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
                                                  14
         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.
                                 12

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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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