EPA REPORT NUMBER 73-KPM-2B
C*I>'IIIIM'- 'TPC*V
SSI ON TEST
o
.* * * *
CHAMPION INTERNATIONAL
Courtland, Alabama
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
Office of Air and Waste Management
Office of Air Quality Planning and Standards
Emission Measurement Branch
Research Triangle Park. North Carolina
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SOURCE TEST REPORT
EPA No.: 73-KPM-2B
Particulate and Gaseous
Emissions From
A Kraft Pulp Mill
CHAMPION INTERNATIONAL
Court!and, Alabama
EPA Contract No.: 68-02-0232
Task No.: 18
Environmental Engineering, Inc.
2324 Southwest 34th Street
Gainesville, Florida 32601
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TABLE OF CONTENTS
Page Number(s)
I. INTRODUCTION 1
II. SUMMARY AND DISCUSSION OF RESULTS 2-4
Table 1 - Source Test Data . 3
Table 2 - Nitrogen Oxide Concentrations 4
III. PROCESS DESCRIPTION AND OPERATION' 5
IV. LOCATION OF SAMPLING POINTS 6-7
Figure 1 - Location of Particulate Sampling Points . 7
V. SAMPLING AND .ANALYTICAL PROCEDURES 8-17
Figure 2 - Particulate and SO^Train 10
Figure 3 - C0?, 0?, and CO Sampling System . .... 15
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I. INTRODUCTION
In accordance with Section 111 of the Clean Air Act as amended
of 1970, the Environmental Protection Agency is charged with the
establishment of performance standards for new stationary sources
which may contribute significantly to air pollution. These standards
are based upon the best air pollution control technology that has been
demonstrated.
This report supplements EPA Report Number 73-KPM-2A, Reduced
Sulfur Gaseous Emissions, and presents the results of an extensive
source testing program conducted at Champion International, Courtland,
Alabama, October 25-November 2, 1971, to obtain data for a partial
.basis in consideration of new source performance standards in the
kraft pulping industry.
Stack emissions were measured from the chemical recovery boiler
for particulate, sulfur dioxide, oxides of nitrogen, carbon dioxide,
carbon monoxide, and oxygen. The recovery boiler utilizes a direct
contact evaporator and strong black liquor oxidation, and exit gases
are controlled with an electrostatic precipitator.
Carbon monoxide and carbon dioxide were measured with infrared
analyzers and oxygen monitored with a paramagnetic oxygen analyzer.
All other stack emissions were measured with EPA reference methods.
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II. SUMMARY AND DISCUSSION OF RESULTS
Results from the participate and sulfur dioxide emission tests
are shown in Table 1. Emission rates were calculated on the basis of
the moisture content determined from the condensate recorded during
each test run. Based upon past sampling data for the recovery furnace,
plus the fact that excessive evaporation of isopropanol usually occurs
when used in the impingers instead of water, the actual moisture content
of the stack gases was probably greater than sample data indicated.
The third and fourth impingers, which contained 3% hydrogen
peroxide, were analyzed for sulfur dioxide by using barium perchlorate
titrations. These data are also included in Table 1.
Complete particulate and sulfur dioxide data are included in
Appendix A. .
Daily mean concentrations for oxygen, carbon dioxide, and
carbon monoxide are presented in Table 3. The results are reported
on a dry gas basis.
All gas concentrations are reported at five-minute intervals and
the maximum, minimum, and mean concentrations with the regression
coefficients for calibration curves are presented in Appendix B.
The results from the nitrogen oxide emission testing are summarized
in Table 2. Complete NO data are included in Appendix A.
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TABLE 1
SOURCE TES_'£
TEST fJO - ' NO OF RUIJS - 3
PL All 7 - CHAMP ion PAPERS' COUHTLAUD, ALA.
SOURCE - RECOVER:; BOILER OUTLET . . , •.'• ,
TYPE OF PL MIT - ..''•••''
COUTROL EQUIPMENT - ' ' . /
POLLUTAUTS SAMPLED - ' .' - ' :
NUMB UK 1 ___ 1 ______ 1 ___ .2 ______ 1 ____ a ______
2)DATE l_lJ)yj?lU:Z2_l_-lJl/.2:kV:Z.2_.J. __ 10.^2.a/.12..
3) Til-IE 'BEGAN . l_lltj:DD ____ 1-.1IU.2.Q _____ L __ 2i2Q _____
H) Til-IE END ' • 1_J^UD ____ 1_J.^I^D ____ i __ lliia"
5)BAROMETRIC PRESSURE, Iff EG ' Jl_J23-J _____ 1-33^.2 _____ I' __ 2S...2. _____
6 )METL'ii ORIFICE PRESSURE DROP, IN HG i_jDLJ71' _____ l_jD,!s5 _____ 1 __ £>Ili!iI_I_'
7)VO£ W?* GAS-METER COW, CUBIC FEET 1_.5_5_.2.3 ____ J._jkl*.2JiJ5___JL __ li2_Za.
8) AVERAGE CAS METER TEMPERATURE, DEC F L.JBJX.j} _____ 1_.&2...5 _____ 1 __ Zi-2. ____
GAS, S.T.P. , Ci/5161 .FA^T 1_J5J-JJJJ ___ l_i^.£J ____ I__li2*.0.15. ___
COLLECTED, ML i_iaj}^J? ____ i_.51'j[i^J5 ____ l.-BVn^S. ___
11)V0£ 7/20 K/1P07? COLLECTED, S.T.P. , CU FT]._J,°^(\ ____ JLJ2L5...B.1 ____ l__2Z,.ll ____
12)STACK GAS MOISTURE, PERCENT VOLUME \._2L^2 _____ l_J3iuJ _____ 1 __ 25.^5. _____
13) ASSUMED STACK GAS MOISTURE, PCT VOL 1_JJ} _______ l_j^ _______ .1 __ 2H _______
IHIPERCEIW C02 . JL.liL..3!> _____ 1_JJ5_J? ___ . __ 1 __ 1&*.!! ____
02 .' . i_iUJJ _____ 1_J3^J?^ _____ 1 __ Ma.20. _____
CO ' . /..-. . 1_J? ________ _L__D ________ 1__0 _______
'
1G)PERCEUT EXCESS. AIR ' 1_25 _______ l_J?j _______ 1 __ 22
IBIMOLECULAR WEIGHT OF STACK GAS, DRY l_JL?j^2 ____ 1_J?^J^ ____ 1 __ ^Hifi
20)MOLECULAR HEIGHT OF STACK CAS , £T# C01'!Dl_2-2^21 ____ l_JIui _____ 1 __ ZH^E
2DSTACK GAS SPECIFIC GRAVITY i_J?^^Jf _____ l.I1^^! _____ 1 __ Ik21
22)-4K6' SQUARE ROOT (VEL HEAD), I!,' 1120 1_JL:!1§ ____ 1^222 ____ 1__I}^2Z
23) AVER AGE STACK GAS TEMPERATURE, DEG F l_^Jj.^£' ____ l_^j)^J ____ 1 __ 2:15.
21)/17C SQUARE ROOT (STK TSMP*VEL HEAD) L.32^222 ___ 1_J1J^J _____ 1 __ 2£i.I
25)PITOT CORRECTION FACTOR . L.®J.*2 _____ 1-S>^*2 _____ ll_£i£2.
2G)STACX PRESSURE, Hi UG, ABSOLUTE 1_2$ •.?__ ___ 1_22^2 _____ l__H2i.2
27) STACK GAS VEL, STACK COiJD, F.P.M. l_'*B.B2'll __ l_lPI'll_:L_ I__!i2il5.
28)5^/16'^ /i/?iM. 5Q FEST . J-2"5-^ ____ 1-^--^ ____ l__5El.!i
29) EFFECTIVE STACK AREA, SQUARE FEET 1_- ____ 1-- : ?----
3o)5ryio'Ax G'/^' j?£o;/ ^/iri>', S.T.P. , SCFMD 1
3i);^r TII;X OF TEST, ;.II;;UTES . • 1
32)SA!.lPLIiiG HOZZLL DIAMETER, INCHES
3 3) PERCENT ISOKIi^TIC !___-:-___ __ L *12^2 ____ -I
34)PARTICULATE EMISSIONS, LBS/HR
FRONT HALF . . 89.18 62.87 24.72
TOTAL ' ' 96.15 68.00 34.54
35)SULFUR DIOXIDE EMISSIONS LBS/HR 196.3 79.3 153.9
36)SULFUR DIOXIDE CONCENTRATION, PPM DRY 213.3 .110.6 217.1
DRY, 70 DEGREES F, 29.92 IllCUES
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TABLE 2
NITROGEN OXIDE CONCENTRATIONS
. RECOVERY FURNACE OUTLET
Date
10/26/72
10/26/72
10/26/72
10/27/72
10/27/72
10/27/72
10/30/72
10/30/72
10/30/72
Time
1345
1510
1645
1000
1130
1255
0910
1025
1135
NOX, ppm
15.9
8.4
1.6
48.6
39.5
4.0 .
61.0
31.8
17.5
TABLE 3
C02, 02, AND CO CONCENTRATIONS
RECOVERY FURNACE OUTLET'
Date
10/25/72
10/26/72
10/27/72
10/30/72
10/31/72
11/1/72
Time
Span
1015-1125
1130-1325
1520-1745
0955-1700
0940-1525
0930-1500
0930-1535
0950-1525
Daily Averages
CO (ppm)
55.7
49.3
70.5
25.0
51.8
13.7
64.5
132.0
co2 (%j
16.5
16.3
16.4
15.4
16.4
16.3
17.1
•15.3
o2 '(*)•
4.4
4.2
4.0
4.4
4.2
4.1
3.3
3.8
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III. PROCESS DESCRIPTION AND OPERATION
The process description and operation is contained in EPA
Report Number 73-KPM-2A, "Total Reduced Sulfur Emissions"" obtained
during this test.
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IV. LOCATION OF SAMPLING POINTS
The outlet stack from the electrostatic precipitator on the
.recovery furnace was sampled at the vertical stack, as shown in Figure 1.
The traverse points sampled in each of the two ports are as
follows: . •
Distance From
Sample Point No. Inside Wall, In.
.1 13/4
2 55/8
3 97/8
4 14 7/8
5 21
6 29 3/4
7 54 1/4
8 63
9 69 1/8
,10 74 1/8
. . 11 78 3/8
12 82 1/4
NOTE: The traverse points were utilized for determination of particulates,
sulfur dioxide, gas volumes, moisture and other necessary stack gas
parameters. The gaseous constituents were extracted from the source
gas stream based upon the assumption that the gases were homogene-
ously mixed. Therefore, nitrogen oxides, carbon dioxide, oxygen,
and carbon monoxide were sampled from relatively fixed points in the
gas handling system.
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84 Inch diameter
Section A-A
Boiler
.
1
1
1
1
Cascad
e -.;•...,•/'
• '
. 1 V.
• .. ' 1 •
1
— ttf —
. !, 1
:•
• . I Fan
^*— L^J^*
Oxidized Black Liquor . . ..
] '• ' '. • •• FIGURE 1 • ,: : ',..•', '
. . LOCATION OF PARTICULATE SAMPLING POINTS
Platform
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V. SAMPLING AND ANALYTICAL PROCEDURES
Sampling Procedure for Particulate Emissions . .
Prior to performing the actual participate emission tests,
certain preliminary stack parameters had to be determined for the
stack gases. This preliminary data included the average stack gas
temperature, velocity head, moisture content, stack dimensions, and
number of sampling points.
The stack gas temperature was determined by using bimetallic
thermometers and a pyrometer.
The approximate-stack gas moisture content selected for
setting the nomograph was based upon previous tests made on the same
'boiler. The final moisture content used in calculating the stack
emissions from the recovery furnace was based upon the amount of conden-
sate collected in the impingers and the silica gel from a separate
moisture test.
The sampling points selected and the respective stack gas
velocities were determined by using Methods Np. 1 and 2 of the Federal
Register (Vol. 36, No. 247, December 23, 1971). Velocity head measure-
ments were made by using a calibrated S-type pi tot tube with an inclined
manometer.
The sampling train configuration used during the tests consisted
of the following: a stainless steel nozzle; a heated glass-lined probe;
a heated glass-fiber filter; two Greenburg-Smith impingers with tips,
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each containing 100 ml of 80% isopropanol; two Greenburg-Smith
i
impingers without tips, each containing 100 ml of 3% hydrogen peroxide;
one Greenburg-Smith impinger without a tip, containing about 200 grams
of silica gel; a flexible sample line; an air-tight vacuum pump; a
dry-test meter; and finally a calibrated orifice with an inclined
manometer (see Figure 2). Velocity head measurements were conducted
simultaneously with the sampling at each point so that each point
could be sampled isokinetically.
The impinger portion of the sampling train was iced down to
collect the condensables, and to determine the actual stack gas moisture.
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1. Stainless steel nozzle
2. Glass-lined probe (heated)
3. Heated box (250°F)
4. Glass-fiber filter and holder
5. Ice bath '
6. Iinpinger with Tip, 100 ml of 80% Isopropanol
7. Impinger vn'th Tip, 100 ml of 80% Isopropanol
_8. Impinger without Tip,. 100 ml of 3% H?0?
D- *-
9. Impincer without Tip, 100 ml
. of 3:rH2o2
10. Impinger with 200 grams
of Silica Gel
11. Thermometer
12. Flexible sample line
13. Vacuum gauge
14. Coarse valve
15. Fine valve
16. Vacuum pump
17. Drg-test meter •
18. Calibrated orifice
19. Inclined manometer
20. S-type pitot.tube
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FIGURE 2
PARTICULATE AND S00 TRAIN
13
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Sample Recovery and Analyses of Particulates
Sample, recovery from the participate train was accomplished
by separating train components into the following containers:
Container N'o.l - The previously weighed glass-fiber filter
was placed into this container, then sealed and labeled.
Container No. 2 - All portions of the train from the nozzle
•through the front half of the filter holder were rinsed with
acetone and the contents placed into a glass container, then
sealed and labeled.
• Container No. 3 - The volume of liquid from the first and
second impingers was measured and the contents placed into
a glass container. Also, all sample-exposed surfaces between
the filter and third impinger were rinsed with 80% isopro-
panol and placed into this container, then sealed and labeled.
Container No. 4 - The volume of liquid from the third and
fourth.impingers was measured and the contents placed into
separate glass containers. All glassware between the second
and fifth impingers was then rinsed with deionized, dis-
tilled water and then added to each respective container.
The liquid samples were then sealed and labeled. Only one
sample container was used for both impingers used in the
smelt dissolving tank sampling.
Container No. 5 - The previously weighed silica gel was re-
moved from the fifth impinger and placed into the original
polyethylene jar and sealed.
11
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The samples recovered were analyzed as follows:
Container Mo.. 1 - The filter and all loose material in the
sealed petri dish were transferred to a tare glass weighing
dish, desiccated, and dried to a constant weight.
Container Mo. 2 - The acetone washings were transferred to a
tared beaker and evaporated to dryness at ambient temperature
and pressure. It v/as desiccated and dried to a constant weight.
Container No. 3 - The contents were transferred to a tared
beaker, and then evaporated at 212°F. The residue was desic-
cated and dried to a constant weight.
Container No. 4 - The liquid contents-were shaken, and then
a 25 ml aliquot of each container was pipetted into separate
250 ml Erlennieyer flasks. One hundred ml of isopropanol,
plus two to four drops of thorin indicator was added to each
. sample. The samples were titrated with barium perch!orate
to a pink end point. Another duplicate sample and blank was
titrated in the same manner as the first sample. Samples
were analyzed at the plant site.
Container Mp. 5 - The spent silica gel was weighed at the site
and recorded.
The filter from Container No. 1, and the beakers from Containers
No. 2 and 3 for each run were sent to the EPA project officer after the
initial analysis for additional analyses.
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'Sampling System -for Oxygen> Carbon D1oxide» and Carbon Monoxide
Figure 3 is a schematic diagram of the sampling system.
Source gases were drawn continuously through a glass-lined probe and
polyethylene tubing to a moisture trap consisting of silica gel im-
pingers immersed in an ice bath. Valves on the pressure side of the
vacuum pump controlled the flow of sample gas to the detectors. A
bleed valve was provided to maintain adequate purging of the sample
line. Gases to the oxygen and carbon monoxide detectors were passed
through an ascarite bed to remove carbon dioxide which potentially
interferes with the.NDIR determination of carbon monoxide. Sample to
the carbon dioxide detector was diluted with nitrogen to accommodate
the range requirements of the detector.
13
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A BeckiH6)>;:Kodel F-3 paramagnetic oxygen analyzer-capable of
measuring 0 - 25" oxygen v/as used for 0? detection. Beckman NDIR
models 315-8 and 315-A, respectively, were use'd-.rn determining carbon
dioxide and carbon monoxide concentrations. The instrument configura-
tions were 0 - 5% C02 and 0 - lOOOppm CO. All instruments were supplied
with a low, medium and high range which were calibrated separately. The
detectors were switched on and allowed to run continuously 24 hours per
day for the entire sampling interval.
Calibration
All calibration gases were supplied and analyzed by Matheson
Gas Products, Inc., Morrow, Georgia, and La Porte, Jexas. The calibra-
tion procedure was conducted prior to sampling each morning and was re-
peated at the end of each day. Nitrogen was introduced into each
instrument and the zero control was adjusted to obtain a steady "zero
trace" on the recorder. Appropriate standards were then passed into
the instruments at less than 100 cc/minute. The gain controls for each
range were adjusted to provide maximum deflection and accuracy.
Daily Operation
Each morning after calibrating the instruments, charging the
traps, and checking the probe, the system was assembled as shown in
Figure 3. The dilution to the carbon dioxide detector was regulated
to provide an accurate deflection range at a total flow rate less than ,
100 cc/minute. Flows for sample gas and dilution nitrogen were measured
with a bubble tube, the recorder traces were observed and the ranges
14
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From Stack
Ice Bath
Silica
Gel
Midget Impinger
w/Silica Gel
To CCL System
is
Bleed V
t
Vacuum Pump
Flow
To CO, 09 System
, Ascarite
Impinger
Vent
CO
NDIR
°2
Paramagnetic
Analyzer
A
CO
Cal
Gas
Flowmeter
Di 1 ujtipnSystem
"TT.
r V
A
co2
Cal
Gas
-txi
A
Vent
°2
Cal
Gas
Vent
co2
NDIR
Dilution
Nitrogen
C02, 02, and CO SAMPLING SYSTEM
Figure 3
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were adjiustecf throughout the- sgr.rpTing interval as required. Occasionally
sampling was interupted to obtain odor samples, charge traps, or to check
the system.
Data Reduction
A computer program, developed by Environmental Engineering,
Inc., was used to reduce recorder deflections to specific gas concentra-
tions. Average calibration deflections and respective calibration - gas .
concentrations were entered for each range, and a second order regression
analysis v/as computed. The general form of the regression equation is:
y = A + Bx + Cx2
where y = measured gas concentration, % or ppm
A, Bj C = regression coefficients as calculated
x = recorder deflection, millimeters.
Strip chart data was reduced to computer input sheets which
are included in the Appendix C. The carbon dioxide con-
centration v/as calculated using the above regression curve and the mean
dilution factor. Oxygen and carbon monoxide concentrations were deter-
mined in like manner and corrected for carbon dioxide absorption. The
correction factor for oxygen and carbon dioxide was determined from the
simultaneous carbon dioxide concentration using the relationship:
Actual 0?, CO = \ T "" 2/1 measured 0?., CO
16
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Sampling Procedure for Nitrogen Oxides'
Nitrogen oxide concentrations of the recovery furnace outlet
gases were determined by using .the EPA Method 7, which is described
in the Federal Register (Volume 36, No. 247, December 23, 1971).
Essentially, the method consisted of collecting a grab sample
of the gas in an evacuated 2-liter flask containing a dilute sulfuric
acid-hydrogen peroxide absorbing solution. The sample remained in the
flask at least 16 hours, and was then placed in a glass storage bottle.
Sodium hydroxide (IN) was then added to the sample until alkaline. The
samples were taken back to the laboratory in Gainesville, Florida, and
measured colorimetrically using the phenoldisulfonic acid procedure.
17
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