74-LIM-3B
(REPORT NUMBER)
AIR POLLUTION EMISSION TES
WOODVILLE LIME AND
(PLANT NAME;
CHEMICAL COMPANY
WOODVILLE, OHIO
(PLANT ADDRESS)
U. S. ENVIRONMENTAL PROTECTION AGENCY
Office of Air and Water Programs
Office of Air Quality Planning and Standards
Emission Standards and Engineering Division
Emission Measurement Branch
Research Triangle Park, N. C. 27711
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PEDCo-EN VI RON MENTAL
SUITE13 ATKINSON SQUARE
CINCINNATI, OHIO 45246
513 1-7-7 1-433O
EMISSION TESTING REPORT
EPA REPORT 74-LIM-3-B
WOODVILLE LIME AND CHEMICAL CO,
WOODVILLE, OHIO
Contract No. 68-02-0237
Task 26
Submitted by:
PEDCo-Environmental Specialists, Inc,
13 Atkdnson Square
Cincinnati, Ohio 45246
Prepared by:
W. G. DeWees
Richard W. Gerstle, P. E,
September 16, 1974
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1. TABLE OF CONTENTS
Page
II. 'INTRODUCTION 1
III. SUMMARY OF RESULTS 3
IV. PROCESS DESCRIPTION 9
V. LOCATION OF SAMPLING POINTS 12
VI. PROCESS OPERATION & TEST CONDITIONS 14
VII. SAMPLING AND ANALYTICAL PROCEDURES 19
A. PARTICULATE RESULTS AND EXAMPLE CALCULATIONS
B. GASEOUS RESULTS AND EXAMPLE CALCULATIONS
C. VISIBLE EMISSIONS RESULTS
D. OPERATING RESULTS
E. FIELD DATA
F. SAMPLE IDENTIFICATION LOG
G. LABORATORY REPORT
H. SAMPLING EMTHODS
I. TEST LOG
J. RELATED REPORTS
K. PROJECT PARTICIPANTS
L. SUMMARY OF TESTING COSTS
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II. INTRODUCTION
Under the Clean Air Act of 1970, as amended, the Environ-
mental Protection Agency is charged with the establishment of
performance standards for stationary sources which may contri-
bute significantly to air pollution. A performance standard is
based, on the best emission reduction systems which have been
shown to be technically and economically feasible.
In order to set realistic performance standards, accurate
data on pollutant emissions must be gathered from the stationary
source category under consideration.
Woodville Lime and Chemical Co. in Woodville, Ohio, was
designated as a possible representative well-controlled
stationary source in the lime production industry and therefore
was selected for an emission testing program. The process under
investigation in this test series was operation of the No. 1 lime
kiln at the Woodville plant, from which emissions are controlled
by a cyclone in series with a Buell electrostatic precipitator.
Preliminary tests were performed during the week of May 20,
1974, to ascertain composition and velocity of the gas stream
and to observe visible emissions.
The emission test program was conducted from July 8 to 10,
1974; on three test runs. Sampling was done at the kiln stack to
determine concentrations of filterable and total particulate,
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oxides of nitrogen, and sulfur dioxide. Determinations of
moisture content and dry molecular weight were performed
simultaneously. Samples of the kiln feed, kiln product,
kiln fuel, and effluent dust from the ESP unit were collected
for calculation of a sulfur balance. In addition, visible
emissions were recorded by two certified observers during this
time. Because of difficulties with process operation and
above-normal production rates, further tests were scheduled
for August 5, 1974. In the interim between test periods the
kiln was shut down, at which time.the ESP was cleaned and
inspected.
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III. SUMMARY OF RESULTS
Data on particulate emissions from the lime kiln are
summarized in Table 1. Emissions of filterable particulate,
as measured by the probe and filter catch, averaged 9.77
pounds per hour at a concentration of 0.041 grain per DSCF.
Total particulate emissions averaged 18.3 pounds per hour
at a concentration of 0.077 grain per DSCF. Emissions of
filterable particulate were higher in the first two tests
than in the third. This can probably be attributed to discon-
tinuity in process operations and to problems with control
equipment, described in Section IV, "Process Operation".
Because of these difficulties, the emissions data reported
in this report are considered questionable with respect to
being representative of a well-controlled lime-producing
process.
Data on oxides of nitrogen emissions are summarized
in Table 2. These data show an average concentration of
339 ppm by volume and an hourly emission rate of 67.7 pounds
per hour of N02.
Data on sulfur dioxide emissions are summarized in Table
3. These data show an average concentration of 44.5 ppm
by volume and an hourly emission rate of 12.0 pounds per
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Table 1. SUMMARY OF PARTICULATE DATA
Run Number
Date
Volume of Gas Sampled , DSCFa
Average Stack Temperature , °F
Percent Moisture by. Volume , %
Stack Volumetric Flow Rate, DSCFM
Stack Volumetric Flow Rate , ACFMC
Percent Isokinetic
Unit Production Rate, ton/hr
Particulates - probe, bypass, and
filter catch
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton
Particulates - total
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton
1
7/8/74
237.923
621
11.3
27619
64393
102.9
781.1
0.051 .
0.022
12.0
1704.6
0.111
0.047
26.2
3_
7/9/74
239.642
669
12.1
27390
67296
104.5
718.9
0.046
0.019
10.9
989.9
0.064
0.026
15.0
5_
7/10/74
248.641
674
11.4
28658
70330
103.6
417.0
0.026
0.011
6.4
Vs
889.3
0.055
0.022
13.6
Avg'.
242.07
655
11.6.
27889
67340
140
639
0.041
0.017
9.77
;
1194.6
0.077
0.032
18.3
Dry standard cubic feet at 70°F, 29.92 in Hg.
b Dry standard cubic feet per minute at 70°F, 29.92 in. Hg.
Actual.cubic feet per minute.
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Table 2. SUMMARY OF OXIDES OF NITROGEN DATA
NOx Test No.
Date, 1974
Time, 24 hour clock
Flow Rate, DSCFM3
Sample Volume , ml
Milligrams of NO-
NOX Concentration,
N0x Ib/hr
Average ppm
Ib/hr
A
7/8
1748
27619
1457
0.83
ppm 299
58.9
B
7/8
1848
27619
1521
0.672
232
45.6
C
7/8
1951
27619
1519
0.953
329
64.8
299
D
7/8
2048
27619
1495
0.957
336
66.1
58.85
E
7/9
915
27390
1554
0.976
330
64.4
F G
7/9 7/9
1015 1115.
27390 27390
1549 1487
0.934 1.034
316 364
61.8 . 71.3
339.75
66.45
H
7/9
1215
27390
1522
1.014
349
68.3
I
7/10
920
28658
1602
1.093
358 .
73.2
J K
7/10 7/10
1033 1130
28658 28658
1938 1616
1.169 1.349
316 438
64.7 89.5
380
77.67
L
7/10
1230
28658
1660
1.290
408
83.3
Average
339.58
67.66
(jt
a) Dry standard cubic feet per minute, corrected to 70° and 29.92" Hg as obtained during particulate test runs.
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Table 3. SUMMARY OF SULFUR DIOXIDE DATA
Test No.
Date, 1974
Flow rate,DSCFMa
Sample volume, DSCFa
S02 in sample, grams
SO- emissions, Ib/hr
S02 concentration, ppm
by volume
2
7/8
27619
166.917
0.867
19.1
70.-2
4
7/9
27390
165.549
0.130
2.42
10.6
6 Avg.
7/10
28658
166.705
0.649
14.4 12.0
52.6 44.5
a) Dry standard cubic feet at 70°F 29.92 in. Hg.
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hour of sulfur dioxide.
Visual determination o-f the opacity of emissions from
the lime kiln exit stack was performed independently by two
PEDCo personnel. Data on opacity measurements are summarized
in Table 4. The average opacity was less than 5 percent
in all tests. A period of high emissions occurred, however,
for about 1 minute in the first test, during which opacity
levels exceeded 20 percent. Failure of a field in the electro-
static precipitator caused the discontinuity,.with the result
that the opacity values are not considered typical of those
occuring with well-controlled lime-production operations.
During sample recovery on test 1, the probe glass liner
tip was found to be broken. This test was therefore not
representative of true emissions. Because of the higher
than expected opacity and various process problems, this
test series was terminated before enough measurements were
obtained to provide representative results.
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No.
Date
Table 4. SUMMARY OF VISIBLE EMISSION DATA
' ! 1
7/8/74 ' 7/9/74
Obs. 1 . Obs. 2 . Obs. 1 . Obs. 2
Interval of Observations start
-. -End
Duration of Observation, min
Total No. of Readings
No. of Readings Unobservable
No. of Readings @ 0% Opacity
5%
.10% '
15%
20%
25%.
30%
' . 35%
40%
45%
. 50%
Percent Readings Unobservable
Percent Readings @ 0% Opacity
5%
10%
15%
20%
Percent Readings Exceeding 20%
24-hour clock start and end times
b
Excluding the time that readings were not recorded'for period of observation.
c
Readings recorded at 15-second intervals unless otherwise noted.
Observer 1 - R. S. Amick
Observer 2. - w. G. DeWees
8
5.
7/10/74
Obs..1 , Obs. ?
1715
2124
247
988
0
986
2
^^
_
»
^
_
_
_
_
0
99.8
0.2
-
_
1713
2112
228
912
. 10
711
184
7
_
_
__
M
_
0.8
78.0
20.2
-
. _
840
1245
245
980
0 .
914
34
26
3
3
_
_
_
.
0
93.3
3.5
2.6
0.3
0.3
.
843
.1235
233
932
154
174
597
7
_
»
»
^ ,
_
_
_
M
16 . 5
18.7
64.1
0.7
-
_
820
1252
272
1088
0
1061
21
5
1
H
_
«.
_
0
97.5
1.9
0.5
0.1
_
838
1239
212.5
850
0
782
66
1
1
^
mu
, ^^
^
_
_
0
92.0
7.8
0.1
0.1
_
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.IV. PROCESS DESCRIPTION
. Limestone consisting primarily of calcium carbonate or combina-
tions of calcium and magnesium carbonate with varying amounts of
impurities is quarried at the Woodville Plant. The limestone is
calcined or burned to form lime, commonly divided into two basic pro-
ductsquicklime and hydrated lime. Calcination expels carbon
dioxide from the raw limestone, leaving calcium oxide (quicklime).
With the addition of water, calcium hydroxide (hydrated lime) is
formed.
The basic processes in production are: (1) quarrying the lime-
stone raw material, (2) preparing the limestone for kilns by crushing
and sizing, (3) calcining the limestone, and (4) optionally processing
the quicklime further by additional crushing and sizing followed by
hydration. The majority of lime is produced, in rotary kilns which
can be fired by coal, oil, or gas. Rotary kilns have the advantage
of producing high production per man-hour and a more uniform product.
However, they do require higher capital investment and unit fuel
costs than most vertical kilns.
The Woodville Lime and Chemical plant has two rotary kilns
each equipped with a Buell electrostatic precipitator. The kilns
are almost identical. The feed for both is a dolomitic stone,
quarried on the site and fed in sizes ranging from 1 inch to
2 1/4.inches at a rate of about 700 tons per day. There is no
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preheater. Normally the kiln is fueled with a mixture of
95 percent Number 6 fuel oil .and 5 percent natural gas. Both
kilns have two heat transfer sections, each 20 feet long. The
product, about 350 tons per day, is,cooled in a Neims cooler before
storage. There is no product crushing, but undersize material
is separated and returned to the kiln. The majority of the
product.is used in the steel industry, mostly in basic oxygen
furnaces; none of the product is hydrated.
The electrostatic precipitator on kiln Number 1 was put in
operation in July 1971. In this kiln the main process fan is
located before the ESP, with a cyclone before the fan to reduce
fan blade erosion. The precipitator on kiln Number 2 was put in
operation in December 1973. The main process fan is after the
ESP and there is no cyclone.
In both systems the inlet gas to the precipitators is cooled
to about 600°F with a combination of water injection and/or
tempering air. Each precipitator has 28,800 square feet of
collecting surface area, which includes one cell and two fields;
design gas velocity is 1.5 feet per second and treatment time,
10.0 seconds. The plant manager reported that an earlier
emission test showed exit loadings of less than 0.005 grain
per dry standard cubic foot.
At present the dust collected from the precipitators is
disposed of in the quarry... It is expected that in the future the
10
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dust will be granulated and used as a component of dry mix
fertilizers that are blended in another part of the complex.
At the time of the initial plant inspection (February 8,
1974) the precipitators were working satisfactorily and had
been very well maintained. The plant is representative of
modern design; raw materials and products are typical of those
in the industry.
11
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V. LOCATION OF SAMPLING POINTS
Figure 1 shows the sampling ports and sampling points used
in the No. 1 lime kiln exit stack. The sampling ports were
located in a 63.5-inch inside-diameter vertical stack, 4 feet
(0.75 diameter) from the stack exit, and 12 feet (2.26 diameters)
from the nearest downstream disturbance. In order to meet the
sampling requirements of Methods 1 and 5 of the Federal Register,
Vol. 36, No. 247, it was necessary to install a stack extension
on the ESP exhaust outlet. Forty-eight traverse points (24
along each of two perpendicular diameters) were used as described
in the Federal Register Method 1. Additional sampling points in
the existing stack at a lower site were used for some of the gas
sampling..
12
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TOP VIEW
A.
45'
24'-
ScoffolcJing
Edge ol roof
w'l
1 1
CROSS SECTION
I S
All Dimensions in Fool Aro Approximate
ELEVATION
Figure 1. Test Site-No. 1 Kiln Precipitator Outlet.
13
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VI. PROCESS OPERATION & TEST CONDITIONS
Before the test series began, EPA engineers had decided
to conduct tests at the Woodville plant only during periods
in. which opacity of visible emissions from the kiln stack
was in the range of 0 to 5 percent. This range had been
described as typical of opacities during operation of the
No. 1 kiln and was judged to be typical of those occurring
in a well-controlled lime-producing plant.
Although plant operations appeared to be normal and
preliminary readings indicated 0 to 5 percent opacity values,
several problems developed during the first day of testing,
July 8,1974. After about 3 hours of testing, PEDCo's team
of opacity readers stopped the tests at 8:22 p.m. because
opacity values were exceeding the 5 percent limit. Testing
was resumed at 8:27 p.m. and continued until 9:13 p.m.,
when the "A" field of the kiln's electrostatic precipitator
malfunctioned, probably because of overload. Sampling was
resumed at 9:16 p.m., when the opacity values again dropped
to the 0 to 5 percent range. The first test was completed
at 9:29 p.m.
The second test was started on July 9 at 8:41 a.m.
Opacities of visible emissions ranged between 0 and 5 percent
14
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throughout the entire test sequence. The test was completed
at 12:48 p.m., and because no problems were encountered
in sampling or process operation the emissions were considered
representative of those occurring normally.
After completion of the second test, plant operators
performed a routine cleaning operation, shutting down a
fan on the inlet to the ESP for removal of adhering dust.
The fan was not re-started after cleaning, however, and
opacity readings during the afternoon ranged between 10
and 15 percent. The third test, therefore, was not begun
until the following day.
Testing was resumed at 8:24 a.m. on July 10. Operations
appeared normal except for a heavy load in the kiln, as
evidenced by the .ampere meter on the kiln-drive motor..
Opacity readings ranged from 0 to 5 percent. Sampling was
hampered, however, by blockage in the silica gel impinger,
which was replaced several times. As testing progressed,
the opacity readers reported an increasing number of 5 percent
readings, with occasional 'puffs' as high as 10 percent.
Observations .of the plume were difficult because of cloudy
skies. Test No. 3 was completed at 12:55 p.m.
Operating variables for the three test runs are summarized
in Table 5,. and sulfur contents of the various process streams
are shown in Table 6.
A fourth test, intended to provide values to replace
those obtained in Test No. 1, was started at 3:00 p.m. July
15
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Table 5. SUMMARY OF OPERATING VARIABLES
Date
Particulate Test No.
Stone Feed Rate, ton/hra
Oil Rate, gal/hr
Firing Zone Temp, °F
Mid Kiln, Temp, °F
Kiln Feed End Temp, °F
Before ESP Temp, °F
Stack Temp, °F
ELECTROSTATIC PRECIPITATOR DATA
"A" Field
Primary current, amps
Primary voltage, volts
Precipitator current, amps
"B" Field
Primary current, amps
Primary voltage, volts
Precipitator current, amps
7/8/74
322
2620-2650
1460-1465
1020-1040
683-700
660-675
39-50
250-275
0.20-0.30
41-55
240-260
0.27-0.35
7/9/74
3
f ' ' ^
I
356
2600-2650
1450-1475
10'00-1035
685-700
660-690
37-46
250-265
0.19-0.23
50-54
240-250
0.28-0.30
7/10/74
5
375
2590-2620
1470-1520
1050-1080
700-725
670-700
48-61
250-270
0.20-0.32
53-61
240-250
0.32-0.37
a) Obtained by multiplying indicated tonnage by
(see Appendix D).
16
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Table 6. SULFUR CONTENT OF KILN, FUEL OIL, FEED ROCK, PRODUCT
AND EFFLUENT. DUST.
Sample
#1 ESP Col. Dust
#1 ESP Col. Dust
#1 ESP Col. Dust
#2 ESP Col. Dust
#2 ESP Col. Dust
#2 ESP Col. Dust
#1 Stone Feed
#1 Rock Feed
#1 Rock Feed
#1 Rock Feed
#2 Stone Feed
#2 Rock Feed
#2 Rock Feed
#2 Kiln Product
#1 Lime Product
#1 Lime Product
#1 Lime Product
#2 Lime Product
#2 Lime Product
#1 Fuel Oil
#1 Fuel Oil
#2 Fuel Oil
#2 Fuel Oil
#2 Fuel Oil
#1 Fuel Oil
Date
7/8/74
7/9/74
7/10/74
7/8/74
7/9/74
7/10/74
7/8/74
7/9/74
7/10/74
7/10/74
7/8/74
7/9/74
7/10/74
7/9/74
7/8/74
7/9/74
7/10/74
7/8/74
7/10/74
7/9/74
7/8/74
7/9/74
7/10/74
7/8/74
7/10/74
Time
1830
1015
0800
2030
1255
1030
1750
1100
1700
1000
2036
1230
1300
1300
1720
0930
1000
2030
1230
0930
1900
1230
1230
2030
1100
Sulfur Content
% by weight
0.9
1.32
1.28
0.78
1.16
.1.64
0.02
0.07
0.06
0.07
0.14
0.04
0.04
0.01
0.07
0.04
0.02
0.06
0.07
1.75
2.26
1.7
0.875
3.22
2.26
17
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10. Except for the heavily loaded kiln, process operations
appeared normal. Because opacity readings rose to the 15
to 20 percent.range, testing was stopped at 4:30 p.m. Cleanup
operations later revealed that the sampling probe was broken.
The values obtained in this test were therefore discarded,
and further sampling was scheduled for the following day.
On-the morning of July 11, however, stack opacity values
were again ranging between 5 and 10 percent. Although plant
personnel tried several variations in kiln operation, the
high opacity readings persisted throughout the day and evening.
A reading at 10:30 p.m. gave values between 20 and 25 percent.
At 6:00 a.m. on July 12, opacity readings still ranged
between 5 and 10 percent. Personnel of the Woodville plant,
EPA, and PEDCo agreed that the kiln should be shutdown briefly
for inspection. Examination of the ESP revealed that several
charge plates were covered with about 1 inch of a sticky
substance, which prevented the dust particles in the effluent
from receiving the positive charge and thus reduced collection
efficiency. It was estimated that cleaning of the plates
would require shutdown of the kiln for a week or so. A
shutdown was scheduled for the week of July 15 to allow
cleaning of the ESP, rebricking of certain kiln sections,
and routine periodic maintenance. Further emissions testing
was to be conducted shortly after resumption of kiln operation.
18
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VII. .SAMPLING AND ANALYTICAL PROCEDURES
Sampling procedures were designated by EPA. Analyses of
collected samples were performed by PEDCo. Appendix H presents
detailed.sampling and analytical procedures.
Velocity and Gas Temperature
Gas velocities were measured with a calibrated type S
pitot tube and inclined draft gage. Velocities were measured
at each sampling point across the stack diameter to determine
an average value according to procedures described in the
Federal Register - Method 2. Temperatures were measured with
the use of a thermocouple.
Molecular Weight
A 4-hour integrated sample of the stack gases was collected
during test 1 by pumping the gas into a Tedlar plastic bag at
the rate of approximately 0.005 CFM. This bag sample was then
analyzed with an Orsat analyzer for C02, 02, and CO as described
in the Federal Register, Method 3.
Particulates
Concentrations of particulate matter in stack gases were
2
measured by Method 5 as described in Federal Register. A rigid
train consisting of a heated glass-lined probe, a 3-inch diameter
1) Federal Register, Vol. 36, No. 247, December 23, 1971.
2) Federal Register, Vol. 36,. No. 159, August 17, 1971.
19
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glass-fiber filter, and a series of Greenburg-Smith impingers
was used for particulate sampling, as shown in Figure 2.
Sampling was conducted under isokinetic conditions by
monitoring stack-gas velocity with a pitot tube and adjusting
the sampling rate accordingly.
The particulate sample was recovered by triple-rinsing
the nozzle, probe, cyclone by-pass, and front half of the filter
holder with acetone into a glass container. The back half of the
filter holder, impingers, and connecting tubes were rinsed with
distilled water and the washings placed in a glass container with.
the impinger contents. These components were then triple-rinsed
with acetone into another glass container. The filter was
placed in a separate container. Blank samples of water and
acetone were also taken.
NO
x
Nitrogen oxides were collected in evacuated 2-liter
flasks containing 25 ml of a dilute sulfuric acid/hydrogen
peroxide absorbing solution. The sampling and analytical
procedure was as described in Method 7 of the Federal Register
except that the final flask vacuum was read immediately after
sampling.
S02
Sulfur dioxide sampling procedures followed those described
in Method 6. However, due to the low expected concentrations,
1) Federal Register, Vol. 36, No. 247, December 23, 1971.
20
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FILTER
NJ
HEATED
GLASS
PROBE
THERMOMETER
STACK WALL
HEATED I
SECTION -
MANOMETER
I | ' / SILICA GEL-^I
| I_LOO_FLL_ 0£_ WAT ER j
THERMOMETERS
UMBILICAL
CORD
CALIBRATED ORIFICE
CONTROL
VALVES
VACUUM
GAUGE
Hh
MANOMETER- I
Figure 2. Particulate Sample Train
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larger sampling .equipment was used. Flue gas was passed
through a set of Greenburg-Smith impingers at a rate of
approximately 0.8 cubic foot per minute. The first impinger
contained 150 ml of 80 percent isopropanol; the second and
third impingers contained 100 ml each of 3 percent hydrogen
per6xide/water solution. After sampling, ambient air was passed
through1the train for 10 to 15 minutes. The isopropanol solution
was discarded,, and the peroxide solution rinsed into a glass
container. The hydrogen peroxide solution was titrated with
barium chloride, using a Thorin indicator as described in
Method 6.
Visible Emissions
<»
Visible emissions were determined according to procedure
in Method 9. Readings were difficult to determine at times due -
to trucks loading and unloading ESP dust and quarry rock in the
vicinity of either the ESP unit or the observer and the light
colored plume against an overcast and partly cloudy sky caused
poor distinction. In addition, certain ESP rappers set up
a visible emission condition (puffs) that read approximately
5 to 10 percent opacity for about 2 to 3 seconds every cycle.
Sulfur Analysis
Solid samples were analyzed using Standard Methods of
Chemical Analysis of Limestone, Quicklime and Hydraded Lime,
C25-67, A.S.T.M. Standards, Part 9, Cement; Lime; Gypsum, 1972,
American Society for Testing and Materials, Philadelphia, Pa.
22
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Fuel oil samples, were analyzed using Standard Method of Test
for Sulfur in Petroleum Products by the Bomb Method/ D 129-64,
A.S.T.M. Standards, Part '17, Petroleum Products - Fuels, Solvents,
Burner Fuel Oils, Lubricating Oils, Cutting Oils, Lubricating
Greases, Hydraulic Fluids, 1972, American Society for Testing
Materials, Philadelphia, Pa.
23
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