
A2
No. of
Cycles
6
24
2
6
12
2
2
23
5
9
8
4
1
TABLE
Avg.
Inlet
ppm
3672
3164
3013
4193
4206
4673
3270
3211
3060
4196
4246
4619
4620
1.
Avg.
Inlet
Ib/hr
276.6
235.0
223.3
316.5
314.8
352.7
245.1
238.3
227.9
316.7
318.7
348.7
341.6
S02 TEST
Avg.
Inlet
kg/hr
125.59
111.54
101.38
143.67
142.90
160.13
111.26
108.28
103.68
143.42
144.70
158.50
155.09
SUMMARY
Avg.
Outlet
ppm
92
65
113
129
99
107
62
55
91
86
77
100
98
Avg.
Outlet
Ib/hr
6.91
4.84
8.38
9.72
7.63
8.04
4.64
4.08
6.73
6.52
5.75
7.51
7.25
Avg.
Outlet
kg/hr
3.14
2.20
3.81
4.42
3.35
3.65
2.11
2.36
3.06
2.99
2.61
3.41
3.29
Efficiency
97.
97.
96.
96.
97.
97.
98.
98.
96.
97.
98.
97.
97.
5
9
3
9
6
8
1
3
9
9
2
9
9
"O
O
M
h
V
-------
PAGE 20
CYCLE
Avg.
Inlet
ppm
2600
3870
3930
3765
3965
3905
CYCLE
2795
2495
2610
3330
3290
3060
2590
3090
3460
2745
2780
3065
2960
3250
3335
3545
3195
3120
3385
2495
3510
3750
3645
3980
CYCLE
3045
2980
LENGTH:
Avg.
Inlet
Ib/hr
192.8
292.1
296.6
284.2
299.3
294.7
LENGTH :
207.2
185.0
193.0
249.9
243.9
226.9
192.0
229.1
256.5
203.5
205.5
226.6
218.9
240.3
246.6
262.1
236.2
230.7
250.3
217.7
259.5
283.0
275.1
300.4
LENGTH:
225.7
220.9
TABLE 2
4:00-4
Avg.
Inlet
kg/hr
87.5
132.6
134.7
129.0
135.9
133.8
4:21-4
94.1
84.0
87.9
113.5
110.7
103.0
87.2
104.0
116.5
92.4
93.3
102.9
99.4
109.1
112.0
119.0
107.2
104.7
113.6
98.8
117.8
128.5
124.9
136.4
4:41
102.5
100.3
. LIST OF
:20 UNIT
Avg.
Outlet
ppm
76
81
101
99
103
91
:40 UNIT
85
57
76
80
76
63
67
49
77
38
46
53
51
63
64
82
62
56
67
55
64
72
75
87
UNIT
123
103
S02 TEST CYCLES
: Al
Avg.
Outlet
Ib/hr
5.63
6.11
7.62
7.47
7.77
6.87
: Al
6.30
4.23
5.63
5.93
5.63
4.67
4.97
3.63
5.71
2.82
3.40
3.92
3.77
4.66
4.73
6.06
4.58
4.14
4.95
4.07
4.73
5.43
5.66
6.57
: Al
9.12
7.64
INLET CONDITIONS:
Avg.
<4000 ppm
Outlet Efficiency
kg/hr
2.56
2.77
3.46
3.39
3.53
3.12
INLET CONDITIONS:
2.86
1.92
2.56
2.69
2.56
2.12
2.26
1.65
2.59
1.28
1.54
1.78
1.71
2.10
2.15
2.75
2.08
1.88
2.25
1.85
2.15
2.47
2.57
2.98
INLET CONDITIONS:
4.14
3.47
97.1
97.9
97.4
97.4
97.4
97.7
<4000 ppm
97.0
97.7
97.1
97.6
97.7
97.9
97.4
98.4
97.8
98.6
98.3
98.3
98.3
98.1
98.1
97.7
98.1
98.2
98.1
98.1
98.2
98.1
97.9
97.8
<4000 ppm
96.0
96.5
-------
PAGE. 21
LIST OF SO? TEST
CYCLE
Avg.
Inlet
ppm
4020
4075
4420
4275
4100
4265
CYCLE
4080
4130
4495
4490
4245
4065
4205
4005
4250
4255
4105
4150
CYCLE
4700
4645
LENGTH:
Avg.
Inlet
Ib/hr
303.4
307.6
333.6
322.7
309.5
321.9
LENGTH:
301.7
305.4
332.0
332.0
313.9
306.8
317.4
302.3
320.8
321.7
309.8
313.2
LENGTH:
354.8
350.6
4:00-4:20
Avg.
Inlet
kg/hr
137.7
139.7
151.5
146.5
140.4
146.1
4:21-4:40
137.0
138.7
150.7
150.7
142.5
13,9.3
144.1
137.2
145.6
146.0
140.7
142.2
4:00-4:21
161.1
159.2
UNIT:
Avg.
Outlet
ppm
107
103
141
136
134
152
UNIT:
94
97
113
110
97
89
112
97
109
91
99
75
UNIT:
114
99
CYCLES (CONTD.)
Al INLET
Avg.
Outlet
Ib/hr
8.08
7.77
10.64
10.27
10.11
11.47
Al INLET
6.95
7.17
8.36
8.13
7.17
6.72
8.45
7.32
8.23
6.87
7.47
8.76
Al INLET
8.60
7.47
CONDITIONS :
Avg.
Outlet
kg/hr
3.67
3.53
4.83
4.66
4.59
5.21
CONDITIONS:
3.16
3.26
3.80
3.69
3.26
3.05
3.84
3.32
3.74
3.12
3.39
2.57
CONDITIONS:
3.90
3.39
4000-4500 ppm
Efficiency
97.3
97.5
96.8
96.8
96.7
96.4
4000-4500 ppm
97.7
97.6
97.5
97.6
97.7
97.8
97.3
97.6
97.4
97.9
97.6
98.2
>4500 ppm
97.6
97.9
-------
PAGE 22
LIST OF SO-) TEST
CYCLE
Avg.
Inlet
ppm
2605
3935
CYCLE
2755
2805
3440
3080
2750
2885
3230
2945
2740
2990
3235
2920
3305
3635
3460
3300
3360
3145
2810
3550
3980
3700
3830
CYCLE
3065
3230
2715
2375
3915
LENGTH:
Avg.
Inlet
Ib/hr
193.1
297.0
LENGTH:
204.2
208.0
255.0
228.3
203.9
213.9
239.5
218.3
203.1
221.1
239.2
215.9
244.4
268.8
255.8
244.0
248.4
232.5
207.8
264.5
300.4
279.3
289.1
LENGTH:
227.2
239.5
201.3
176.1
295.5
4:00-4:20
Avg.
Inlet
kg/hr
87.7
134.8
4:21-4:40
92.7
94.4
115.8
103.7
92.6
97.1
108.7
99.1
92.2
100.4
108.6
98.0
111.0
122.0
116.1
110.8
112.8
105.6
94.3
120.1
136.4
126.8
131.3
4:41
103.2
108.7
91.4
80.0
134.2
UNIT:
Avg.
Outlet
ppm
54
70
UNIT:
74
61
81
63
68
40
50
45
28
33
49
40
52
62
71
53
54
50
51
54
64
59
64
UNIT:
111
107
66
102
67
CYCLES (CONTD.)
A2 INLET
Avg.
Outlet
Ib/hr
4.00
5.28
A2 INLET
5.49
4.52
6.01
4.60
5.04
2.97
3.71
3.34
2.07
2.33
3.62
2.96
3.84
4.58
5.25
3.92
3.99
3.70
3.77
3.99
4.83
4.45
4.83
A2 INLET
8.23
7.93
4.89
7.56
5.06
CONDITIONS
Avg.
Outlet
kg/hr
1.82
2.40
CONDITIONS
2.49
2.05
2.73
2.09
2.29
1.35
1.68
1.52
.94
1.11
1.64
1.34
1.74
2.08
2.38
1.78
1.81
1.68
1.71
1.81
2.19
2.02
2.19
CONDITIONS
3.74
3.60
2.22
3.43
2.30
: <4000 ppm
Efficiency
97.9
98.2
: <4000 ppm
97.3
97.8
97.6
98.0
97.5
98.6
98.5
98.5
99.0
98.9
98.5
98.6
98.4
98.3
98.0
98.4
98.4
98.4
98.2
98.5
98.4
98.4
98.3
: <4000 ppm
96.4
96.7
97.6
95.7
98.3
YORK RESEARCH CORPORATION
STAMFORD, CONNECTICUT
-------
PAGE. 23
LIST OF S02 TEST CYCLES (CONTD.)
CYCLE
Avg.
Inlet
ppm
4500
4000
4290
4150
4040
4225
4365
4090
4100
CYCLE
4445
4500
4215
4000
4270
4170
4165
4200
CYCLE
4540
4800
4520
4615
CYCLE
4620
LENGTH:
Avg.
Inlet
Ib/hr
339.7
301.9
323.8
313.2
304.9
318.9
329.5
308.7
309.5
LENGTH:
328.7
332.7
318.1
301.9
322.3
314.7
314.4
317.0
LENGTH:
342.7
362.7
341.2
348.3
LENGTH:
341.6
4:00-4:20
Avg.
Inlet
kg/hr
151.1
137.1
147.0
142.2
138.4
144.8
149.6
140.2
140.5
4:21-4:40
149.2
151.1
144.4
137.1
146.3
142.9
142.7
143.9
4:00-4:20
155.6
164.7
154.9
158.1
4:41
155.1
UNIT:
Avg.
A2 INLET
Avg.
Outlet Outlet
ppm
72
77
86
75
101
106
118
75
68
UNIT:
84
87
75
70
80
70
73
74
UNIT:
91
87
110
110
UNIT:
98
Ib/hr
5.43
5.81
6.49
5.66
7.62
8.00
8.91
5.66
5.13
A2 INLET
6.21
6.43
5.66
5.28
6.04
5.28
5.51
5.59
A2 INLET
6.87
6.57
8.30
8.30
A2 INLET
7.25
CONDITIONS
Avg.
Outlet
kg/hr
2.92
2.40
2.95
2.57
3.46
3.63
4.05
2.57
2.33
CONDITIONS
2.82
2.92
2.56
2.40
2.74
2.40
2.50
2.54
CONDITIONS
3.12
2.98
3.77
3.77
CONDITIONS
3.29
: 4000-4500 ppm
Efficiency
98.1
98.2
98.0
98.2
97.5
97.5
97.3
98.2
98.3
: 4000-4500 ppm
98.1
98.1
98.2
98.2
98.1
98.3
98.2
98.2
: >4500 ppm
98.0
98.2
97.6
97.6
: >4500 ppm
97.9
-------
PAGE 24
from Al. The typical curve of plant tail gas concentration has
a period of higher S02, beginning at the start of the second
hour in the PuraSiv cycle and continuing for 1% to 2 hours. This
is caused by the desorbed S02 being released from the regenerating
bed and recycled through the plant. Following the recycle period
is a light lowering of S02 concentration, caused by a dilution
of plant tail gas from the flush of cool air through the bed at
the end of the regenerative cycle.
Efficiency of the PuraSiv S is represented by:
Inlet-Outlet
Inlet
Graph 3 shows efficiency of adsorbers Al and A2 using the emission
data from Graph 1 and Graph 2. Efficiency for each adsorber de-
creases with time and is relatively unaffected by inlet concen-
tration. This is demonstrated by the fact that no discontinuities
are shown where inlet concentration changes in the second and
third hours of the cycle. Upon extrapolation of the curves, we
would experience breakthrough. However, since we have no supporting
mathematical data as to the limits involved, this phenomenon has
not been predicted. The curves do show, however, that breakthrough
would occur on Al before A2.
B. Transient Conditions
The analyzer, operating continuously, has documented emissions
during several minor process upsets as well as recorded two plant
shutdowns and startups. The delicate nature of the equilibrium
balance of a contact sulfuric acid plant is responsible for drastic
changes in S02 tail gas concentrations. Low S02 caused by a high
converter temperature is responsible for the upset shown in Graph
4. As inlet concentration drops, so does emission level. The
average emission level over the cycle, however, does not vary
appreciably from normal operation.
Erratic converter temperature caused by a malfunction in a con-
denser controller is responsible for the upset represented in
Graph 5. Again, the PuraSiv average emission does not vary appre-
ciably from the emission found under normal conditions. The upset
represented in Graph 6 is different in nature from the previous
ones in that inlet concentration is excessively higher than normal
(greater than 5000 ppm). The emission level rises rapidly during
this period but drops when inlet concentration drops. It is ob-
vious, however, that if the inlet concentration had continued
at the high level for a longer period of time, then the emission
would have reached 300 ppm (maximum scale) before the end of the
cycle. This upset occurred when a sulfur plug in the burner feed
line was dislodged, and a slug of sulfur was dumped into the burner.
Graph 7 and Graph 8 represent emissions recorded during two separate
plant shutdowns. Graph 7 was a plant shutdown taking place on
-------
PAGE 25
February 9, 1975 due to a freezeup in the absorbing tower.
During this shutdown the PuraSiv was taken off-line and tail gas
was bypassed and vented to the atmosphere. Graph 8 depicts a
shutdown which took place on February 13, 1975 in order to make
repairs on an acid pump. During this shutdown the PuraSiv was
left on-line with the obvious characteristic of low emission levels
throughout.
Graph 9 and Graph 10 show the S02 concentrations experienced during
two separate plant startups. Concentrations in excess of maximum
scale on the instrument were experienced at both inlet and outlet
locations. After the first two PuraSiv cycles, however, normal
conditions were re-established.
C. Wet Tests
The results of the wet tests are shown in Tables 3 through 11
and define the location, date, and time of the tests. Results
are in terms of averages plus or minus the 95 percent confidence
limit. Sulfur trioxide results are not reported due to erroneously
high values obtained. It is believed that incorrect purging of
the sample train was responsible for the high results.
One of the original objectives of the test period was to define
any change in performance of the adsorber over a period of 4 weeks
and to correlate the change with the presence of tail gas impurities,
The delicate nature of the acid plant equilibirum was responsible
for constantly changing conditions: e.g., composition of feed,
temperature of converter, and fluctuating of S02 by recycle. Daily
performance change was documented; however, a performance change
over 4 weeks would be unnoticeable because of the drastic changes
mentioned above. In order to obtain documentation of performance
versus time, a program with a time span of at least 6 months would
be necessary.
The results of the tests for certain tail gas impurities - e.g.,
sulfide, chloride, and total acid - was dependent primarily upon
composition of furnace feed. Due to their variable nature, these
results are considered as base-line data.
It was noted that these compounds were adsorbed on the PuraSiv
beds in varying degrees since the outlet wet tests yielded results
which were generally lower than the inlet results. The effect
of these compounds on the performance of the sieve material on
both efficiency and life is unknown since wet tests were not per-
formed on the desorbed gas returning to the plant.
-------
NO. 34DR-lO'/i DIET2GEN GRAPH PAPER
ID X ID PER HALT INCH
EUBENE DIETZGEN CO.
MADE IN U. 5. A.
Graph 1
Typical Cycle During Normal
Operation-Adsorber Al
Cycle Start At 0900 2-20-75
Time (Hours)
-------
GRAPH PAPER
X 1 O PER HALF INCH
EUGENE DIET2GEN CO.
MADE IN U. S. A.
Graph 2
Typical Cycle During Normal
Operation-Adsorber A2
Cycle Start At 1025 2-19-75
Time (Hours)
-------
NO. a-lOR-lD'-a DIETZGEN GRAPH PAPER
ID X ID PER HALF INCH
EUGENE DIETZGEN CO.
MADE IN U. S. A.
Graph 3
Adsorber Efficiency Vs.
Time For Typical Cycle
During Normal Operation
Time (Hours)
-------
1830
Graph 4
Process Upset-High Converter
Exit Temperature
Cycle Start At 1830 2-5-75
T~ Of Upset
Time (Hours)
-------
ND. 34DR-lD'/i DIETZQEN GRAPH PAPER
ID X 1D PER HALF INCH
EUGENE DIETZGEN CO.
MADE IN U. S. A.
Graph 5
Process Up set-Malfunction
Of Condenser Controller
Causing Erratic Converter
Temperature Cycle Start At
1015 2-12-75
Beginning
I I I I I I ! I I I I i I ! I I II
Time (Hours)
0
-------
Graph 6
Process Upset- "Slug" Of Sulfur
Dumped Into Burner
Cycle Start At 1600 2-18-75
-------
K...
10 X 10 TO '-i INCH- 74 X 10 INCHES
KEUFFEL a ESSER CO. MADE IN u S *
46 1473
Graph 7
Plant Shutdown With PuraSiv
Off-Line 2200 2-9-75
en
tn
to
-------
R-E
KLUU II ft Eb^rR CO
46 1473
Graph 8
Plant amtdown With PuraSiv
On-Line 1400 2-13-75
tSHHUTSHHil
^ Time (Hours)
-------
K
UC 10 X 10 TO H INCH»7H X 10 INCHES
- *^ KEUFFtL & ESSER CO. M*Df IN U S *
46 1473
Graph 9
Plant Startup
Begin At 1400 2-11-75
Adsorbers
Alternate Adsorbers
"_\ Time (Hours)
-------
Graph 10
Plant Startup
Begin At 1000 2-13-75
S
ui
-------
TABLE 3. DUPONT SO? ACCURACY CALCULATIONS
Date
2/12
2/12
2/12
2/14
2/14
2/14
2/14
2/17
2/17
2/17
2/17
2/17
2/18
2/18
Time Test No. Location
1035
1147
1555
0924
0925
1134
1224
1133
1135
1320
1340
1435
1116
1110
- 1 n
C.I. 95 =
C I 95 -
v * -L. ' ^
Accuracy =
1
2
3
4A
4B
5
6
7
8
9
10
11
12
13
= 51.5
t.975 { n (
n/n-1
2160 {14
14/13
{51.5 + 42
1576.4
Inlet
Outlet
Inlet
Inlet
Inlet
Oulet
Outlet
Inlet
Outlet
Inlet
Outlet
Outlet
Outlet
Inlet
Ex-2)
1
(106913
.28} x
Method 6
ppm/v
3322
72.3
3359
3176
3022
115
15.1
2615
88.3
2749
16.2
45.7
120.6
3354
( Ex.)2}
\ f-»J^. / J
h
100 = 5.95%
DuPont
ppm/v
3300
73
3385
3217
3217
102
7.5
2500
84
2525
10.5
39
135
3400
X
Difference
22
0.7
26
41
195
13
7.6
115
4.3
224
5.7
6.7
14.4
46
(X2)
484
.49
676
1681
38025
169
57.76
13225
18.49
50176
32.5
44.9
207.4
2116
-------
TABLE 4.
Date
2/20
2/20
2/20
2/21
2/21
2/21
2/26
2/26
2/26
2/26
2/27
2/27
Time Location
1105
1230
1420
1022
1128
1225
1117
1120
1315
1315
1032
1030
AVERAGE
AVERAGE
*Loss
of sampl
Inlet
Inlet
Inlet
Outlet
Outlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
e during
ppm/V
1.04
3.66
.22
.13
.21
1.47
1.06
1.89
1.24
1.40
.87
1.89
.62
SULFURIC ACID
mg/SCM
4.27
14.97
.883
.530
.883
5.90
4.27
7.27
4.98
5.58
3.50
7.60
2.51
kg/hr
.0540
.1891
.0113
.0068
.0109
.0762
.0549
.0975
.0639
.0721
.0449
.0978
.0321
MIST EMISSION RESULTS
kg/metric
ton
.0095
.034
.002
.001
.002
.012
.009
.016
.0105
.012
.0075
.017
.0065
mg/SCF
.121
.424
.025
.015
.025
.167
.121
.206
.141
.158
.099
.215
.071
gr/SCF
.0019
.0065
.0004
.0002
.0004
.0026
.0019
.0032
.0022
.0024
.0015
.0033
.0011
Ib/hr
.119
.417
.025
.015
.024
.168
.121
.215
.141
.159
.099
.216
.071
Ib/ton
.019
.068
.004
.002
.004
.025
.018
.032
.021
.024
.015
+ .025
+ .009
transportation.
-a
O
LO
vj
-------
PAGE. 38
TABLE 5. TOTAL ACID
Date
2/6
2/6
2/6
2/6
2/6
2/6
2/24
2/24
2/24
2/24
2/25
2/25
AVERAGE
AVERAGE
*Emissions
including
Time
0927
0915
1030
1010
1110
1058
1452
1452
1040
1040
1150
1153
are
H2S04
Location
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
EMISSION RESULTS
Meq/SCF*
.143
.0189
.135
.0225
.131
.0262
.122
.0179
.0778
.0140
.0605
.0193
.111
.0198
reported as mil Hi equivalents of
Meq/SCM*
5.050
.667
4.767
.795
4.626
.925
4.308
.632
2.747
.494
2.136
.682
+1.259
± -146
total acid,
-------
TABLE 6. CHLORIDE EMISSION RESULTS*
Date
2/6
2/6
2/6
2/6
2/6
2/6
2/24
2/24
2/24
2/24
2/25
2/25
Time
0927
0915
1030
1010
1110
1058
1452
1452
1040
1040
1150
1153
AVERAGE
AVERAGE
Location
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
ppm/V
.911
.025
4.11
.010
1.494
.026
.370
.009
.201
.019
.578
.009
1.277
.016
mg/SCM
2.871
.0777
12.716
.0330
4.718
.0836
1.166
.0285
.6362
.0617
1.818
.0279
3.988
.0521
kg/hr
.0471
.0013
.2125
.0005
.0772
.0013
.0191
.0004
.0104
.0010
.0299
.0004
.0660
.00082
mg/SCF
.0813
.0022
.36
.0009
.133
.0024
.0330
.0008
.0180
.0017
.0515
.0008
.1128
.0015
gr/SCF
.00125
.00003
.00555
.00001
.0205
.00004
.00051
.00001
.00028
.00003
.00079
.00001
.00481
.000022
Ib/hr
.104
.003
.469
.001
.170
.003
.042
.001
.023
.002
.066
.001
+ .105
+ .001
*Reported as Cl~.
oo
-------
TABLE 7. SULFIDE EMISSION RESULTS
Date Time
2/14 0924
2/14 0925
2/14 1134
2/14 1224
2/17 1133
2/17 1320
2/20 1105
2/20 1230
2/20 1420
2/21 1022
2 21 1128
2 '21 1225
AVERAGE
AVERAGE
*Reported as CS2
^Indicates that
Location ppm/V
Inlet <.5fc
Inlet <.5
Outlet 6.87
Outlet 6.18
Inlet <.5
Inlet 12.0
Inlet 14.4
Inlet 13.1
Inlet <.5
Outlet <.5
Outlet < . 5
Outlet 19.0
Inlet 5.93
Outlet 6.61
mg/SCM kg/hr
<2
<2
21.68 .871
19.49 .248
<2
37.80 .481
45.20 .576
41.32 1.656
<2
<2
<2
59.68 .762
18.90
20.97
concentration is below the detectable
mg/SCF gr/SCF Ib/hr
<.05
<.05
.614 .0095 1.92
.552 .0085 .546
<.05
1.07 .016 1.06
1.28 .020 1.27
1.17 .018 3.65
<.05
<.05
<.05
1.69 .026 1.68
.53
.59
limit of the analysis method.
-------
PAGE 41
Date
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
2/7
AVERAGE
AVERAGE
* Re ported
TABLE 8.
Time
0840
0850
0900
0910
0920
0930
0940
0950
1000
1010
1055
1105
1115
1125
1135
1145
1155
1205
1215
1225
as Hexane.
tLoss of sample due
HYDROCARBON EMISSION RESULTS*
Location ppm/V
Inlet
Inlet
Inlet
Inlet
Inlet
Inlet
Inlet
Inlet
Inlet
Inlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Inlet
Outlet
to flask
20.
71.
t
70.
38.
23.
41.
18.
58.
29.
5.
10.
8.
18.
-11.
35.
79.
t
51.
35.
41.
28.
leakage
1
9
1
5
3
3
4
9
9
3
9
2
6
5
9
3
3
6
38
51
kg/hr
.911
3.26
3.18
1.75
1.06
1.87
.834
2.67
1.36
.240
.494
.372
.844
.522
1.63
3.60
2.33
1.61
1.88
1.29
Ib/hr
2
7
7
3
2
4
1
5
2
0
1
0
1
1
3
7
5
3
+1
+1
.01
.19
.01
.85
.33
.13
.84
.89
.99
.53
.09
.82
.86
.15
.59
93
.13
.56
.61
.89
-------
TABLE 9. OXIDES OF NITROGEN EMISSION RESULTS
Date
2/6
2/6
2/6
2/6
2/6
2/6
2/6
2/6
2/6
2/6
2/6
2/6
2/25
2/25
2/25
2/25
2/25
2/25
2/25
2/25
2/25
2/25
2/25
2/25
Time
1105
1105
1110
1110
1115
1115
1120
1120
1125
1125
1130
1130
1400
1400
1405
1405
1410
1410
1415
1415
1420
1420
1425
1425
AVERAGE
AVERAGE
Location
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
ppm/V
13.2
7.9
19.5
9.2
11.1
*
16.7
13.5
9.1
9.8
14.8
11.4
*
21.5
15.3
11.8
23.1
11.2
18.6
19.9
21.0
18.3
22.8
11.4
16.84
13.26
mg/SCM
.0293
.0164
.0391
.0198
.0222
.0361
.0292
.0192
.0206
.0310
.0243
.0403
.0285
.0233
.0428
.0236
.0365
.0378
.0379
.0335
.0448
.0216
.0334
.0264
kg/hr
.32
.19
.43
.22
.27
.40
.33
.22
.24
.35
.28
.53
.38
.29
.57
.28
.46
.49
.52
.45
.56
.28
.41
.33
mg/SCF
.00083
.00046
.00111
.00056
.00063
.00102
.00083
.00054
.00058
.00088
.00069
.00114
.00081
.00066
.00121
.00067
.00103
.00107
.00107
.00095
.00127
.00061
.00095
.00075
gr/SCF
x 10-5
1.28
.71
1.71
.86
.97
1.58
1.28
.84
.90
1.35
1.06
1.76
1.24
1.02
1.87
1.03
1.59
1.65
1.66
1.46
1.96
.94
1.46
1.15
Ib/hr
.70
.42
.94
.48
.59
.89
.72
.49
.52
.78
.61
1.16
.83
.64
1.25
.61
1.01
1.08
1.14
.99
1.23
.62
+ .17
+ .17
*Loss of sample due to flask leakage,
-------
PAGE 4 3
Date
2/12
2/12
2/14
2/14
2/15
2/15
2/16
2/16
2/17
2/17
2/18
2/18
2/19
2/19
2/20
2/20
2/21
2/21
Time
0930
1105
1450
1535
1005
1120
0915
1055
1325
1445
1520
1645
0830
1000
0925
1050
0820
0955
AVERAGE
AVERAGE
TABLE 10
Location
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet 18
Outlet 4
. MOISTURE RESULTS
PPM
18
5
20
4
15
3
22
5
18
4
18
4
18
4
17
4
18
5
.2 + 1.5
.2 + .5
mg/SCM
13.42
3.71
14.90
2.97
11.19
2.22
16.38
3.71
13.42
2.97
13.42
2.97
13.42
2.97
12.68
2.97
13.42
3.71
13.58
3.13
mg/SCF
.380
.105
.422
.084
.317
.063
.464
.105
.380
.084
.380
.084
.380
.084
.359
.084
.380
.105
.385
.089
gr/SCF
.0058
.0016
.0065
.0013
.0049
.0010
.0072
.0016
.0058
.0013
.0058
.0013
.0058
.0013
.0055
.0013
.0058
.0016
.0059
.0014
-------
PAGE 44
TABLE 11. ORSAT READINGS
Date Time Location % CO 7
2/3 1530 Inlet 3.5
2/3 1530 Outlet 2.9
2/6 1100 Inlet 2.7
2/6 1100 Outlet 2.8
2/6 1200 Inlet 2.2
2/6 1200 Outlet 2.2
2/24 1030 Inlet 4.7
2/24 1030 Outlet 4.8
2/24 1120 Inlet 4.8
2/24 1120 Outlet 4.3
2/27 1300 Inlet 3.8
2/27 1300 Outlet 3.9
AVERAGE Inlet 3.6
AVERAGE Outlet 3.5
% 02 % CO
7.8 0.0
6.0 0.0
5.2 0.0
5.2 0.0
5.6 0.0
7.2 0.0
5.3 0.0
5.6 0.0
5.8 0.0
5.7 0.0
4.4 0.0
4.5 0.0
5.7 0.0
5.7 0.0
-------
PAGE 45
APPENDIX A
INSTALLATION AND OPERATION OF CONTINUOUS MONITORING SYSTEM
Description of Equipment
The DuPont 460/1 operates on the principle that specific gases
absorb radiant energy at specific wave lengths in proportion to
their concentrations. The sample gas passes through a No. 316
stainless steel sample cell which is a tube with a quartz window
covering each end. An ultraviolet light source projects a beam
through the cell that is picked up by a photometric detection system.
The detector consists of a series of optical filters that permit
only the light of certain wave lengths to pass through. A prism
splits the selected light beam in two and transmits each beam
to a separate phototube. One measures the energy at 280 nm (mea-
suring band) and the other the energy at 578 nm (the reference
band). The difference between these resultants is equivalent
to the amount of energy absorbed by the sample gas, which is then
proportional to the pollutant concentration. The detector output
is amplified and transmitted to the recorder, which provides an
analog instrument output. Precision of this instrument is claimed
by DuPont to be +2 percent.
The DuPont 460/1 was .included with the capability of measuring
gaseous concentrations at two separate sampling locations. An
integral programmer determines which mode the analyzer is operating
in at any given time. Since the instrument has only one sampling
interface, it cannot sample two locations simultaneously; instead,
it samples one location and backflushes the system with clean
air before it samples the other location. Normal operation is
to sample one location for 90 seconds and backflush for 30 seconds
and to sample a second location for 90 seconds and backflush again
for 30 seconds to complete one full cycle. The instrument also
has the capability to measure NOX; however, a measurement at either
location increases the total cycle time by 12 minutes per reading.
Since this would drastically reduce the number of S02 readings,
it was decided that the NOX analysis mode would not be used so
that trends and patterns of SO2 emissions could be more clearly
defined.
The recorder used with the DuPont 460/1 was a Leeds & Northrup
Speedomax H multipoint unit. A modified Leeds & Northrup Flexelect
B programmer is an integral part of the recorder; it provides
programmable, sequential sample-point selection and automatic
zero control.
-------
PAGE 46
Installation
The entire DuPont system was permanently mounted in a 12-foot
steel trailer and was complete with a sample-handling system and
calibration input manifold, valves, and switches. Once at the
site the necessary hookups were made, including:
(1) electrical power (110 v).
(2) compressed air (50 psig).
(3) sample lines (2^-inch od Teflon).
(4) calibration standards (zero air and three ranges of S02).
After the instrument was set up, it became apparent that a single
range for both sampling points would be ineffective since the
inlet concentrations ranged from 2500 to 4000 ppm, while the outlet
concentrations ranged from 0 to 150 ppra. A dual range capability
was adapted to the instrument which allowed an inlet span of 0
to 5000 ppm and an outlet span of 0 to 300 ppm. The adaptation
consisted of a relay and an extra 20 K potentiometer wired into
the Flexelect; each sampling mode was transferred through a separate
potentiometer, thus permitting independent calibration of each
mode.
Operation
Normal operation of the plant is 24 hours per day. The analyzer
also operated 24 hours per day and was left running even during
shutdowns. Normal procedure was to calibrate with standard gases
once per day per channel. Zero adjustment is automatic on the
DuPont.
The sample cell windows were cleaned once per week. This insured
that no build-up of foreign material interfered with the photometer.
-------
PAGE 47
APPENDIX B
CALCULATION OF S02 MASS EMISSION RATE
(1) S02 Mass Rate to PuraSiv S Inlet
Ib/hr inlet = (Q) x (ppm inlet) x 64.1 Ib x mole x 60 min
mole 387 cu ft hr
-6
ppm
where: Q = inlet flow rate as calculated by plant personnel -
(SCFM)
ppm = SO 2 concentration as measured by photometric
analyzer.
(2) S02 Mass Emission Rate
Ib/hr outlet = (Q) x (ppm outlet) x 64.1 Ib x mole x 60 min
mole 387 cu ft hr
x 60 min x 10"6
hr ppm
where: Q = inlet flow rate as calculated by plant
personnel - (SCFM)
ppm outlet = SO 2 concentration as measured by photo-
metric analyzer.
(3) S02 Mass Collected by PuraSiv S per Cycle
Ib S02 = Ib/hr inlet - Ib/hr outlet x (t)
cycle
where: t = length of cycle in hours
(4) S02 Mass Emission on a Daily Basis:
N
I. Ib/hr outlet
Ib S02 = i = 1 x 24 hr/day
day n
where: n = number of cycles in a 24-hour period
-------
PAGE 48
(5) S02 Mass Emission Rate per Ton of Acid Produced:
Ib/ton SO2 = Ib/day SO?
daily production rate
(6) Efficiency of S02 Removal:
Efficiency = 100 x Ib/hr inlet - Ib/hr outlet
Ib/hr inlet
-------
PAGE 49
APPENDIX C
WET CHEMICAL TEST METHODS
Sulfur Dioxide
The test method followed in the collection of sulfur dioxide samples
was a modified version of EPA Method 6, "Determination of Sulfur
Dioxide Emissions from Stationary Sources."* The modification
consisted of saving the catch from the isopropyl alcohol bubbler
and analyzing the contents for sulfur trioxide and/or sulfides.
A glass probe, wound with nichrome wire and sheathed with stainless
steel, was used to extract the sulfur dioxide samples. A glass
wool prefilter in the end of the probe inhibited acid mist entrain-
ment into the sample stream. The probe was attached to the sample
train by means of a three-way stopcock tee utilizing ground-glass
ball and socket joints. At the inlet sample location, where
postive internal duct pressures were encountered, the pump was
bypassed and the sample stream allowed to be pushed through the
train and gas meter by the duct pressure. Adjustment of the sample
flow rate was accomplished by turning the stopcock tee.
The midget impinger train included a midget bubbler containing
15 ml of 80 percent isopropyl alcohol initially, followed by
two midget impingers in series with each containing 15 ml of
3 percent hydrogen peroxide initially. A final midget impinger
was left blank in order to collect any carry-over from the previous
impingers. Incorporated into the sample line between the final
impinger and the pump (the gas meter at the inlet) was a drying
tube filled with silica gel. The gas measured total sample
volume and a rotameter measured sample flow rate (see Figure
Al) .
Sulfuric acid is soluble in isopropyl alcohol; therefore, any
acid mist or sulfur trioxide will be scrubbed out in the midget
bubbler, while sulfur dioxide will pass through. Available oxygen
from the hydrogen peroxide in the second and third impingers
combines with sulfur dioxide, forming the reactive trioxide,
which is then readily absorbed in the water. A small amount
of sulfur dioxide will remain in the isopropyl alcohol and must
be removed prior to cleanup of the train. This is accomplished
by pulling clean, sulfur-free air through the train, entraining
the sulfur dioxide, and allowing the second and third impingers
to scrub it out. The hydrogen peroxide impingers have a collection
*Federal Register, Vol. 36, No. 247, Thursday, December 23, 1971.
-------
SOZ
TR9IIO
ROTAMETER
15
MANOMETER
567
IMPINGERS IN
ICE BATH
"O
O
fn
FIGURE AI
en
o
-------
PAGE 51
efficiency of 90 percent for S02,thereby providing a combined
collection efficiency of 99 percent. The analysis has an accuracy
of 1.53 standard error.
The cleanup was accomplished by transferring the contents of the
first midget impinger to a 4-ounce plastic sample bottle and
adding the alcohol rinse. The contents of the second, third,
and fourth impingers were transferred to a second bottle and
the distilled water rinse was added.
Sulfuric Acid Mist
Sulfuric acid is a liquid that forms droplets with extremely small
diameters at temperatures less than 640°F. In order to catch these
small particles, the sample gas was pulled through a high-effi-
ciency Fiberglas filter contained in a stainless steel holder.
These filters have a collection efficiency of 99.9 percent of
particles greater than 0.3 microns as measured by the OOP test,
and have an over-all efficiency of 98 percent of all particles
greater than 0.05 microns. Prevention of water condensation on
the filter, and hence the loss of the catch by leaching, was pro-
vided by enclosing the filter holder in an insulated box with
a heating element and controller set to a temperature of 250°F.
At this temperature, no condensation of water occurs, although
sulfuric acid will remain in the liquid state (see Figure A2).
The filter was connected to the heated glass probe on the inlet
side and to the three-way stopcock tee on the outlet side through
ground glass to stainless steel ball and socket joints. The
tee serves as connector between the filter holder and the inlet
to the series of four sequential midget impingers. The first
midget impinger is used to collect any sulfur trioxide that may
have passed through the filter and contains 15 ml of 80 percent
isopropyl alcohol. The second and third impingers in the series
each contain 15 ml of hydrogen peroxide, collecting the sulfur
dioxide from the sample stream. A fourth remains empty in order
to collect any carry-over.
At the inlet, sulfuric acid mist tests were performed by the
same method used for sulfur dioxide but without using the pump.
The gas meter was used to measure total sample volume, while a
rotameter measured sample flow rate. Gas velocity in the duct
was measured with the use of a pitot tube (standard-type at inlet,
S-type at outlet), and sample flow rate was adjusted to isokinetic
conditions through the use of a needle valve inserted in the sample
line prior to the gas meter.
The cleanup included removing the filter and carefully placing
it in a sealed plastic container for storage until analysis.
The contents of the first midget impinger and the alcohol rinse
of the impinger and stopcock tee were transferred to a Nalgene
4-ounce plastic sample bottle. The contents of the second, third,
-------
M midget impingers
in ice bath-55°F
Filter and
Holder
250°F
2
Probe
Nozzle
Fan
Thermostatic Switch-250°F
DIAGRAM OF A HEATED MIDGET .SAMPLE TRAIN 8 PROBE
FIGURE A 2
O
m
tn
-------
PAGE 53
and fourth impingers were transferred to a separate 4-ounce plastic
sample bottle, and a distilled water rinse was added to it. The
collection efficiency of the train is 99.9 percent.
Sulfur Trioxide and Sulfides
Samples for these tests were obtained by drawing sample gas through
a heated glass-lined probe and bubbling the gas through a series
of four impingers, as described on page Cl. The first impinger
contained 15 ml of 80 percent isopropyl alcohol, while the second
and third contained 15 ml of 3 percent hydrogen peroxide, and
the fourth remained empty. Sulfur trioxide forms sulfuric acid
with the water in the isopropyl alcohol, while sulfur dioxide
passes through the hydrogen peroxide upon purging of the train.
A sample prefilter was used to prevent sulfuric acid from entering
the probe. The collection efficiency is 95 percent.
The impingers were connected with glass U-connectors with ground-
glass ball and socket joints. A silica gel drying tube was used
between the exit of the last impinger and the entrance to the
pump in order to prevent water vapor from entering the pump.
A gas meter was used to measure total gas sample volume on a dry
basis. As with sulfur dioxide and sulfuric acid mist tests,
no sample pump was used at the inlet location where internal
duct pressure was allowed to push the sample through the train.
Sample flow rate was adjusted by partially closing the stopcock
tee.
Cleanup was accomplished by collecting the contents of the first
impinger and the alcohol rinses of the impinger and the probe
into a 4-ounce plastic sample bottle.
Total Acids and Chloride
The equipment for these tests included a stainless steel probe,
large-diameter rubber tubing, and three impingers of the Greenburg-
Smith design. 100 milliliters of distilled water were placed in
each of the first and second impingers, while the third was modified
by replacing the tip with an open tube extending to within % inch
of the bottom. Three hundred grams of silica gel in the third
impinger prevented water from entering the gas pump and gas meter.
The impingers were linked using large-diameter rubber tubing;
at the inlet location the precaution of taping the impinger to
the bottle in order to prevent separation under pressure was taken.
A sliding vane pump was used to pull the sample, while a standard
gas meter was used to measure total sample volume. Sample flow
rate was measured by timing the revolutions of the meter face,
while adjustment of sample flow rate was maintained with a gate
valve across the pump connections (see Figure A3).
The water samples were transferred to glass jars with Teflon lids
and to this was added the distilled water rinse of probe, hoses,
-------
IMPINGERS
AIR PUMP
TEMPERATURE
DRY GAS METER
35
m
SAMPLING TRAIN
FIGURE A3
.1U1
-------
PAGE 55
and impingers. Collection efficiencies for both parameters above
are 99 percent.
Hydrocarbons
Hydrocarbon samples were obtained in 500-ml glass grab flasks
which are cylindrically shaped and have an opening at each end
with a ground-glass stopcock. One end was connected to the heated
glass-lined probe from which the sample was extracted, while the
other end was attached to a sliding vane vacuum pump with large-
diameter rubber tubing. Each flask was conditioned by wrapping
it with a heating tape. Each was heated to approximately 130°F,
being simultaneously purged with stack gas. After approximately
5 minutes of conditioning the flask, the sample was enclosed
by shutting both valves. The flasks were transported to the
Stamford laboratory in a foam-packed case for analysis by gas
chromatography (see Figure A4). Collection efficiencies are 99.9
percent and analysis accuracy +0.5 percent of full-scale deflection.
Nitrogen Oxides
Nitrogen oxides were sampled using EPA Method 7, "Determination
of Nitrogen Oxide Emissions from Stationary Sources."* The samples
were obtained' in 2-1 glass boiling flasks, encased in styrofoam
and equipped with a three-way glass stopcock tee utilizing ground-
glass ball and socket joints. Twenty-five milliliters of a dilute
sulfuric acid/hydrogen peroxide absorbing solution were placed
in each flask prior to sampling. A sliding vane vacuum pump
capable of producing 26 inches of Hg negative pressure was connected
to the back of the tee via high-vacuum gum rubber, while the
front of the tee was connected to the heated, glass-lined stack
probe. The vacuum induced by the pump was monitored with a mercury
manometer, one leg of which was tied into the pump vacuum while
the other leg was open to the atmosphere. After evacuating the
flask, the pump inlet was pinched in order to see if a leak were
present; if not, the three-way stopcock was positioned so that
the flask was sealed and the probe open for purging. After purging,
the sample was taken by turning the three-way stopcock very slowly,
allowing the sample to enter the flask at a rate whereby the pres-
sures were equalized after about 15 seconds (see Figure A5).
In order to ensure complete absorption of nitrogen oxides into
the solution of dilute sulfuric acid/hydrogen peroxide, each flask
was shaken vigorously for a period of 5 minutes. After a period
of 16 hours, during which the solution and the sample gas come
to an equilibrium state, the flasks were shaken again and a final
pressure was obtained from the mercury manometer. The contents
*Federal Register, Vol. 36, No. 247, Thursday, December 23, 1971.
-------
STRCK
V9R1BC
punp
FIGURE A4
TJ
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o
w
U1
CTi
-------
S0r)PZ.IK)G TR91U
STFICK
0 PURG6
punp
FIGURE AS
-------
PAGE 58
of the flasks were transferred to 4-ounce plastic sample bottles;
each flask and tee was rinsed twice with distilled water and
the rinse added to the sample bottle. The collection efficiency
was above 98 percent, and the precision was + 5 percent.
Moisture
Moisture tests were performed through the use of a Panametrics
Model 2000 hygrometer. The hygrometer is a sensitive instrument
for measurement of water vapor pressure that utilizes an aluminum
oxide probe placed inside a stainless case through which a con-
tinuous stream of sample gas is pulled. Each probe is individually
calibrated and comes with a curve of dew point versus meter reading.
Computation of moisture concentration is performed by measuring
gauge pressure of the gas stream and application toward a nomograph.
The accuracy is within 1 percent absolute error.
At the inlet location the positive pressure of the gas stream
pushed a sample through the probe holder, while a vacuum pump
was utilized at the outlet. A 1-hour conditioning period for
each test at each location assured that readings were not affected
by residual moisture in the holder.
Orsat
Orsat analyses were performed on-site. Samples were obtained
with two plastic 5-gallon leveling bottles. The bottles were
set at unequal levels with the higher filled with a dilute solution
of sulfuric acid/methyl red indicator while the lower bottle
remained empty. With a rubber tube from a stainless steel probe
inserted into the stack to the top of the higher bottle, the
solution was allowed to flow to the lower bottle. After a suitable
period of time, the tube ends were sealed and the sample analyzed
(see Figure A6).
-------
PAGE
59
STACK
FLUE 6A5 COLLECTION/ 6Y
LEVELING BOTTLE
GAS FLOW
Jill SAMPLE
ft 4 GA5
VENT
.IN
WATER
FLOW
ORSAT SAMPLE ANALYSIS
VENT
GAS FLOW
SAMPLE
-6 AS
ORSAT
FIGURE # A6
-------
PAGE 60
APPENDIX D
EXAMPLE CALCULATIONS FOR WET TESTS
(1) Weight of Component Found in Sample:
mg in sample = microliters of comp. x liters of liquid sample
liters of liquid sample
x specific gravity of component
(2) Parts per Million by Volume in Stack Gas:
ppm/V = mg in sample x 387 cu ft x 1 mole
std. cu ft dry gas sampled mole MW
x 1 Ib x 1
454,000 mg IQ-b
(3) Pounds per Hour in Stack Gas:
Ib/hr = mg in sample x Q x 60 min 1 Ib
std. cu ft dry gas sampled 1 hr 454,000 mg
where: Q = inlet flow rate as calculated by plant personnel
-------
APPENDIX E
SO? SUMMARY DATA (ENGLISH UNITS)
Date
2/4
2/4
2/5
2/5
2/5
2/5
2/5
2/6
2/6
2/6
2/6
2/6
2/7
2/7
2/7
2/7
2/7
2/8
2/8
2/8
2/8
2/8
Unit
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
Time
Start
1915
2345
0430
0930
1350
1855
2310
0345
0820
1330
1830
2330
0430
0930
1300
1830
2300
0330
0810
1240
1715
2145
Length
of Cycle
(hr)
4:30
4:45
5:00
4:20
5:05
4:15
4:35
4:35
5:10
5:00
5:00
5:00
5:00
3:30
5:30
4:30
4:30
4:40
4:30
4:35
4:30
4:30
ppm Avg
Inlet
2655
2335
2495
2400
2810
2535
2720
2795
3065
3045
3230
2980
2715
2600
2375
2495
2755
2610
2805
3330
3440
3290
Ib/hr Avg
Inlet
202.4
178.0
190.2
182.9
208.3
187.9
201.7
207.2
227.2
225.7
239.5
220.9
201.3
192.8
176.1
185.0
204.2
193.5
208.0
249.9
255.0
243.9
ppm Avg
Outlet
83
83
75
67
71
76
64
85
111
123
107
103
66
76
102
57
74
76
61
80
81
76
Ib/hr Avg
Outlet
6.33
6. 33
5.72
5.11
5.26
5.63
4.74
6.30
8.23
9.12
7.93
7.64
4.89
5.63
7.56
4.23
5.49
5.63
4.52
5.93
6.01
5.63
ppm Max
Outlet
147
144
132
111
138
144
126
165
183
207
195
192
129
135
120
123
141
153
144
162
138
135
Ib/cycle Ib/day Ib S02
Adsorbed Outlet ton acid
882.
815.
922.
800.
1015.
774.
886.
920.
1131.
1082.
1157.
1066.
982.
655.
927.
813.
894.
876.
915.
1118.
1120.
1072.
3
4
4 127.00 .79
1
2
6
3
8 188.26 1.18
3
9
9
3
1 133.44 .83
1
0
5
2
1 133.06 .83
7
2
5
2
TJ
O
-------
Date
2/9
2/9
2/9
2/9
2/9
2/11
2/12
2/12
2/12
2/12
2/12
2/13
2/13
2/14
2/14
2/14
2/14
2/14
2/15
2/15
2/15
2/15
2/15
Unit
A2
Al
A2
Al
A2
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
Time
Start
0215
0645
1115
1545
2015
2045
0115
0545
1015
1455
1930
0001
2245
0315
0745
1215
1650
2120
0155
0625
1100
1530
2000
Length
of Cycle
(hr)
4:30
4:30
4:30
4:30
4:05
4:30
4:30
4:30
4:40
4:35
4:30
4:30
4:30
4:30
4:30
4:35
4:30
4:35
4:30
4:35
4:35
4:30
4:40
SO? SUMMARY
ppm Avg Ib/hr Avg
Inlet Inlet
3080
3060
2750
2590
2605
2885
3090
3230
3460
2945
2745
2740
2780
2990
3065
3235
2960
2920
3250
3305
3335
3635
3545
228.3
226.9
203.9
192.0
193.1
213.9
229.1
239.5
256.5
218.3
203.5
203.1
205.5
221.1
336.6
239.2
218.9
215.9
240.3
244.4
246.6
268.8
262.1
DATA (ENGLISH
ppm Avg
Outlet
62
63
68
67
54
40
49
50
77
45
38
28
46
33
53
49
51
40
63
52
64
62
82
UNITS)
Ib/hr Avg ppm Max
Outlet Outlet
4.60
4.67
5.04
4.97
4.00
2.97
3.63
3.71
5.71
3.34
2.82
2.07
3.40
2.44
3.92
3.62
3.77
2.96
4.66
3.84
4.73
4.58
6.06
111
117
114
123
96
72
105
111
129
87
72
57
75
72
123
96
96
78
126
102
132
129
183
Ib/cycle Ib/day Ib S02
Adsorbed Outlet ton acid
1006
1000
894
841
772
949
1014
1061
1170
985
903
904
909
984
1002
1060
968
976
1060
1102
1108
1189
1194
.7 111.74 .70
.0
.9
.6
.2
.2 .45
.6 92.21 .58
.6
.4
.2
.1
.6
.5
.0 80.21 .50
.1
.1
.1
.0
.4 114.58 .72
.6
.6
.0
.9
>
O
w
to
-------
Date
2/16
2/16
2/16
2/16
2/16
2/16
2/17
2/17
2/17
2/17
2/17
2/18
2/18
2/18
2/18
2/18
2/19
2/19
2/19
2/19
2/19
2/20
2/20
2/20
Unit
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
Time
Start
0040
0515
0940
1415
1845
2315
0355
0820
1250
1730
2200
0230
0700
1130
1600
2030
0100
0550
1025
1455
1920
0001
0425
0900
-
Length
of Cycle
(hr)
4:35
4:25
4:35
4:30
4:30
4:40
4:25
4:30
4:40
4:30
4:30
4:30
4:30
4:30
4:30
4:30
4:40
4:35
4:30
4:35
4:40
4:25
4:35
4:30
S02 SUMMARY
ppm Avg Ib/hr Avg
Inlet
3460
3195
3300
3120
3360
3385
3145
2945
2810
-
-
4080
-
3510
3550
4130
4445
4495
4620
4490
4500
4245
Inlet
255.8
236.2
244.0
230.7
248.4
250.3
232.5
217.7
207.8
-
_
-
301.7
-
259.5
264.5
305.4
328.7
332.0
341.6
332.0
332.7
313.9
DATA (ENGLISH
ppm Avg
Outlet
71
62
53
56
54
67
50
55
51
85
67
78
64
94
94
64
54
97
84
113
98
110
87
97
Ib/hr
UNITS)
Avg ppm Max
Outlet Outlet
5.25
-
3.92
4.14
3.99
4.95
3.70
4.07
3.77
6.28
4.95
5.76
4.73
6.95
6.95
4.73
3.99
7.17
6.21
8.36
7.25
8.13
6.43
7.17
126
126
105
117
111
126
78
108
144
162
126
165
135
192
135
120
117
195
153
213
174
198
162
183
Ib/cycle Ib/day Ib S02
Adsorbed Outlet ton acid
1148.4 107.32 .67
1023.0
1100.4
1019.5
1099.8
1145.0
1010.5 109.30 .68
961.3
952.1
_
-
139.78 .87
_
1326.4
1146.5
1215.7 158.30 .99
1366.9
1451.2
1483.3
1560.3
1430.4 155.76 .97
1495.4
1380.3
T3
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O
tfl
^^
-------
Date
2/20
2/20
2/20
2/21
2/21
2/21
2/21
2/21
2/22
2/22
2/22
2/22
2/22
2/23
2/23
2/23
2/23
2/23
2/23
2/24
2/24
2/24
2/24
2/24
Unit
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
Al
Al
A2
Al
A2
Al
A2
Al
Time
Start
1330
1805
2230
0305
0735
1200
1640
2110
0140
0630
1045
1520
1950
0020
0455
0930
1400
1830
2305
0330
0810
1210
1815
2215
Length
of Cycle
(hr)
4:35
4:25
4:35
4:30
4:25
4:40
4:40
4:30
4:50
4:15
4:35
4:30
4:30
4:35
4:35
4:30
4:30
4:35
4:25
4:40
4:00
6:05
4:00
3:55
SO
ppm Avg
Inlet
4215
4065
3980
3750
3700
3645
4000
3980
3915
3870
3830
4205
4270
4005
4170
4250
4164
4255
4200
4105
4540
-
4500
4700
2 SUMMARY
Ib/hr Avg
Inlet
318.1
306.8
300.4
283.0
279.3
275.1
301.9
300.4
295.5
292.1
389.1
317.4
322.3
302.3
314.7
320.8
314.4
321.7
317.0
309.8
342.7
-
339.7
354.8
DATA (ENGLISH UNITS)
ppm Avg
Outlet
75
89
64
72
59
75
70
87
67
81
64
112
80
97
70
109
73
91
74
99
91
130
72
114
Ib/hr Avg
Outlet
5.66
6.72
4.83
5.43
4.45
5.66
5.28
6.57
5.06
6.11
4.83
8.45
6.04
7.32
5.28
8.23
5.51
6.87
5.59
7.47
6.87
9.81
5.43
8.60
ppm Max
Outlet
150
174
126
141
123
159
141
162
129
159
138
186
138
183
174
198
123
181
156
189
195
204
138
207
Ib/cycle Ib/day Ib S02
Adsorbed Outlet ton acid
1432.
1325.
1354.
1249.
1213.
1257.
1384.
1332.
1403.
1215.
1302.
1390.
1423.
1352.
1418.
1406.
1390.
1443.
1375.
1410.
1343.
-
1337.
1355.
0
4
7
1 131.47 .82
9
4
2
2
8 146.35 .91
5
9
3
2
0 155.20 .97
2
6
0
0
4
9 183.26 1.15
3
1
9
>
0
o
*
-------
SO2 SUMMARY DATA (ENGLISH UNITS)
Length
Time of Cycle ppm Avg Ib/hr Avg ppm Avg Ib/hr Avg ppm Max Ib/cycle
Date Unit Start (hr) Inlet Inlet Outlet Outlet Outlet Adsorbed
Ib/day Ib S02
Outlet ton acid
2/25
2/25
2/26
2/26
2/26
2/26
2/27
2/27
2/27
2/27
2/27
2/28
2/28
2/28
2/28
2/28
2/28
3/1
3/1
3/1
3/1
3/1
3/1
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
0210
0610
1010
1420
1835
2255
0305
0720
1140
1550
2010
0020
0435
0845
1300
1715
2130
0145
0600
1010
1415
1830
2245
4:00
4:00
4:10
4:15
4:20
4:10
4:15
4:20
4?10
4:20
4:20
4:15
4:10
4:15
4:15
4:15
4:15
4:15
4:10
4:05
4:15
4:15
4:15
4800
4645
-
-
_
-
4520
4020
3935
3930
4000
4075
4290
4420
4615
4275
4150
4100
4040
3765
4225
362.7
350.6
-
-
_
-
341.2
303.4
297.0
296.6
301.9
307.6
323.8
333.6
348.3
322.7
313.2
309.5
304.9
284.2
318.9
87
99
100
129
100
111
85
147
110
107
70
101
77
103
86
141
110
136
75
134
101
99
106
6.57
7.47
7.55
9.74
7.55
8.38
6.42
11.10
8.30
8.08
5.28
7.62
5.81
7.77
6.49
10.64
8.30
10.27
5.66
10.11
7.62
7.47
8.00
156
174
186
237
189
195
195
270
192
171
141
174
144
213
168
255
237
216
144
249
177
207
216
1424
1372
_
-
-
-
_
1387
1279
1264
1228
1233
1274
1348
1372
1445
1327
1281
1222
1263
1176
1321
.5
.5
.1
.7
.1
.2
.7
.3
.6
.6
.0
.8
.4
.5
.4
.1
.3
199.32 1.25
188.06 1.18
186.52 1.17
196.52 1.23
o
CTi
Ul
-------
S09 SUMMARY DATA (ENGLISH UNITS)
Length
Time of Cycle ppm Avg Ib/hr Avg ppm Avg Ib/hr Avg ppm Max Ib/cycle
Date Unit Start (hr) Inlet Inlet Outlet Outlet Outlet Adsorbed
3/2 Al 0300 4:15 4265 321.9 152 11.47 282 1319.3
3/2 A2 0715 4:15 4365 329.5 118 8.91 234 1362.5
3/2 Al 1130 4:30 4150 313.2 116 8.76 198 1370.0
3/2 A2 1600 4:20 4090 308.7 75 5.66 147 1313.2
3/2 Al 2020 4:05 3965 299.3 103 7.77 171 1190.4
3/3 A2 0025 4:20 4100 309.5 68 5.13 150 1318.9
3/3 Al 0445 4:00 3905 294.7 91 6.87 159 1151.3
Ib/day Ib S02
Outlet ton acid
204.34 1.28
O
-------
APPENDIX F
SO? SUMMARY DATA
Date
2/4
2/4
2/5
2/5
2/5
2/5
2/5
2/6
2/6
2/6
2/6
2/6
2/7
2/7
2/7
1/7
2/7
2/8
2/8
2/8
2/8
2/8
2/9
Time
Unit Start
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
1915
2345
0430
0930
1350
1855
2310
0345
0820
1330
1830
2330
0430
0930
1400
1830
2300
0330
0810
1240
1715
2145
0215
(METRIC UNITS)
Length
of Cycle ppm Avg kg/hr Avg ppm Avg kg/hr Avg ppm Max
(hr) Inlet Inlet Outlet Outlet Outlet
4:30
4:45
5:00
4:20
5:05
4:15
4:35
4:35
5:10
5:00
5:00
5:00
5:00
3:30
5:30
4:30
4:30
4:40
4:30
4:35
4:30
4:30
4:30
2655
2335
2495
2400
2810
2535
2729
2795
3065
3045
3230
2980
2715
2600
2375
2495
2755
2610
2805
3330
3440
3290
3080
91.
80.
86.
83.
94.
85.
91.
94.
103.
102.
108.
100.
91.
87.
79.
83.
92.
87.
94.
113.
115.
110.
103.
98
91
35
04
57
31
57
07
15
47
73
29
39
53
95
99
71
85
43
45
77
73
65
83
83
75
67
71
76
64
85
111
123
107
103
66
76
102
57
74
76
61
80
81
76
62
2
2
2
2
2
2
2
2
3
4
3
3
2
2
3
1
2
2
2
2
2
2
2
.87
.87
.60
.32
.39
.56
.15
.86
.74
.14
.60
.47
.22
.56
.43
.92
.49
.56
.05
.69
.73
.56
.09
147
144
132
111
138
144
126
165
183
207
195
192
129
135
120
123
141
153
144
162
138
135
111
kgS02/
kg/cycle kg/day metric
Adsorbed Outlet ton acid
400.6
370.2
418.8 47.66 .40
363.2
460.9
351.7
402.4
418.0 85.47 .59
513.6
491.6
525.7
484.1
445.9 60.58 .42
297.4
420.9
369.3
406.0
398.0 60.41 .42
415.7
507.7
508.7
486.8
457.0 50.73 .35
en
-------
S09 SUMMARY DATA (METRIC
Date
2/9
2/9
2/9
2/9
2/11
2/12
2/12
2/12
2/12
2/12
2/13
2/13
2/14
2/14
2/14
2/14
2/14
2/15
2/15
2/15
2/15
2/15
Unit
Al
A2
Al
A2
A2
Al
A2
Al
Al
Al
Al
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
Time
Start
0645
1115
1545
2015
2045
0115
0545
1015
1455
1930
0001
2245
0315
0745
1215
1650
2120
0155
0625
1100
1530
2000
Length
of Cycle
(hr)
4:30
4:30
4:30
4:00
4:30
4:30
4:30
4:40
4:35
4:31
4:50
4:30
4:30
4:30
4:35
4:30
4:35
4:30
4:35
4:30
4:30
4:40
ppm Avg
Inlet
3060
2750
2590
2605
2885
3090
3230
3460
2945
2745
2740
2780
2990
3065
3235
2960
2920
3250
3305
3335
3635
3545
kg/hr Avg
Inlet
103.01
92.57
87.17
87.67
97.11
104.01
108.73
116.45
99.11
92.39
92.21
93.30
100.38
102.88
108.60
99.38
98.02
109.10
110.96
111.96
122.04
118.99
ppm Avg
Outlet
63
68
67
54
40
49
50
77
45
38
28
46
33
53
49
51
40
62
52
64
62
82
kg/hr
UNITS)
Avg ppm Max
Outlet Outlet
2.12
2.29
2.26
1.82
1.35
1.65
1.68
2.59
1.52
1.28
.94
1.54
1.11
1.78
1.64
1.71
1.34
2.12
1.74
2.15
2.08
2.75
117
114
123
96
72
105
111
129
87
72
57
75
72
123
96
96
78
126
102
132
129
183
kgSOo/
kg/cycle kg/day metric
Adsorbed Outlet ton acid
454
406
382
350
430
460
482
531
447
410
410
412
446
455
481
439
443
481
500
503
539
542
.0
.3
.1
.6
.9
.6 41.86 .29
.0
.4
.3
.0
.7
.9
.7 36.42 .25
.0
.3
.5
.1
.4 52.02 .36
.6
.3
.8
.5
TJ
o
frt
G\
CO
-------
S02 SUMMARY DATA (METRIC UNITS)
Date
2/16
2/16
2/16
2/16
2/16
2/16
2/17
2/17
2/17
2/17
2/17
2/18
2/18
2/18
1/18
2/18
2/19
2/19
2/19
2/19
2/19
2/20
2/20
2/20
Unit
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
Time
Start
0040
0515
0940
1415
1845
2315
0355
0820
1250
1730
2200
0230
0700
1130
1600
2030
0100
0550
1025
1455
1920
0001
0425
0900
Length
of Cycle
(hr)
4:35
4:25
4:35
4:30
4:30
4:40
4:25
4:30
4:40
4:30
4:50
4:30
4:30
4:30
4:30
4:30
4:50
4:35
4:30
4:25
4:41
4:24
4:35
4:30
ppm Avg
Inlet
3460
3195
3300
3120
3360
3385
3145
2945
2810
-
3090
4080
-
3510
3550
4130
4445
4495
4620
4490
4500
4245
kg/hr Avg
Inlet
116.13
107.23
110.78
104.74
112.77
113.64
105.56
98.84
94.34
-
-
136.97
-
117.81
120.08
138.65
149.23
150.73
155.09
150.73
151.05
142.51
ppm Avg
Outlet
71
62
53
56
54
67
50
55
51
85
67
78
64
94
94
64
54
97
84
113
98
110
87
97
kg/hr Avg
Outlet
2.38
2.08
1.78
1.88
1.81
2.25
1.68
1.85
1.71
2.85
2.25
2.62
2.15
3.16
3.15
2.15
1.81
3.26
2.82
3.80
3.29
3.69
2.92
3.26
ppm Max
Outlet
126
126
105
117
111
126
78
108
144
162
126
165
135
192
135
120
117
195
153
213
174
198
162
183
RcsSO-)/
kg/cycle kg/day metric
Adsorbed Outlet ton acid
521
464
490
462
499
519
458
436
432
-
_
-
602
-
520
551
620
658
673
708
649
678
626
.4 48.72 .34
.4
.5
.19
.3
.8
.8 49.62 .34
.4
.3
63.46 .44
.2
.5
.9 71.87 .49
.6
.8
.4
.4
.4 70.72 .49
.9
.1
"0
>
O
m
ty\
V£>
-------
SO? SUMMARY
Date
2/20
2/20
2/20
2/21
2/21
a/al
2/21
2/21
2/22
2/22
2/22
2/22
2/22
2/23
2/23
2/23
2/23
2/23
2/23
2/24
2/24
2/24
2/24
2/24
Time
Unit Start
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
1330
1805
2230
0305
0735
1200
1640
2110
0140
0630
1045
1520
1950
0020
0455
0930
1400
1830
2305
0330
0810
1210
1815
2215
Length
of Cycle ppm Avg
(hr)
4:35
4:25
4:25
4:30
4:25
4:40
4:30
4:30
4:50
4:15
4:35
4:30
4:30
4:35
4:35
4:30
4:30
4:35
4:25
4:45
4:00
6:05
4:00
3:55
Inlet
4215
4065
3980
3750
3700
3645
4000
3980
3915
3870
3830
4205
4270
4005
4170
4250
4165
4255
4200
4105
4540
-
4500
4600
kg/hr Avg
Inlet
144.42
139.29
136.38
128.48
126.80
124.90
137.06
136.38
134.16
132.61
131.25
144.10
146.32
137.24
142.87
145.64
142.74
146.05
143.92
140.65
155.59
154.22
161.08
DATA (METRIC UNITS)
ppm Avg kg/hr Avg
Outlet
75
89
64
72
59
75
70
87
67
81
64
112
80
97
70
109
73
91
74
99
91
130
72
114
Outlet
2.56
3.05
2.19
2.47
2.02
2.57
2.40
2.98
2.30
2.77
2.19
3.84
2.74
3.32
2.40
3.74
2.50
3.12
2.54
3.39
3.12
4.45
2.47
3.90
ppm Max
Outlet
150
174
126
141
123
159
141
162
129
159
138
186
138
183
174
198
123
171
156
189
195
204
138
207
kgS02/
kg/cycle kg/day metric
Adsorbed Outlet
650
601
615
567
551
570
628
604
637
551
591
631
646
613
643
636
631
655
624
640
609
_
607
615
.1
.7
.0
.1 59.69
.1
.9
.4
.8
.3 66.44
.8
.5
.2
.1
.8 70.46
.9
.6
.1
.1
.4
.5 83.20
.9
.0
.6
ton acid
.41
.46
.49
.57
O
-------
Date
2/25
2/25
2/26
2/26
2/26
2/26
2/27
2/27
2/27
2/27
2/27
2/28
2/28
2/28
2/28
2/28
2/28
3/1
3/1
3/1
3/1
3/1
3/1
Time
Unit Start
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
Al
A2
0210
0610
1010
1420
1835
2255
0305
0720
1140
1550
2010
0020
0435
0845
1300
1715
2130
0145
0600
1010
1415
1830
2245
S0?
Length
of Cycle ppm Avg
(hr)
4:00
4:00
4:10
4:15
4:20
4.: 10
4:15
4:20
4:10
4:20
4:20
4:15
4:10
4:15
4:15
4:15
4:15
4:15
4:10
4:05
4:25
4:15
4:15
Inlet
4800
4645
-
-
_
-
4520
4020
3935
3930
4000
4075
4290
4420
4615
4275
4150
4100
4040
3765
4225
SUMMARY DATA (METRIC UNITS)
kg/hr Avg
Inlet
164.67
159.17
-
-
_
-
154.90
137.74
134.84
134.66
137.06
139.65
146.01
151.45
158.13
146.51
142.19
140.51
138.42
129.03
144.78
ppm Avg kg/hr Avg ppm Max
Outlet
87
99
100
129
100
111
85
147
110
107
70
101
77
103
86
141
110
136
75
134
101
99
106
Outlet
2.98
3.39
3.43
4.42
3.43
3.80
2.91
5.04
3.77
3.67
2.40
3.46
2.63
3.53
2.95
4.83
3.77
4.66
2.57
4.59
3.46
3.39
3.63
Outlet
156
174
186
237
189
195
195
270
192
171
141
174
144
2.13
168
255
237
216
144
249
177
207
216
kg/cycle kg/day
Adsorbed Outlet
646.
623.
__
_
-
_
629.
581.
573.
557.
560.
578.
612.
623.
656.
602.
581.
555.
573.
533.
599.
7
1
90.49
83.38
7
0
9
7 84.68
1
5
3
2
0
8 89.22
8
0
6
9
9
kgS02/
metric
ton acid
.62
.59
.58
.61
o
-------
Length
Time of Cycle
Date Unit Start (hr)
3/2 Al 0300 4:15
3/2 A2 0715 4:15
3/2 Al 1130 4:30
3/2 A2 1600 4:20
3/2 Al 2020 4:05
3/3 A2 0025 4:20
3/3 Al 0445 4:00
SO, SUMMARY DATA (METRIC UNITS)
ppm Avg kg/hr Avg ppm Avg kg/hr Avg
Inlet Inlet Outlet Outlet
4265 146.14 152 5.21
4365 149.59 118 4.05
4150 142.19 116 3.98
4090 140.15 75 2.57
3965 135.89 103 3.53
4100 140.51 68 2.33
3905 133.79 91 3.12
kgS02/
ppm Max kg/cycle kg/day metric
Outlet Adsorbed Outlet ton acid
282 599.0 92.77 .64
234 618.6
198 622.0
147 596.2
171 540.4
150 598.8
159 522.7
O
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to
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PAGE 73
APPENDIX G
STRIP CHART
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PAGE 74
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PAGE 75
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PAGE 76
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PAQE 77
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PAGE
STDP.OUTLEfT
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PAGE 79
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PAGE
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PAGE 81
CRSOOO/ilNLET
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84
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85
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86
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89
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90
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ca
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93
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95
C
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98
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PAGE 103
G
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PAGE 104
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M I ! i ! ; : i ! I i'
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118
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I I ' I Pi ! I I I ^f I VU* ' ' 1 I ' : I 1 I I I I . I ! I II
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PAGE 137
M : ' ' I
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139
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PAGE 183
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PAGE
192
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PAGE 193
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PAGE 194
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195
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PAGE
196
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198
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199
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-------
PAGE
200
! i T. ! I I I i J i .-.-./-H.! , I
-------
201
PAGE
APPENDIX H
RAW DATA SHEETS - WET TESTS
1) SC>2 Calibration Standards
2) S02/0rganic Sulfides
3) H2SO^ Mist/Organic Sulfides/S03
M-) Chloride/Total Acid
S) Nitrogen Oxides
6) Moisture
7) Orsat
8) Visible Emissions
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GAS SAMPLING FIEL2 DATA
- 227
Material Sampled for_
Date
Plant C. 0 0 CTb vp C H £"VH 'Location
Bar. Pressure <^/
15'-
"
METEK (Ft3)
'\}\".otff ' ' '
- /^-
III \)^-
'
»:
.
. .
1 FLOW METER
SETTING (CFM)
"'".: ,0V
' ',d^
' ''
.
METER TEMPERATURE
TM
3^
48- '--
' .
>' '
"
'
Comments
Impinger Bucket No,
Meter Box No.
-------
GAS SAMPLING FIELD DATA
JOB
Katerial Sampled far
JDate
Plant
' Location
Bar. Pressure" "25?.
Ambient Temp..
Run No. _ _ _
J'Hg Comments:
Power Staf^Setting ^5 '
Yes I/ No
Filter
Operator
CLOCK
TIME
)3^X
'(M^X
METER (Ft3)
// 3.070"
///;r^
»>
*
. FLOW METER
SETTING (CFM) -
' -.-,.(> 4
0^
'
-
METER TEMPERATURE
TM
q^
. JT"-
* ^ *
- 'x '
Comments:
Impinger Bucket No._
Meter Box No.
s
-------
GAS SAMPLING FIELD DATA
JOB ___
Material Sampled for M,
*""
jate
'PAGE .:.". 2:29
Plant crt
' Location
Bar. Pressure^
Ambient Temp._
Run
wHg Comments:
Power Stat Setting
Filter Used: Yes
Operator^
No
;".*_ _ .-v
:« .' . :' . ''
; . _ . .
'*:
CLOCK
TIME
/^
//30
....
METER (Ft3)
J/S.S'&O^ ' '"'
^ llt^lb
.
> -.
_
*
FLOW METER
SETTING (CFM) -
..-.-.
- '
METER TEMPERATURE
TM
2£ "
^o ' '-
' . - _»
- ''' '
-
Comments
Impinger Bucket
Meter Box No.
n
-------
GAS SAMPLING FIELD DATA
w
Haterial Sampled for
Date «
Plant
Location
Bar* Pressure^
Ambient Temp.^
Run No. I
Comments:
Power Stat Setting^
Filter Used: Yes_
Operator^
No
CLOCK
TIME
0^1
/^t
METER (Ft3)
ll.'bo
7/^,^0
»:
*
- FLOW METER
SETTING (CFM)
"in
\-n
- '
METER TEMPERATURE*
TM
</
-------
- -
JOB NO. y*f*/T?~ ifc.
Material Sampled fox_
~
Date
GAS SAMPLING FIELD DATA
f9jT ~'r
.
PAGE
Plant 0o u i Th»u (T
Location
Ki LPT
Bar. Pressure
Ambient Temp.
Run No.
nHg Comments:
Power Stat Setting_
Filter Used:
Operator
No
1
CLOCK
TIME
1030"
HOD
METER (Ft3)
fib-i'Zv:
-&%£ ;"!&'. * "
. - - ' - - . '
»>
... . . , ....
. FLOW METER
SETTING (CFM)
"./.2&
- 7. po
*
METER TEMPERATURE
TM
W
(f>O
-_..
'
->-.'
"
Comments:
Impinger Bucket No
Meter Box No.
-------
CAS SAMPLING FIELD DATA
JOB NO.
Material Sampled for
9
Date
A
PAGE 232
di)) ; #4
Plant
Location
Bar. Pressure
Ambient Temp._
Run No. _ _
"Kg Comments:
Power Stat Setting
Filter Used: Yes
Operator
No
CLOCK
TIME
^1.0
/2«r
METER CFt3)
fcU,MD
^?^,^
»;-
_
4
. FLOW METER
SETTING (CFM) -"
'..I- -7
I,'?
METER TEMPERATURE
TM
qu|
7^
'
. x ,
-Ji-" '
-
Comments:
Impinger Bucket
Meter Box No.
-------
JOB NO.,
Material Sampled for_
Date
GAS SAMPLING FIELD DATA
ftfcAES -.
;PAGE- 233
Plant
Bar* Pressure,
Ambient Temp._
Run No. ^
"Hg Ccxnments:
Power Stat Setting
Filter Used: Yes No
Operator
CLOCK
TIME
oaiir
NOOA
METER (Ft3)
^8-a.s.fe^
- 2>° *
>:-
_
. FLOW METER
SETTING (CFM)
'.'..;-' 1-6
l.O
METER TEMPERATURE
TM
48
. SO ' '.-.
'
-'-'' -
-
Comments :
Impinger Bucket No.
Meter Box No.
T> a C fit
-------
-. J«
GAS SAMPLING FIELD DATA
JOB
- 2.
Material Sampled for
Bate _ Z 6 75
PAGE''.234
Plant.
Bar* Pressure^
Ambient Temp._
Run No.
Location
» e» O
"Hg Comments:
Power Stat Setting «
Filter Used: Yes
Operator
CLOCK
TIME
CO|P
IOMB
^ ^JBL^
METER (Pt3)
3.802
&s.tf
jft
<
_
» \
- FLOW METER
SETTING (CFM)
1.6
1.6
METER TEMPERATURE
TM
4-ft
S?
*.
f ^ ' *
- '-' '
Comments:
Impinger Bucket
Meter Box No.
-------
GAS SAMPLING FIELD DATA
JOB NO..
Material Sampled for_
Date 1 6 "75
; PAGE. > 235
Bar. Pressure
Ambient Temp.
Location OU
"Hg Comments:
Fever Stat Setting_
Filter Used: Yes
Operate
CLOCK
TIME
1058
>r (^/^
METER (ptBj
5. foe.
66-66
''
*;.
. .... . .. .
.....'
' . .: ' ; .' ' ;:"
. FLOW METER
SETTING (CFM) -
1.6
METER TEMPERATURE
TM
48
5J
'.
- *s ' *
» *
Comments:
Impinger Bucket No,
Meter Box No.
-------
GAS SAMPLING FIELD DATA
JOB
Material Sampled fear
sate
Q
Plant
Bar. Pressure
Ambient Temp.
Run No. /_
Location
nHg Comments :
Power Stat Setting_
Filter Used: Yes__
.
Operator
No
'"PAGE.'.2 36:
JCLOCK
TIME
F*-"
Jl4^e
i'3S>
METER CFt3)
^i;°ivo .
in .^10-
fr>
'
_
*
. FLOW METER
SETTING (CFM)
.;
*
. ' :
ft
.
METER TEMPERATURE
TM
^o p - -
. 4o° -
^
->" ' . '
"
Comments:
Impinger Bucket No,
Meter Box No.
-------
JOB NO.
Material Sampled fear
GAS SAMPLING FIELD DATA
f ' ff)W?RA'L- ~
C
y ' - ' -.
('At*-MCrtJr' ' Location
Bar. Pressure -2*7, frQ
Ambient Temp. ^> 4
Run No.
Comments:
Power Stat Setting__
Filter Used: Yes -*
Operator ^ D , -/TS-
No
PAGE . 237
CLOCK
TIME
y^^o
\\^o
METE31 (Ft3)
^iiB, 600 " .
§^-540
, ... ,. . ... ... -.
>>
. '
.
. FLOW METER
SETTING (CFM) -
. . , , - . .
. ' - .
METER TEMPERATURE
TM
^6- . .
<"--
.
f-s ,
Comments;
Impinger Bucket No,
Meter Box No.
-------
GAS SAMPLING FIELD DATA
Material Sampled for.
>AGE 238
Plant
/i ' fy
yg~-
Bar. Pressure A//
Ambient Temp.
Run No.
Power Stat Setting
Filter Used: Yes
Opera tor t
.
_
«
. FLOW METER
SETTING (CFM) -
- . :
METER TEMPERATURE
TM
4\
. 44 ' '
** i» -
*' * *
- ^ " *
m
Impinger Bucket No._
Meter Box No.
-------
JOB
W. Cf
rial Sai
GAS SAMPLING FIELD DATA
Material Sampled for H *HcJ £-£ *K.. Y\<-+rG~'a JL Ac , "£> J
1 Plant
Location
l/T
Bar. Pressure^
Ambient Temp._
Run No* /
Comments:
Power Stat Setting
Filter Used:
Operator
Comments:
No
CLOCK
TIME
;y^
y^-D-
l
MEXER (Ft5)
"lixfoi' :
-)7Q>1ZO
....... . .... - . . .
-..- ..- -»;-
-
.. ...» ... . ... ... ... '
... . .......
-
. FLOW METER
SETTING (CFM)
hcf"
f
l^f^
*
METER TEMPERATURE
TM
*fi
£2
'
.- *
'
-
Impinger Bucket No,
Meter Box No.
-------
GAS SAMPLING FIELD DATA
NO.
Material Sampled for
S i~ ft\iAjf'#XL'-
Plant
CJ)a
' Location
Bar. Pressure
_^7,
Cooroents
Ambent Temp.
Run No.
Power Stat Setting_
Filter Used: Yes -
No
PAGE
.240
CLOCK
TIME
^ya
1Mb
'%' *
/*
"^j»
.' ^
/ A>
* ~
METER (Ft3)
-7 -71X^0
*££ 9f /;
»>
t«
^"
_
. FLOW METER
SETTING (CFM) -
'.'to
/,i)-
'
METER TEMPERATURE
TM
3'$*
6~v '
' . -
f- *
-** ' *
CcxTunents :
Impinger Bucket
Meter Box No.
-------
'AS SAMPLING FIELD DATA
Hater ial Sampled for A//4 lofry./ 4 /
''D5
PAGE-: 241
T
Plant
w /.. x-
. Pressure
AsubSent Tf-mn,
Fo" ' «' .c* S i : a t: S t.> 1 1 i. n $r
Filter Ucc.-d:
Operator CTf . -1 J?LM .'. ' ' '.'' " : ' - . ; > .".
"
CLOCK
TIME
'111?
/^
..,....,,,,
1 * -" '
METER (Ft3)
r'i ;'???'
.. - ....... . - . . ... .. '. . .,, , ... .-. .
«>>
.
.f : : . . '
. FLOW METER
SETTING (CFM) -
/,C)
'7.0
'.. , ... . ......
*
METER TEMPERATURE
TM
3?
54 ' '-
"* -M '
/:>''' -'
Cocnments:
Impinger Bucket No,
Meter Box No.
-------
PAGE .
242
OXIDEfL OF NITROGEN FIELD DATA
Job No.
Client
- a
Plant Location COU&.
Unit No.
TO
Sampling Location
Operator
Run Number
Date
Flask Number
Flask Volume Corrected (liters) (Vj?)
Initial Flask Vacuum(in.Hg) (Pi)
Final Flask Vacuum (in. Hg) (Pf
Flask Temperature (Tf)
% 02
I
«/*
22-
^,D«?
Slfl
^i4
4(»
t
V*
ro,
P,CHIfl
J5.)
-1,3
4tf
3
v^
^
7,00
W
/,-3
4.9
4
Vi
55-
AOK
M?
-^
40
5
Vi
Mb
0,0ft
25, fe
"-2.
^
6
vi
?
O.OiM
35.0
,s
^<9
ES-054
-------
PAGE 243
OXIDES OF NITROGEN FIELD DATA
Plant Location Cg>U^.TTQlL>
unit NO.
Sampling Location
Operator
Run Number """
Date
Flask* Number
32.
Z.7
FlaVk'Yolume Correcte'd (liters) (Vf)
a, OH i,
Initial Flask Vacuum(in.Hg) (Pi)
as
Final Flask Vacuum '(in. Hg) (Pf
-fe
-.6
-.3
Flask Temperature" (Tf)
4-0
40
40
% 02
6-0
6-0
fc.O
-0
.ES-054
-------
PAGE
244
OXIDES OF NITROGEN FIELD DATA
Job No.
Client
i3=.
Plant Location
Unit No.
Sampling Location
Operator_
Run Number
Date
Flask Number
Flask Volume Corrected (liters) (Vf)
Initial Flask Vacuum (in. Hg) (Pi)
Final Flask Vacuum(in.Hg) (Pf
r
Flask Temperature (Tf),
7" ,
% 02
*t
C
(
W
2_
X
/
^
?
*j'
/
»
l>^
>
/
\
\
^
dfes
3$
?t$
&l
/<0<
g
*/ar
10
3lM>
v <: /
25.3
/. 3
<0
'.
V
^,-
f?
?,o/7
Z3,j?
o
VO
5"B
.?»-
/
3,oi>/
' . '-.
23.2
'y
Vo
43
V^".;
^W ^
P,pP/
" '' ' (
^./
.O
V6
YORK
-------
PAGE "245
OXIDES OF NITROGEN FIELD DATA
Job No.
Client
Plant Location (_,£> 0
Unit No. V
( _
\\)
Sampling Location^
Operator ^ L U/1
70
Run Number
Date
Flask Number
Flask Volume Corrected (liters) (Vf)
^,077
Initial Flask Vacuum(in.Hg) (Pi)
Final Flask Vacuum (in. Hg) (Pf
3
Ci
.0
2-
Flask Temperature (Tf)
% 02
Vo
-------
sueer-
joe vo.
PAGE ?46
8//3/75"
INLET
' .210
OUTLSf hEU pQ/tJT- 6? ° C
MOISTUR6- /g
' S'
-------
wr/\ suetf-
J08 MO. "-""-"-* PAGE 247
owe- 3//4/V
. a
- ,i$o
/VIOISTU# - 20
QUTLgf HoisfuQZ* 4
-------
rieu*
sneer -
MT6-
INLET
ouTLer
,175"
C
- <$g°c
PAGE 248
- 3
-------
sueer-
PAGE '249
MOISTURE.
368 MO.
INLET
INLET
-------
sneer-
PAGE -250
Jog uo.
75-
INLET
,/gp
INLET
ouTLer
MO/STUM' /8
-------
sneer-
MT6-
INLET £fil~ . ZIP
- ,,/go
inter Q£v POINT-
MM pot/or-
MOISTURE ~
- 4__
f t
PAGE
-------
sneer -
- 0030-1000
- J0Q
INLET
OUTLSf
PAGE 252
-------
MT6'
inter
bfiT/\ sneer-
PAGE 253
MO.
INLET 6ADI- ,g/o
- ./#
-------
$08 NO. f-
PAGE 254
INLET D£U POltiT-
-------
PAGE .'255
JOB
ORSAT FIELD DATA
Location lNL&f - OUTLET
Date "<
Comments:
i
Time /5itO
Operator
Test
|N)L£T
OUTLET .
(C02)
Reading 1
3>S"
Z?l
(02)
Reading 2
7,2
i
6.0
(CO)
Reading 3
0,0
0,0
-------
PAGE '-256
JOB NO.
Location
Date
Time
nnti
Operator
ORSAT FIELD DATA
Comments:
Test
(C02)
Reading 1
(P2)
Reading 2
(CO)
Reading 3
0,0
-------
PAGE 257
ORSAT FIELD DATA
Location 1 NLtil * (jUI *" ' Comments:
Date "2J 6 / 7b
Time I'&OG
Operator v\
Test
||Ol£T
ajrczr
(C02)
Reading 1
^
^^
(02)
Reading 2
$.(,
7. -a
(CO)
Reading 3
O.o
0,0
CONTIOLLIO
-------
PAGE .258
JOB NO.
*''
- 2.
ORSAT FIELD DATA
Location_
Date 7>
Comments:
Time IC)3°
Operator
Test
II^L6^
OltfL£l
(C02)
Reading 1
4.7
4.8
(02)
Reading 2
^-3
£<$
(CO)
Reading 3
0,0
d.o
-------
PAGE 259
JOB NO.^gf7?'Z
ORSAT FIELD DATA
Location IML6T
Date <:
Time lied
Operator
Comments:
Test
IUL&C
ouf(£T
(C02)
Reading 1
4.$
4.1
(02)
Reading 2
r.e
5^7 '
(CO)
Reading 3
0.0.
0,0
-------
PAGE
DATA
Location
Date
"27 Z 7
Time
Operator
Comments:
Test
/A/lgT
ourfLBT
(C02)
Reading 1
3,g
3.^
C°2>
Reading 2
4,^
4 ?"
(CO)
Reading 3
0,0
0/0
-------
REPORT NO. Y-81*79-2
VKUfiL
PAGE" 261*
COMPANY NAME.
ENVIRONMENTAL PROTECTION AGENCY
L.
EQUIPMENT LOCATION ( ADDRESS).
TIME Of OBSERVATION: FROM
O *1 1 0
RECORD OF
VISIBLE EMISSIONS
tit "5 *'M'
//>giO PM
A.M.
M DATE
-
O
L_L I I I i._L_ULJL
% Mm. Qi 02 03 04 06 OS 07 08 09 10 11 12 13 14 15 16 I/ 18 19 20
i: 11 r"Ti'i iii I i. j i.ji. . i *' j i JTTI M n i li 11 iTni 111! rri i n 11 ntt
( I 1 i i ! I .
NOTE: Eech smjll square ropreor-nis :in moividual r"-jdii- of intensity corresponding to tiint shov.r, in !hn loft-hand column
over a time span o' 'i minute. I"1- '' «" ' S :n the top row of blank squares to indicnte the ?xftct minutu of the start of
observation. In the next square ;:':er ;' 3' . :nsr-n tha hour in which the measurement wns madiv Each paye of this form
CCn thus bo usod to record 1 r.our of nv.Tr.u'pmenls
-------
REPORT NO. Y-8479-2
PAGE .. 262
OUIHWD VI n" \fVt
Type of Air Conta
Point of Discharg
Point of Observat
Distance to Ba
Height of Poin
Background Descr
Weather: Clear
Wind C
iminants ^iL/^ *
0: Stack P\ Other
I
ion:
so of Point of Discharge, fee
t of Discharge Above Ground
iption G^F-A^r Ot/£&
Overcast 2S 1
)irection /^Af*/
<^0\ *- Hd'O yyrf>T
t
Level, feet ^,^0 / '
-(.sia/- cJ^Sy //& /?/so ^A/0*J"^JC
x
'art ly Cloudy Other ^/\/O^Ji^J^>
Wind Velocity, mi/hr \3"-5
Plume Description:
Detached: Yes [ | No
Color: Slack
White
Other
Plume Dispersion Behavior: Looping
Lofting
Coning
Fumigating
Fanning
See Comments
Estimated Distance (feet) Plume Visible (Maximum)
Comments
(Minimum)
7~0
Signed
Title
-------
REPORT NO. Y-8479-2
PAGE 26B
COMPANY NAME.
ENVIRONMENTAL PROTECTION AGENCY
/
EQUIPMENT LOCATION ( ADDRESS).
TIME OF OBSERVATION: FROM_
RECORD OF
VISIBLE EMISSIONS
29 '-) .11 3? 23 . 34 .lb 36 3' 38 39 40
Z^ttMtZttttM
NOTE: Each small srL:rer,rn!s 'in
over c timo span of 'i minute, ii's "i
observation, in thtv next squciro ufior !'-.
can thus 6c used io record 1 hoar of I'l'-.
iial ff-ading of ir.tonsity cor;csoonrimg to tb.ot shown in Ihc left-hand column
S 'in the to,-) tow of blank squares to indicntR the exfict minute of the start ot
msi-rr tho hour in which the meesurement was made. Each page of this form
-------
REPORT NO. Y-8479-2
'PAGE:26*
ENVIRONMENTAL PROTECTION AGENCY
COMPANY NAME.
EQUIPMENT LOCATION { ADDRESS).
TIME or OBSERVATION: FROM
3 A/,'.
RECORD OF
VISIBLE EMISSIONS
DATE
Mm. 01 02 03 04 05 06 07 08 09 10 11 12 13 14 15 16 \l 18 19 20
_%!!!!_ II. mH^itjjlL^ H ,ui|ii _ . i. !;,. 4. ;.r| 4 |4^^m.i 4^jjj-^.i^.......
NOTE: Fach small squarp rcprosonis ;m individual fading of intensiry cor.-Cr-tJor.c'mg lo thnt ?licv.p" in me left-hand column
Over a lime span o' !< minute. Ins '( ;<" "G ' i" the top row of blank squares to indicotn IMP exfict minute of the start of
observation. In the next square after i('" 3' . insert thci hour in whicli the mnDSurcmenl w«3 made. Each page o' thic form
CBn thus bo used to rtco.-d 1 hour of pv.v.u'pmeris
-------
REPORT NO. Y-8479-2
PAGE
265
Source of Air Contaminants
Type of Air Contaminants
/&*=/ s»'
Point of Discharge: Stack
Other
Point of Observation:
Distance to Base of Point of Discharge, feet
Height of Point of Discharge Above Ground Level, feet
Background Description Cr? ^-^j/ -=^n/
Weather: Clear
Overcast
Partly Cloudy
Other
Wind Direction
Wind Velocity, mi/hr
Plurne Description:
Detcched: Yes \ ! No
Color; Black
White
Other
Plume Dispersion Behavior: Looping
Lofting
Coning
Fumigating
Fanning
See Comments
Estimated Distance (feet) Piume Visible (Maximum)
Comments
(Minimum)
Signed /^^fkfc^
Title
-------
REPORT NO. Y-8479-2
PAGE . 266
ENVIRONMENTAL PROTECTION AGENCY
COMPANY NAME.
EQUIPMENT LOCATION ( ADDRESS).
TIME OF OBSERVATION: FROM ,/£
RECORD OF
VISIBLE EMISSIONS
A.M.
.P.M.
A.M.
IP.M. DATE
Mm. 01 C2 03 04 05 06 (17 03 09 10 11 12 13 14 15 16 I/ 18 19 20
ffiffiffiffi
^444^+414+4. -j-H-H-K -W- iff- --H4
n^^5P5ttiITTi -m- I:I t^
t_M-Tf ^-(-,44. -L ^0-M . - -U. - - i J t.- .-i. i.r
P^jJip;Tf[i]5^^^
UM-l-^J-t-U* »i-,.j-U-;-4-u4.i-
NOTE: Eech snail squdre rpprei-'nis in "ir;ividu3! f??.')ing of irlonsity corresponding 10 ii nt shown in ihe left-hand column
Over a timo span o' 'i minute. In; -i ;m ' 3" in ihc !op row of blank squares to indicnle the exfict minutfi of tho start of
observation. In the next sciuaic .Tie" I'v j . insert t^c tiour in whicli the mftascrertieiit w;i3 niarie. Each page of this form
can thus be used to record 1 hour of i!v-,ir.ot."N!ei!;s.
-------
REPORT NO. Y-8479-2
PAGE 267
Source of Air Contaminants
Type of Air Contaminants
*/
Point of Discharge: Stack
Other
Point of Observation:
Distance to Base of Point of Discharge, feet
Height of Point of Discharge Above Ground Level, feet
Background Description
Weather: Clear | | Overcast
Partly Cloudy
Other
Wind Direction
Wind Velocity, mi/hr
Plume Description:
Detached: Yes | | No
White
Color: Black | |
Other
Plume Dispersion Behavior: Looping
Coning
Lofting | ( Fumigating
Fanning
See Comments
Estimated Distance (feet) Plume Visible (Maximum)
Comments
(Minimum)
Signed
Title ^+J".
-------
REPORT NO. Y-8479-2
PAGE
268
ENVIRONMENTAL PROTECTION AGENCY
COMPANY NAME.
EQUIPMENT LOCATION ( ADDRESS).
»EC ORD OP
VISIBLE EMISSIONS
*'M'
TIME or OBSERVATION: FROM
>» f ' "=
-------
REPORT NO. ₯-8479-2
PAGE 269
Source of Air Contaminants
*J-£/
Type of Air Contaminants.
Point of Discharge: Stack
Other
Point of Observation:
Distance to Base of Point of Discharge, feet
Height of Point of Discharge Above Ground Level, feet
Background Description
& ^
Weather: Clear
Overcast
Partly Cloudy
Other
Wind Direction ^.
Wind Velocity, mi/hr
Plume Description:
Detached: Yes | |
Color: Black
White
Other
Plume Dispersion Behavior; Looping
Lofting
Coning
Fumigating
Fanning
See Comments
Estimated Distance (feet) Plume Visible (Maximum)
Comments
(Minimum)
?
Signed
Title
-------
REPORT NO. Y-8479-2
PAGE
270
///,
ENVIRONMENTAL PROTECTION AGENCY
COMPANY NAME
EQUIPMENT LOCATION (ADDRESS).
£""
RECORD OF
VISIBLE EMISSIONS
TIME OF OBSERVATION: FROM
LL.I \ \ L\ \
01 02 03 04 05 06 07 08 09 10
L.TTT]
U.U-:,-. . i.!!'. I ; | I !
I ' i i i i ; I i i I T . ri T i i T: r
NOTE: Each small square represftnts -'in individual reading of ir.tensity conesponcimg lo that snovin in the left-hand columi
over a time span of '.', minute Ins "i an ' S" in the top row of blank squares to indicnti; tip? t-xfict minute of the start of
observation. In the next square after thf 3' . insert the hour in which the measurement was made. Each page of this form
COn thus be used to record 1 hour of nvnsurpments.
-------
REPORT NO. Y-8479-2
PAGE
Source of Air Cwuaminants
Type of Air Contaminants _c
Point of Discharge: Stack
Other
Point of Observation:
Distance to Base of Point of Discharge, feet
Height of Point of Discharge Above Ground Level, feet
Background Description
Weather: Clear! | Overcast
Partly Cloudy
Other
Wind Direction ^O^
Wind Velocity, mi/hr /£> ~/I
Plume Description:
Detached: Yes | | No I I
Color: Black
White
Other
Plume Dispersion Behavior: Looping
Lofting
Coning
Fumigating
Fanning
See Comments
Estimated Distance (feet) Plume Visible (Maximum)
Comments
(Minimum)
Signed
Title
-------
REPORT NO. Y-8479-2
COMPANY NAME
AGE
ENVIRONMENTAL PROTECTION AGENCY
EQUIPMENT LOCATION ( ADDRESS).
5
TIME OF OBSERVATION:
°*.nmg to tl-nt sliov.n in me lefl-hanjj co'umn
r.ii'iu!'.1. IO'B -i »in "S'
-------
REPORT NO. Y-8479-2
PAGE _.2.73
Source of Air Contaminants
Type of Air Contaminants.
Point of Discharge: Stack
Other
Point of Observation:
Distance to Base of Point of Discharge, feet
Height of Point of Discharge Above Ground Level, feet
Background Description
Weather: Clear
Overcast
Partly Cloudy
Other
Wind Direction
Wind Velocity, mi/hr
Plume Description:
Detached: Yes | j No I I
Color: Black
White
Other
Plume Dispersion Behavior; Looping
Lofting
Coning
Fumigating
Fanning
See Comments
Estimated Distance (feet) Plume Visible (Maximum)
Comments
(Minimum).
L/s
'
SigncxJ
Title
-------
REPORT NO. Y-8M79-2
PAGE. 274
COMPANY NAME.
ENVIRONMENTAL PROTECTION AGENCY
L.
EQUIPMENT LOCATION ( ADDRESS).
TIME OF OBSERVATION: FROM _£.'
S° 4 ^
C/t/' °
RECORD OF
VISIBLE EMISSIONS
11 12 13 14 15 16 \! 18 19 20
32 33 . 34 .15 36 37 38 39
(>X)7E: Each small square rep'poonts .'in individual trading of intensity corresponding to thnl shown in ihe le'l-Hand column
ovor s time spar, o' "* minut'j Ins "t .m "S" in the top row of blanc. s'luares to indicnin (lie exfict minote nt tha si-jrt of
obsorvction. In the next sguaie .'jfier inv a . insert tho hour in which ihe .-nnasurement W.TS made. Each page; of this 'onn
CSR t!ius bo usod to record 1 hour of Mi'-ir-u'r-rnerits.
-------
REPORT NO. Y-8479-2
PAGE 275
Source of Air Contaminants
Type of Air Contaminants
Point of Discharge: Stack V\
Point of Observation:
Distance to Base of Point of Discharge, feet
Height of Point of Discharge Above Ground Level, feet
Background Description (->£./»'/ <£>^Y
yo A.
Weather: Cie?r
Overcast
Partly Cloudy
Other
Wind Direction
Plume Description:
Del^cfiod: Yes L I
Color: Black
Wind Velocity, mi/hr >
"o
White
Other _./l/g>A/C
Plume Dispersion Behavior. Looping
Lofting
Coning
Fumigating
Fanning | I
See Comments
Estimated Distance (feet) Plume Visible (Maximum)
Con-jnents
(Minimum)
7
-k IK nther
C«
-------
REPORT NO. Y-8479-2
PAGE.274
COMPANY HAMC.
ENVIRONMENTAL PROTECTION AGENCY
L.
EQUIPMENT LOCATION
TIME OP OBSERVATION; FROM.
RECORD OF
VISIBLE EMISSIONS
SW/hOUT
n. NO.
D
4M
4J4
4«
4
3K
3»
3K
3
2H
254
2'-*
2
1H
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IX
t
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ti
U
0
1
% Mm. 01 02 03 04 OS 06 07 08 09 10 11 12 '3 14 IS
100, ,
95
90 (1 '
85
80
75
70
65 1
60
55
so ' '
45
40
35 !
30 ,
25 1
20 ' ~ T
15 '
10
0 jlSUA v* 'at"
S"»'«/hour
n. NO.
6
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41,.
4%
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too
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90
85
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75 ! ' i '; |
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MOTE: Each small square represents ;m individual rrading of iriensity corrcfpcr.o'mg to that shov.n in the left-hand oo'umn
Over a time span O' "* minute. Inst nn "SP in the top row of blanK squares to iodicotn the exSct minute ot the siart of
observ&tion. In the next square after ihv 3' . insert the hour in which the measurement was made. Each page of this form
C9P. thus be used to reco.'U 1 hour o' ni-ar-uipments.
-------
REPORT NO. Y-8479-2
PAGE
277
Source of Air Contaminants
Type of Air Contaminants
-So*
x/. / . ... /
Pcint of Discharge: Stack
Other
Point of Observation:
Distance to Base of Point of Discharge, feet
Height of Point of Discharge Above Ground Level, feet
Background Description
&/***-
Weather: Clear LAI Overcast
Wind Direction
Partly Cloudy I I Other
Wind Velocity, mi/hr /*
Plume Description:
Detached: Yes j j No' '
Color: Black
White
Other
Plume Dispersion Behavior: Looping
Lofting
Coning
Fumigating
Fanning
See Comments
Estimated Distance (fest) Plume Visible (Maximum)
Comments XUo
(Minimum)
/?t*>
sa
£7< /Z. g,C/^
//
'r'r' ""
<' -n^
itiO
-------
REPORT NO. Y-8479-2
PAGE
ENVIRONMENTAL PROTECTION AGENCY
COMPANY NAME.
EQUIPMENT LOCATION ( AOORESSL
in.
TIME OF 03SERVATIONI
. Q/v/o
necopo OF
VISIBLE EMISSIONS
P.M. TO
p.M. PATE
M 15 16 t; 19 19 20
iip
:
.
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' M -
n T i r I'l '<' > 'i *: T, 11
^<
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r«"07E: Eflch si-.all ;qu
-------
REPORT NO. Y-8479-2
PAGE
Source of Air Contaminants
Type of Air
Point of Discharge: Stack
Other
Point of Observation:
Distance to Base of Point of Discharge, feet
16 o A"
Height of Point of Discharge Above Ground Level, feet
Background Description
Weather: Clear
D
Overcast
I/S
Partly Cloudy
Other
Wind Direction
Wind Velocity, mi/hr
/O ^ /Z
Plume Description:
Detached: Yes j j No j \
Color: Black!
White
Other
Plume Dispersion Behavior: Looping
Lofting
Coning
Fumigating
Fanning
See Comments
Estimated Distance (feet) Plume Visible (Maximum)
Comments
(Minimum)
ix C f; r
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing}
1. REPORT NO.
EPA-600/2-76-047
2.
3. RECIPIENT'S ACCESSION-NO.
4. TITLE AND SUBTITLE
Molecular Sieve Tests for Control of Sulfuric
Acid Plant Emissions
5. REPORT DATE
March 1976
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Karl R. Boldt and Richard F. Timmons
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING OR6ANIZATION NAME AND ADDRESS
York Research Corporation
One Research Drive
Stamford, Connecticut 06906
10. PROGRAM ELEMENT NO.
1AB014-ROAP 21ADH-006
11. CONTRACT/GRANT NO.
68-02-1401, Task 2
12. SPONSORING AGENCY NAME AND ADDRESS
EPA, Office of Research and Development
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
Task Final; 9/74-12/75
14. SPONSORING AGENCY CODE
EPA-ORD
15. SUPPLEMENTARY NOTES
Project officer for this report is E. J. Wooldridge, Ext 2547.
16 ABSTRACT The report gives results of tests of a molecular sieve control system for
sulfuric acid plant tail gas. The system, the PuraSiv S, was developed by Union
Carbide Corporation and is now operating at the Coulton Chemical Corporation's
plant in Oregon, Ohio. The PuraSiv S utilizes a molecular sieve adsorbent material
that releases SO2 when heat is applied. The SO2 is recycled for an additional 2-3%
production of acid. The report evaluates the PuraSiv S, using data gathered during
a 4-week test period. SO2 concentrations were continuously measured and recorded
by a DuPont 460/1 Photometric Gas Analyzer at both the inlet and outlet gas streams.
Average removal efficiency was 98.0%. Average SO2 emissions during the tests
were below 100 ppm.
7.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
Air Pollution
Sulfuric Acid
Chemical Plants
Absorbers (Materials)
Surlfur Dioxide
Adsorption
b.IDENTIFIERS/OPEN ENDED TERMS C. COSATI Field/Croup
Air Pollution Control
Stationary Sources
Molecular Sieves
Tail Gas
PuraSiv S
13B
07B
07A
11G
8. DISTRIBUTION STATEMENT
19. SECURITY CLASS (This Report)
Unclassified
21. NO. OF PAGES
280
Unlimited
20. SECURITY CLASS (This page)
Unclassified
22. PRICE
EPA Form 2220-1 (9-73)
280
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