COAL  PREPARATION  PLANT EMISSION  TESTS
                         TEST NO. 1281-35
                   WESTMORELAND COAL COMPANY
                          WENTZ PLANT
                         Stonega, Virginia
                           PREPARED FOR
                 ENVIRONMENTAL PROTECTION AGENCY

                       Research Triangle Park
                        North Carolina  27711
                       Contract No 68-02-0233
                 SCOTT  RESEARCH LABORATORIES, INC.
                      PLUMSTEADVILLE, PENNSYLVANIA 18949

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         SRL 1281 35 0472
         Test No.  1281-35

     Westmoreland Coal Company
            Wentz Plant
Stonega, Virginia, Norman R.  Troxel
 SCOTT RESEARCH LABORATORIES, INC.
Plumsteadville, Pennsylvania  18949

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SRL 1281 35 0472

                            TABLE OF CONTENTS
                                                                 Page
1.0  INTRODUCTION                                                1-1
2.0  SUMMARY OF RESULTS                                          2-1
3.0  PROCESS DESCRIPTION                                         3-1
4.0  LOCATION OF SAMPLE POINTS                                   4-1
5.0  PROCESS OPERATION                                           5-1
6.0  SAMPLING AND ANALTYICAL PROCEDURES                          6-1
     6.1  PARTICULATE SAMPLING AND ANALYTICAL PROCEDURES         6-1
     6.2  GASEOUS SAMPLING PROCEDURES                            6-1
     6.3  NO  SAMPLING AND ANALYTICAL PROCEDURES                 6-2
            x
     6.4  ORSAT SAMPLING AND ANALYTICAL PROCEDURES               6-3
     6.5  TOTAL HYDROCARBON SAMPLING AND ANALYSIS PROCEDURES     6-3
APPENDIX A     COMPLETE PARTICULATE RESULTS WITH
               EXAMPLE CALCULATIONS                              A-l
APPENDIX B     COMPLETE GASEOUS RESULTS WITH EXAMPLE
               CALCULATIONS                                      B-l
APPENDIX C     FIELD DATA                                        C-l
APPENDIX D     STANDARD SAMPLING PROCEDURES                      D-l
APPENDIX E     LABORATORY REPORT                                 E-l
     E.I  ON-SITE HANDLING AND TRANSFER, PARTICULATE             E-2
     E.2  LABORATORY HANDLING AND ANALYSIS, PARTICULATE          E-3
     E.3  NO  ANALYSIS                                           E-7
            x
     E.4  ORSAT ANALYSIS                                         E-8
     E.5  TOTAL HYDROCARBON ANALYSIS                             E-10
APPENDIX F     TEST LOG                                          F-l
APPENDIX G     PROJECT PARTICIPANTS AND TITLES                   G-l
    SCOTT RESEARCH LABORATORIES, INC

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                                   1-1




SRL 1281 35 0472






                            1.0  INTRODUCTION




          Scott Research Laboratories, Inc. performed source sampling




tests at the Wentz Plant of Westmoreland Coal Company during the week




of March 20, 1972.  This plant is located in Stonega, Virginia.  The




plant uses a Research Cottrell venturi scrubber to control the exhaust




gas emissions from a coal cleaning and preparation operation.




          The exhaust gases, as they were being emitted to the atmos-




phere, were sampled and analyzed for the determination of total




particulate loading, oxides of nitrogen, total hydrocarbons, carbon




monoxide, carbon dioxide, and oxygen concentrations.




          There are two types of coal processed at the plant, Osaka




coal and Wentz coal.  The Osaka coal is a low sulfur, medium ash,




high volatile steam coal of 55 grindability index, while the Wentz




coal is a low sulfur, low ash, high volatile metallurgical coal of 55




grindability index.  One sample run with Osaka coal being processed




was performed on March 20, 1972, and two other runs were conducted on




March 22, 1972.  Two sample runs were performed with the Wentz coal




being processed on March 23, 1972.  Figure 1 shows the location of the




sampling point at the plant.
     SCOTT RESEARCH LABORATORIES, INC.

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                                    1-2
SRL 1281 35 0472
WESTMORELAND COAL Cg.

    STONEQA, VIRGINIA
                               BLOWER
                                 LLEVATION

                        FIGUKK 1 - SAMPLE POINT LOCATION
                                                                .«. MIST
                                                                ELIMINATOR
     SCOTT RESEARCH LABORATORIES, INC

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                                   2-1





SRL 1281 35 0472






                         2.0  SUMMARY OF RESULTS




          A summary of test results is presented in Table 1.  The




particulate weights are summarized and shown in Table 2, with all of




the particulate results included as Appendix A.  Appendix B presents




all of the gaseous results, and the raw data sheets are included as



Appendix C.




          From Table 2 it is observed that the particulate matter



collected during the three runs while Osaka coal was being processed




averaged approximately 40 percent more than what was collected during



the two runs performed while Wentz coal was being processed.  This is



also shown in Table 1 where the particulate emission rate to the atmosphere




was approximately 50%  higher for Osaka coal compared to Wentz coal.




          A visible trail of brownish smoke was observed from the stack




during the processing of Osaka coal.  It was difficult to compare this




occurrence with the visible emissions during processing of Wentz coal,




since it was snowing the day of the tests.  However, there did appear



to also be somewhat of a brownish trail.




          The NO  concentrations were fairly consistent for all of the
                x


tests.  The total hydrocarbon concentrations, however, varied considerably.



They ranged from 18 ppm to 208 ppm.
     SCOTT RESEARCH LABORATORIES, INC

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                                             TABLE  1 -  SUMMARY OF TEST  RESULTS
OJ
g

§
SO
S
Run Number
Type of Coal
Sample Date
Sample Gas Vol., scf.
Moisture, %
Stack Gas Temp., °F
Stack Gas Vel., fpm.
Stack Gas Vol., SCFM
Partlculate Collected
   Probe, cyclone, filter, mg.
   Total, mg.
Particulate Concentration
   Probe, cyclone, filter, gr/scf.
   Total, gr/scf.
Particulate Emissions
   Probe, cyclone, filter, Ib/hr.
   Total, Ib/hr.
Percent Isokinetic
Carbon Monoxide, %
Carbon Dioxide, %
Oxygen, %
Total Hydrocarbon (ppm-C)
NO , ppm
  A.

1
Osaka
3/20/72
88.56
12.61
120
5165
137,310
261.5
337.0
0.046
0.059
53.54
68.96
87.89
0.0
0.2
18.2
208.2
52.8

2
Osaka
3/22/72
86.95
13.61
120
4961
128,520
206.5
280.5
0.037
0.050
40.31
54.74
92.19
0.0
0.3
19.6
102.0
54.4

3
Osaka
3/22/72
86.09
12.56
120
4847
127,100
242.0
314.0
0.043
0.056
47.16
61.22
92.30
0.0
0.2
19.4
48.0
37.6

4
Wentz
3/23/72
95.90
11.93
120
5120
135,450
169.5
220.5
0.027
0.035
31.57
41.09
96.48
0.0
0.3
19.8
31.5
59.6

5
Wentz
3/23/72
94.51
9.37
120
4998
136,070
173.0
225.0
0.028
0.037
32.88
42.80
94.65
0.0
0.4
19.8
18.0
44.6
CO
f
to
oo
u>
Ul
o
to













                                                                                                                       NJ
                                                                                                                        I

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                                   2-3
SRL 1281 35 0472


                  TABLE 2 - PARTICULATE WEIGHTS  SUMMARY

Run Number                       1         2         3         4        5
Container 1, mg.               92.0    101.5      94.0     64.0     78.0
Container 2, mg.               169.5    105.0     148.0    105.5     95.0
Container 3a, mg.                5.0       9.0       8.0      9.0      8.0
Container 3b, mg.              61.0     54.0       5.5     32.5     30.5
Container 5, mg.                 9.5     11.0      13.5      9.5     13.5
Probe, cyclone filter, mg.     261.5    206.5     242.0    169.5    173.0
Total, mg.                     337.0    280.5     314.0    220.5    225.0
     SCOTT RESEARCH LABORATORIES, INC

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                                    3-1


 SRL 1281 35 0472






                         3.0  PROCESS DESCRIPTION
i


           At the Wentz plant the coal from the mines is screened,



 washed and then dried.  The exhaust from the drier passes  through  a



 Research Cottrell venturi scrubber before it is emitted to the



 atmosphere.  Figure 2 shows a flow diagram of the Wentz plant.
      SCOTT RESEARCH LABORATORIES, INC

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o

s


n
i
Bd
O
»

25
2
    StAM :
                                        FIGURE 2  COAL FLOW IN WENTZ CLEANING PLANT

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                                   4-1





SRL 1281 35 0472







                     4.0  LOCATION OF SAMPLE POINTS




          The exhaust gases from the coal cleaning operation pass through




a Research Cottrell venturi scrubber to a mist eliminator and then are




emitted to the atmosphere through an 81 inch diameter stack.  Two




sampling ports located at 90° apart were in the stack at a point




approximately 10 feet upstream from the top  of the stack and approximately




25 feet downstream from the outlet of the mist eliminator.




          There had been a platform installed at the sample point location




for some previous test work.  An angle iron support rail extending ten




feet out from each port was used to hold the sample box.  The sample




control unit was located in the same area.  Figure 1 shows the physical




layout of the system and the location of the sample ports.




          Figure 3 shows the traverse points used.  A total of 48 traverse




points were sampled two and one half minutes each.  In order to stay




at least two inches away from the wall, the first two and last two points




on the traverse were combined.  Thus, the first and last points (each




containing two traverse points) were samples for five minutes each.  The




traverse points were chosen in accordance with Method 1 published in




the Federal Register, Volume 36, No. 24.




          The two ports were designated as A and B, with A being the




port on the left and B the port 90°  to  the right of A.
     SCOTT RESEARCH LABORATORIES, INC

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                                   4-2
SRL 1281 35 0472
                                                  WESTMORELAND COAL CO.
                                                    STONEGA,  VIRGINIA
                  FIGURE 3  TRAVERSE POINT LOCATIONS
    SCOTT RESEARCH LABORATORIES, INC.

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                                   5-1


SRL 1281 35 0472


                         5.0  PROCESS OPERATION

          During the test all filter cake from flotation cells was  fed

to the dryer.  Measured loadout of rail cars indicated that  the plant

production during our tests was 300 TPH, of which 200 TPH had been

thermally dried.

          Process variables monitored during the tes.t were the furnace

combustion zone temperature.  These were recorded as follows:
                         Dryer Temperature
                          Combustion Zone        Exhaust Temperature
Date
3/22
3/22
3/23
3/23
Test No.
2
3
4
5
Hi
1300
1250
1200
1200
Lo
1100
1100
900
700
Avg.
1150
1150
1100
1050
Hi
180
180
150
155
Lo
155
170
140
140
Avg,
170
175
145
145
          Process operating data was not obtained  during  the first test

on March 20, 1972.
     SCOTT RESEARCH UBORATORIES. INC

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                                   6-1



 SRL 1281 35 0472








                 6.0  SAMPLING AND ANALYTICAL PROCEDURES




6.1  PARTICIPATE SAMPLING AND ANALYTICAL PROCEDURES




          Samples were collected for the determination of particulate matter




from the outlet of the venturi scrubber.  The sampling and analytical pro-




cedures used were the same as those specified by Method 5, "Determination of




Particulate Emissions from Stationary Sources", and published in the Federal




Register, Volume 36, No. 247, Thursday, December 23, 1971.  In addition, the




impinger catch was analyzed.  This method is attached as Appendix D.




          Briefly, the method consists of withdrawing a sample isokinetically




from the stack through a heated glass probe into a cyclone, filter, and




impinger train.  The cyclone and filter are contained in a heated box.




The sample volume is measured with a dry gas meter, and isokinetic conditions




are maintained by monitoring the stack gas velocity with an "S" type pitot




tube.  After testing is completed, the train is thoroughly washed including




the probe.  The washings are evaporated, dried, and weighed along with the




filter in order to obtain a total weight of particulate matter collected.




          The stack gas velocity and flow rate was measured using




Method 2, "Determination of Stack Gas Velocity and Volumetric Flow Rate




(Type S Pitot Tube)", and published in the Federal Register.  Using both




the weight of sample collected and the flow rate determined, a total




particulate emission rate was calculated.






6.2  GASEOUS SAMPLING PROCEDURES




          Stack gas samples were taken at regular intervals during each




particulate sampling traverse to determine the concentrations of 0«,
     SCOTT RESEARCH LABORATORIES. INC

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                                   6-2



SRL 1281 35 0472





CO, C09, NO  and total hydrocarbons present in the stack effluent.  The
      Z-    X


sampling location was the same with respect to the venturi scrubber as



that used for the particulate samples.  The sampling and analytical



procedures used were in accordance with Federal Register, Volume 36,



No. 247, December 23, 1972, "Standards of Performance for New Stationary



Sources".





6.3  NO  SAMPLING AND ANALYTICAL PROCEDURES
       x


          All NO  samples were taken through a ^ inch O.D. glass probe
                x


heated to approximately 250 F.  Each sample was drawn through this probe



into a previously evacuated 2 liter flask containing 25 ml. of NO



absorbing solution.  The flasks were shaken for 5 minutes following each



sampling period and then allowed to stand for at least 16 hours.



Following this, the samples were shaken again for 2 minutes just prior



to measuring the final flask pressure.  The samples were then transferred



to glass shipping bottles with distilled water washes and neutralized



with 1.0 N sodium hydroxide.  At the end of the test period, all samples



were returned to the laboratory for analysis.



          The samples were analyzed via the phenoldisulfonic acid



procedure described in the aforementioned Federal Register.  The absor-



bances were measured with a Bausch and Lomb Spectronic 20 Colorimeter



and the results were reported as parts per million N0_.
     SCOTT RESEARCH LABORATORIES, INC

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                                   6-3




SRL 1281 35 0472






6.4  ORSAT SAMPLING AND ANALYTICAL PROCEDURES




          Integrated bag samples were taken for Orsat analysis (CO,




C0_ and 0 ) during each particulate sampling period.  The sampling




apparatus consisted of a ^ inch O.D. stainless steel probe, a stainless




steel coiled tube condenser, a glass water trap, a carbon vane pump,




a flowmeter and needle valve assembly, a 3 inch #21 stainless steel




hypodermic needle, and a 5 liter Tedlar sample bag fitted with a




syringe cap.




          The sampling procedure was initiated by purging the probe




and condenser system with stack air, adjusting the sample flow rate




to approximately 80 cc per mintue, and inserting the hypodermic needle




into the syringe cap on the sample bag.  The integrated sample was




taken over a 1 hour period yielding approximately 4.8 liters of sample




for analysis.




          At the end of each test day, the sample bags were analyzed




by Orsat for CO, C0~, and 0 .   Repetitive analyses were performed on




each bag to insure satisfactory duplication.  The results were reported




in percentages.






6.5  TOTAL HYDROCARBON SAMPLING AND ANALYSIS PROCEDURES




          The same integrated bag sample that was taken for Orsat analysis




was analyzed for total hydrocarbons via a Beckman Model 108-A Total Hydro-




carbon Analyzer.  Following each Orsat analysis the Tedlar sample bag was




connected to the hydrocarbon analyzer via a Teflon sample tube.  The




sample was drawn into the instrument until a stable reading was recorded




on the meter.  Before and after each analysis the instrument was zeroed




with hydrocarbon free air (<0.1 ppm-C) and spanned with a Scott close
     SCOTT RESEARCH LABORATORIES, INC

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                                    6-4





SRL 1281 35 0472






tolerance blend of  99.9  ppm propane in  nitrogen (analysis: ±2.0%).  The




meter readings for  each  sample were converted to ppm-C as shown in




Section E-5 of Appendix  E.
     SCOTT RESEARCH LABORATORIES, INC.

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                                    A-l




SRL 1281 35 0472
                                APPENDIX A




          COMPLETE PARTICULATE RESULTS WITH EXAMPLE CALCULATIONS
     SCOTT RESEARCH LABORATORIES, INC

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                                   A-2
                                                                   • OF
                               SOURCE TESTING CALCULATION FORMS
 Test.  No.
                                                             No.  Runs
Name of Firm
                             CM/..
 Location of Plant	
 Type of Plant     £-«P al
                                           
J.olZ
».K
n
tw
;«?.37
. 	
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5-£
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...... 	
f
SlS°i
Mto
ty^.&Q
, ..^... — .- ^
o(0 o« /



!
.



7.77 ;
     * 70°F,  29.92" Hg.

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A-3
    ITVTC
     '   '

P.un I.'o. ...
/:M - % Krnst'jrc i-: IV? stack g<.s by volume
"M, - Mole fraction of dry gas
AC02 ( W r\ f d s f. i\
2 I ffss-) )
. -- . v i/ „
A N • / • \
* N2 -( *"j) .. ' •
M W . - Molecular weigiit. of dry steel: gas
. .
M W - Molecular weight of stack gas
0
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1


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•Run to. '
C. • - Parties: tLte, total ,-$r7'cf
. L-.U r, ,- .-. -. ... 1. ~r r ,.;

C.M - Pn rti f'U • atcT1 pvoo.';'. cyclone'^
-c" and filter, lo/hr.
C - Particulate - total > Ib/hr.
3X •
% EA - % Excess air &
samp 'ring point
^
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"" ~^«

ust
19.%
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tf.o?6o

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j
i
I
'70°F.  29.9a" Hg.

-------
1;
                                  A-5
                              'ARTICULATE CALCULAT'JOi'.'S
    Volume of dry ges  sampled c.t standard conditions - 70°F, 29.92'''-
    lig,  ft. 3
             17.7  X  V /Pp   •:•   P]
                     ""   K   -ire-/
2%  Volunie of water- vapor at 70°F  & 29.92"  lig,  Ft.
          «  0.0474 X
                        =  Ft.3

3.  % moisture -in  stack  gas

          mstd   wgas
4.  Mole fraction  of  dry  gas
              100
5.  Average molecular  v/eight  of  dry  stack  gas
                                                    x

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                                 A-6
           - K W ,  X  H . .  is  [I
  7.   Stack  velocity P stack conditions.
 v  « 4350 xA      T+
                              o)/,
                                            I 1/2-
                                             = fprn  r
  8.
 Stack gas  volume  @  standard conditions, SCFM

      0.123 X  Vc X A, X Mj X P

                   + 460)
                                  S   =  SCFM
                                              = .  '/.3-73I.O
 9.  Per cent isokinetic
          1032 X (T  -i-  460)  X  V
          YsXTtXPs  XMdX  -(Dj2
                                                      81. B
10.   Panticulate - probe, cyclone, & filter,  gr/SCF
Can = 0.0154  x;/  = gr/SCF
               Vstd
                                                x  «?6/,
                                       =-  o.o

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                                  A-7


';].  Pcirticin<'.li: tola], gr/'SCF
     C    --- 0.0154 X 7>--=.gr/SCF
      3O              m        '

                    -.  mst
-------
16.  %  c-ixcurj5.. sir ..re
                :v;  point
TOO  X  %
                         •-= %.
0.266  X

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                                    B-l





SRL 1281 35 0472
                                APPENDIX  B




           COMPLETE GASEOUS RESULTS WITH EXAMPLE CALCULATIONS
     SCOTT RESEARCH LABORATORIES, INC

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                                    B-2

SRL 1281 35 0472
                         ORSAT  ANALYSIS DATA SHEET


 Run                        Analysis          %          %           %
 No.         Date            Number         CO         C00          00
 --          ---.--.  .-I---,              .             -^—        ' 	Z        ~~~~"Z"~~
  1         3/20/72            1             0.0        0.2         18.2
                               2             0.0        0.2         18.1
                               3             0.0        0.2         18.2
                             Avg.           0.0        0.2         18.2

  2         3/22/72            1
                               2
                               3
                             Avg.

  3         3/22/72            1
                               2
                               3
                             Avg.

  4         3/23/72            1
                               2
                               3
                             Avg.

  5         3/23/72            1
                               2
                               3
                             Avg.           0.0        0.4         19.8
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.3
0.2
0.3
0.3
0.2
0.2
0.3
0.2
0.3
0.4
0.3
0.3
0.4
0.4
0.5
19.6
19.7
19.6
19.6
19.4
19.4
19.5
19.4
19.8
19.7
19.8
19.8
19.8
19.8
19.8
     SCOTT RESEARCH LABORATORIES, INC

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                                   B-3
SRL 1281 35 0472
                          TOTAL HYDROCARBON DATA
Run
No.
1
2
3
4
5
Date
3/20/72
3/22/72
3/22/72
3/24/72
3/23/72
Sample
No.
1
2
1
2
1
2
1
2
1
2
Range
100
100
100
100
100
100
100
100
100
100
Meter
Units
69.5
69.5
35.0
33.0
16.0
16.0
10.5
10.5
5.0
7.0
THC*
(ppm-C3HQ)
69.4
69.4
35.0
33.0
16.0
16.0
10.5
10.5
5.0
7.0
THC
(ppm-C)
208.2
208.2
105.0
99.0
48.0
48.0
31.5
31.5
15.0
21.0
    *  All spans were set at full scale on Range  100 using  a 99.9

       ppm C_HQ standard.




    Sample calculation:


       Run #1, Sample #1:

              n ti    meter units x 99.9 ppm-C0Hn
          Ppm-C2Hg =                         3-8
          nraB
          ppm-
                     (69.5H99.9)
                             -
               38
          ppm-C-H_ =69.4
               J o



       ppm-C = ppm-C_HQ x 3
                    J O



       ppm-C = 208.2
     SCOTT RESEARCH LABORATORIES. INC

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                                 B-4
                              NO,  MISSION CAM
Run io.
.Date -
ing K0?
T. - Fle.s!; Ten.pGraturc?, °F
Vf - Flr.sk Vclu:.ie, liters
P- - Initial Fliisk VACUUM, "Kj.
Pf- Final Flask Vacuum, "Hg.
ppni NC^
l-l
2o*«~?i
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^
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ppm
29.63 x mg !!02  X  (Tf * 460)

 Vf X  (P. - Pf)
     •*'-
             \-\
                                                 z^ .  8s)

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                                                B-5
                                            i-;ox  EMISSION'
                                              "
         Run  io.
          .Oats
                                    °
          Tf  -  Flo.?.!; Ter,i|>e>r£ture,   F
          Vf  -  Flask VcU;:ne,  liters
          P.. -  Initial H^s';  Vocuu;:!,  "Kj.
          Pf-  Final  Flask Vacuum,  "Hg.

          ppm  i.'Cp'
'"
         ppm
                    29.63 x mg NO 2   X  (Tf + 460)
Vf  X
                                 -  P)

-------
                               r;fX.B~fcssjc:; DATA
Run io.
.Date
mg N0?
T,r - Flo?.!; Tempora lure, °F
Vf - Flask VcUi.-.ie, liters
P -. - I n i ti a 1 Fl as k V';; ci:u;n , !1 K j .
Pf- Final Flask Vacuum, "Hg.
ppni UCj
i-i
Z^M...
0.111.
•jz-
2.0^0
Z*
16
£2..*?
«/-z
^^ Mftv
o o"
32-
2.031
2-S"
0-5
&.f
1
am-u
O.HL
3,
^.^

I- 3
$CG
                                                         2-2.
                                                                sz
                                                             "V
                                                                       2-?
                                                                      6 ,
         29.63 x mg K02  X  (Tf
ppm N02=  r
           /f  X  (P, -

-------
                                     C-l






SRL 1281  35 0472
                                 APPENDIX C




                                 FIELD  DATA
      SCOTT RESEARCH LABORATORIES, INC

-------
        -i  I
                                     -?
                                     <—
                  ant
**<    _
Location

Operator

Date,	
                Run No.

Sampl-e Box  No.

Meter Box No.

   er AHg 	

  Fact9i»
                                                                             Ambient; Temperature

                                                                             Barometric Pressure
                                                                             Assumed Moisture,  %

                                                                                       Setting _
                                                                          ™3MM&...
                                                               Schematic Of Stack Cross Section
                                                                                                                            1,
                                                                                                                   ter,  In. _
                                                                                                                    Setting _
                                                                                                                    t6$0
Traverse  Point
    Number
Sampling
  Time
(6) min.
   Static .« 0
  Pressure"!,
'
                     "
                                                                                           '97

                                                                         ,'
                                                                     ,/
                                                                                           Avg.

-------
Plant 	
Location
Operator
Date	
Run -No. 	
Sample Box Ho
Meter Box No.
Meter AHg
C Factor
Ambient Temperature
             W -    ~"
Barometric Pressure _
Assumed Moisture,  X _
Heater Box Setting 	
Probe Length, m. _,	._
Nozzle Diameter, la.
Probe Heater Setting
                                                            of Stack Cross Section

-------

Plant - ^
' Location *
Operator
Date
Run No. / ' ^

Sample Box No. -

i
Traverse Point
Number
/t-Z
•\
;-i
z~~"
*
-.,
k
(. •**
• /a

^Tptal - ,.,.
Meter Box
Meter AHg
C Factor
No.
'
V
;•
Sampling
Time
(6) mln.
C
' •' •-
' '?






~-?
~1 *
Average
r
Static
Pressure
(Ps) In. Hg.
.7^
'' ' /
• - r
i ^1.
•" ' ' 'v
I, o
/,/<"""
1^0
}<\&
I _:;,x-~
^"'- '
«•
Stack
Temperature
(Ts) °F













''
' ° • ~
•
. ..^
•' <
6
*
» t
Schematic of Stack Cross Section
C>
Velocity
Head
(APB)
>,f
/,. ,.
./, ,
,'" , —
IK'
/, r-
^y
/, -..
l^
/ ••:.•
( '- ' fr
•/
^
Pressure
Differential
Across
Orifice (1
Meter f
(AH)
In. H20
- •';' •
^y -

F
! _ ;.;/

r,/
'.
*ljf /
*-£.._
•'i, ,^'^"3
/
Gas Sample;
Volume,
(Vm) ftJ
\ '"••'
•i-f'/fl
^7
&?t ><*b
/,' ; ': <" • s"
*< -
fT^


05V2

Ambient Temf
Barometrifct I
» •:,-.. *
Assume^ Wbif
r
Heatej Box £
Probe» Lengtt
Nojizle Diamt
Probe Heatei
* '
«
*V V"
Gas* Sample Temperature
at Dry G s Meter
Inlet
(Tmin)°F
V f.
v-

""7 ' L '
~**\ > J
") S" 	
7b
,•••" v'fl.
'"'•' 7
AV87^
1
•
>erature - ...j
"ressure 4
i'ture, %
etting •
tim. * H*
;ter, In. *
• Setting i ,•
*
*
•;• •
Sample Box
Temperature
1 ^
*



i:


,»
«»-
• -.•*/
,.
Tempe rat ufe^^
Condenser or
Last Injpinger
b*
' £ J
- / J
-' / f
^X^A0
(^ ^
," *"?
(^7"
X ^J^
K'"'? IT
^
"> Z-
>z^-
-

?
4S

-------
        &•
                Plant 	
               ' Location
                Operator
                Date
                Run No.
Sample Box No.
Meter Box No.
Meter AHg 	
C Factor

                                                                                   Ambient Temperature

                                                                                   Barometric Pressure

                                                                                   Assumed Moisture, %

                                                                                   Heater Box Setting 	

                                                                                   Probe Length, m.,

                                                                                   Nozzle Dianeter,4ln.

                                                                                   Probe Heater Setting
                                                             Schematic of Stack Cross Section
Traverse Point
    Number
Sampling
  Tine
(0)  min.
             Static
            Pressure
          (Pfl)  In. Hg.
                                  Stack
                               Temperature
Velocity
  Head
  Pressure  t
Differential
    ross
   rifice
   Meter
    (AH)
  In. H20
Gas Sample
  Volume.
 (Vm) ftj
                                                                                                Temperature
                                                                                            DryGas Meter
/ Inlet.
  Outlet
(Tm   )°F
  out
 Sample Box
Temperature
                                                                                                                          '• Temperature
Condena^'r or
Last Impinger
                                                     1*1
                                                                                              ,-*'
                                                                                                           72.
      f
t
           AC.
                                     £7
                                                                                                                           70
                           A?
                                       7
                                                              -?   v •
                                                                       fdj  '
      "

                                                                       fOb


                                                               •i.7
      1-2--'

                                                                                       Ay
                                                                                                                                    -V
Total
          /. /
                                                                       Avg. K (
                                                                                                  Avg.
                                                                                                                             f
Average
                                                                       Avg.

-------
                                      C-6
                                                                                   7
                              WATER  VOLUME
Run No
                 .  /
Date
          Bubbler *
                                Silica Gel No.  61    Wgt. g. t> ' ^> c 3>
                  n  I b
                                          Bubbler tf
                                                                        .  O
         Gross
 Water Added (-)
                               Gross T,Jgt.(-)
       Net
          (A)
                                  Net
                                      (B,
                             Net
                                 (A)
                             Net    (+)
                                 (B)
                                        34.7
               Total Water	06^? / > /
                                       cc
Fom R&D 109

-------
               Plant
                             i
                             '  *       ,
                            •I         'Sp
                       kC *•!-..; -g|f.\r i.,''
               Sample Box No..
                  V
               Meter Box No.
               Meter *Hg       /.,
               C Factor      A
                                                                                   Ambient Temperature

                                                                                   Barometric Pressure   "2-//

                                                                                   Assumed MpJja&W^i. % _£

                                                                                  .••«Hoir'- Box Setting

                                                                                   Probe Length, m. 	

                                                                                   Nozzle Diameter, In.

                                                                                   Probe, Heater Setting
                                              Schematic of Stack Cross Section
Traverse Point
    Number
'Sampling
  Time
 (6) min.
.Jfelpcity
'   Head
  Pressure
Differential
  Across
  Orifice
   Meter '
    (AH)
  In. H20
7i U

Gas

 (Vm) ft
                                                                                  ^L I  Gas Sample Temperature
                                                                                  ^^^K- •   At- T)w ^ a MA«-A^
                                                                                         at Dry G
 Inlet
(Tmln)°F
          s Meter
                                                 Outlet
                                                (Tm   )°F
                                                  out
 Sample Box
Temperature
     F
•
Temperature
   leaving.
Condenser, or
Last Impinger
     ,' f '
                /o
                                               us
                                               •hZ.
                                                                                                   TO
                                                    -
                                     t.H
           /
                                     £L
                                                                                                   r
                                                                                                   -T?-
                                                              ''
Total
                                     /-r
Average
                                                                        A»s.
                                                                                                          .:>-»*

-------

Plant
Location
Operator
Date **
Run No. "2^ ;pf

Sample Box No.

Traverse Point
Number
,<>
|
. ( 7-
.'$>
f >
^ '
./ y
xa
i /
f - i
--.
Total "j. '*' \ •*-'<
Meter Box
Meter iHg
C Factor
No.

^

Sampling
Time
(6) min.
5 V-
N -. V , ,
-, / *"*:~*
..} ^
,..:• )
,'. . v-
4' v -
> s, —-
rs
5~$«^"
5T~
60
Average •->.
Static
Pressure
(P ) In. Hg.
O
'r S~~
l>€
/C ^
A b
rr i^f
'c V
f/3
/.a
" ' D
• i *^
Stack
Temperature
(Tg) 5F
/^.o





/






/

A i I/
</^^-r
7sv.,5-r
>n(j^
irr.j^
ls-7,7^
7«i-/?^


Gas Sample Temperature
at Dry G s Meter
Inlet
(Tmln)°F
' £-£.
fr^
fr**
S-t
f-y .
• g-c.
^ r
f -7
^
*n
Avg.^j./
Outlet
P-— ,.^-
f !T~
rs>
rt
r ^?
r 7
• r ?
.r?:^
/^
^X
Avg. / X
Avg.

Sample Box
Temperature











„
Temperature
Leaving
Condenser or
Last Impinger
°F

(e 5^
^>
$f- *
& i
<£~-
& *-r~~
i'



•

-------
                Plant ;	
                Location

                Operator

                Date 	
                Run No.
                Sample Box No.

                Meter Box Mo.

                Heter AHg 	

                C Factor
                                                                                                             i 0
                                                                                      Ambient Temperature _

                                                                                      Barometric Pressure

                                                                                      Assumed Moisture, %

                                                                                      Heater Box Setting 	

                                                                                      Probe Length, m. 	

                                                                                      Nozzle Diameter, In.

                                                                                      Probe Heater Setting
                                               Schematic of Stack Cross Section
Traverse Point
    Number
Sampling
  Time
(6) mln.
   Static
  Pressure
(P,) In. Hg
   Stack
Temperature
                                                     Velocity
                                                       Head
  Pressure^
Differential
  Across
  Orifice
   Meter
    (iH)
  In. H20
Gas Sample
  Volume.
 (Vm)  ft3-
                                                                          Gas Sample Temperature
                                                                             at Dry Gas Meter
                                                                                           Inlet
                                                                                        Outlet
                                                                                      (Tm   )°F
                                                                                         out
 Sample Box
Temperature
Temperature
   Leaving
Condenser or
Last fmpinger
fc-    °F
                    r
                                                                u.
                                                                                       6*-
                7,5"
                /(D
                                                  Z-.i
                                                                                                                                 I
                                                                                                                                 VD
                                                                                  7 /
       6-
1ZO
      (Q
      rr
Total f~l _
50
                                                     2-,
Average
                                                                          Avg.

-------
Plant 	
Location
Operator
Date
Run Ho.
             1.  &
Sample Box No.
Meter Box No.
Meter AHg 	
C Factor
Ambient Temperature
Barometric Pressure  r~ /f j ^/ '
Assumed Mois.ture, % 	
Heater Box Setting 	
Probe Length, m. 	
Nozzle Diameter, In. 	
Probe Heater Setting 	
                                                 Schematic of Stack Cross Seetion
Traverse Point
Number
f>
rn
^
t
f •--,
•':>
4f
;:.:->
f~f
*
Total ">. •"?-••'
Sampling
Time
(8) min.
*> ••-> r~~
".>--•' !
3T
'„>?' >
-v -o
~, • . .--_.
- •
', '"•• "-—
,^
r- ..v «—-
V L*
>-o
•Average f • ~:\.
Static
Pressure
(Po) In. Hg.
S
/I"?
^^
/r'7
0
A -7
(<*$
fi<0
>r
>if
n^
ibf

Stack
Temperature
(Tg) °F
1








\
\
a







1

J

Velocity
Head
(APB)
'' 7-
;'/ 7
A -7
I, r-
^ s-
/.r
A^
/?7
A^
/f 7
ff^-
i.
Pressure
Differential
Across
Orifice
Meter
(AH)
In. H20
2V
^ ' / .
-7 , (
'*•*(
\
»*l
''?
2>(
2-« 5k-
1J
> J^
z, (

Gas Sample
Volume,
(Vm) ftj
>4v
T^^-^r
7f/, /,/
m, t.
•??r,vr
7^V%-
7^f-X
£» '. ' 5
g6i»/
^f'^^f ^ /
^,^

Gas Sample Temperature
at Dry G s Meter
Inlet
(Tmin)°F
g 5"
i^
6> ^ ,
ir<* ••••_*
S /
8 -V
rv
9 -
4"^ ^i»~"
1Y
Avg.^ ^
Outlet
(Tm ) F
v out
&y
^j
.^ y
-'."' ^;..
; "/ ^J
(cS
J-l
>
&£,

-------
                                    C-ll
                              WATER  VOLUME
          Run No.
 Date
          Bubbler /'
 Silica Gel No.
                                         Bubbler
         Gross
 VJater Added (-)
       Net
          (A)
                            cc
Gross Wgt.(-) C/3
Net
      (B)
                  f.
                             Net   (+)  ^ T
                                (B)
               Total Water
                                                cc
                      r-
Fom R&D 109

-------
 Plant _
"Location

 Operator

 Date
                                                IT  ~!
                                    O
               Run No.
 Sample Box No.

 Meter Box No.

 Meter AH0
                      g
                              1',
                                                                      Ambient Temperature

                                                                      Barometric Pressure. 	

                                                                      Assumed Moisture, % 	/

                                                                      Heater Box Setting 	
                                                                                       •
                                                                      Probe Length, m. 	

                                                                      Nozzle Diameter, ,In.  / >

                                                                      Probe Heater Setting 	
               C Factor
                                            Schematic of Stack Crosfi Section

                                            O
Traverse Point
   Number
 Sampling
  Time
 (9) min.
  Static
 Pressure
(Pg) In. Hg.
   Stack
Temperature
      °
Velocity
  Head
  Pressure
Differential
  Across
  Orifice
  Miter
    (AH)
  In. *20
                                                                            , C
Gas Sample
  Volume.
 (Vm) ft"
                                                                                   Gas Sample Temperature
                                                                                     at Dry G s Meter
                                   Inlet
                                   (Tmln)°F
Outlet
    °
                                                                                                 out
 Sample Box
Temperature
Temperature
   Leaving
Condenser or
Last Impinger
       ff
                                              '-7
                                                                                   nr-
                ,• • V

                                                 A /I
                                                                                   7>
                                                           lO-
        Y.
                                                                                                       tU-
       A
                                             /  ' **
                                             /.
                                                          71
                                                                                                                      FT-
Total
Average
                                            z,/
                                                                                             60
                                                                     Avg.

-------
                Plant .,	
                Location
                Operator

                Date
Run No.       ^

Sample Box No.

Meter Box No.

Meter AHg 	

C Factor 	
                                                                                       Ambient Temperature _

                                                                                       Barometric Pressure _

                                                                                       Assumed Moisture, % _

                                                                                       Heater Box Setting	

                                                                                       Probe Length, m. 	

                                                                                       Nozzle Diameter, In.

                                                                                       Protre Heater Setting
                                                                Schematic of Stack Cross Section
Traverse Point
    Number
Sampling
  Time
(6) rain.
             Static
            Pressure
           (Ps) In. Hg.
   Stack
Temperature
  (T8)  5F

Velocity
  Head ijg.
  Pressure
Differential
  Across
  Orifice
   Meter
    (AH)
                                                                  In.
                H20
Gas Sample
  Volume.
 (Vm)  ftj
                                                                                           Gag Sffinple T.^)etature
                                                                                              at Dry 'Ggg Hetet
bilet
Outlet
 Sample Box
Temperature
Temperature
   Leaving
Condenser  or
Last Impinger
                 I
                                                                            7?
                                                                                                                   (f
                                                      A?
                                                                                            r-y
                                                                                                                *'-
                                                                                                                                                      .*
                                                         i
                cv
                                                                                             o   ,
                                                                                     (.6
Total
          4-
Average
                                                                                                                ;• 'sf^iS^f^i^S,.'-.  :iftt .. '.,'.   '•'•'• •\.
-------
                -:  t

                 Plant 	
                 Location
                 Operator
                 Date
                Run No.
                                                           •,*, :
Sample Box No.

Meter Box No.

Meter AHg	

C Factor
                                                                                         Ambient Temperature _

                                                                                     .i.  Barometric Pressure
                                                                                     •«                    * —
                                                                                         Assumed Moisture, % _

                                                                                         Heater Box Setting _J_

                                                                                         Probe Length, m.	

                                                                                         Nozzle Diameter, In.

                                                                                                     Setting
                                                                 Schematic of Stack Cross Section
Traverse Point
    Number
Sampling
  Time
(9) min.
              Static
             Pressure
           (P=)  In. Hg.
   Stack '
Temperature
  (Ts)  °F%
Velocity
  Head
 Pressure
ifferential
 Across
 Orifice
  Meter
   (AH)
 In.  H20
Gae Saople
  Volume.
 (Vn)  ftj
                                                                                             Gas  Sample Temperature
                                                                                               at Dry G s Meter
                                        Inle
  Outlet
(Tm  _>s
   out
 Sample Box
Temperature
Temperature
   Leaving
Condenser or •
Last Impinger
        t.f J-
   r
                                                                                                                     -70
                 7
               -
              * /^"
              o 0
                                                                   v, y
                  /o

                                                                   1,  f
                                                                                                                                                  '«•*(

          7
r/r
                                      %

                                                                   2,
          '
Total
                                                                                               -,/
Average
                                                                            Avg.

-------
                                                                                    -;
                                                                                 V
                Plant 	
                Location
                Operator

                Date
                Run No.
                Sample Box^No.

                Meter Box No.
                Meter AHg

                C Factor
                                                                                   Ambient Temperature

                                                                                   Barometric Pressure _

                                                                                   Assumed Moisture, % _

                                                                                   Heater Box Setting 	

                                                                                   Probe Length, m. 	

                                                                                   Nozzle Diameter, In.

                                                                                   Probe Heater Setting
                                             Schematic of Stack Cross Section
Traverse Point
    Number
Sampling
  Time
(6)  min.
   Static
  Pressure
(P8) In. Hg.
   Stack
Temperature
  (T8) 6F
Velocity
  Head
 (AP8)
  Pressure
Differential
  Across
  Orifice
   Meter
    (AH)
                                                                In.
     H20
Gas Sample
  Volume.
 (Vm) ftj
                                                                                       Gas Sample Temperature
                                                                                          at Dry G s Meter
Inlet
Outlet
 Sample Box
Temperature
    °
    . V

Temperature
   Leaving
Condenser or
Last Implnger
        a
         t
                                     14-
                                                                                        0
                                                                                                   60
                                                                               71
                                                                           ?
                                                                                                       '*:
                                                   A
                                                   /.r
                                                                                        77
                                                                                   66	1

Total'
                                                                                                             57
Average

-------
                                     C-16
                               WATER  VOLUTtE
          Run No.
                                 Date
Bubbler /(
                               H/vC
                                           Silica Gel No.       Wftt.  g
                                          Bubbler il
         Gross
 Water Added(-)
                                Gross TJgt.(-)     <. /S>.  g
       Net
          (A)
                             cc
                                   Net
                                      (B)
                              Net
                                 (A)
                              Net   (+)
                                 (B)
               Total Water
                                                 cc
Fom R&D 109

-------
                                                                                            Ambient Temperature

                                                                                            Barometric Pressure

                                                                                            Assumed Moisture, Z

                                                                                            Heater Box Setting _.

                                                                                            Probe Length, m
Istratinn

Operatbr

Date
Sample Box No

Meter Box No,
Mater AHg

CF
                                                                                            Nozzle Diameter, In.
                                                                                            Probe Heater Setting
                                                  Schematic of Stack Cross Section
                                                     Pressure
                                                   Differential
                                                                                                                       Temperature
                                                                                                                          Leaving
                                                                                                                       Condenser or
                                                     ^Orifice
                                                      Meter
                                                       (AH)
Gas Sample Temperature
   at Dry Gas -Meter
Velocity
  Head
      '
                                                                                                                       Last Jmpinger

-------
                Plant 	
                Location

                Operator

                Date
                Run No.
                Sample  Box No.
                Meter Box No.
                Meter AHg 	
                C Factor
                                                                                      Ambient Temperature
                                                                                      Barometric Pressure

                                                                                      Assumed Moisture, %

                                                                                      Heater Box Setting

                                                                                      Probe Length, m.

                                                                                      Nozzle Diameter, In.

                                                                                      Probe Heater Setting
                                               Schematic of Stack Cross Section
Traverse Point
    Number
Sampling
  Time
(6) min.
   Static
  Pressure
Sft£lur£
                                                                               .£.:*»*

-------
;:r^T:'•  •T'TTT^" •TT7~"'--:7Ji;,1^.'.'.-* -•-  T'~ •>'.• ^:-,t'••" ;".    " " "
-;..•;••; ^y^9^v#.  ,.•  ;  ?  • •-.:' •-.-..
6

Plant
Location
Operator
Date
Run No. ff / C?

•



i
Sample Box No.

Traverse Point
Number
;-./*T_
^
^

'6 '
L -- :
: - "7
; fr
^f
to
? f
tota! r^
Meter Box
Meter AHg
C Factor
No.






Sampling
Time
(6) min.
'TT
7. 9-
^
fi~,r
\r'
nr
i-& ,
II,T
ar
M>
•^c>
Average
Static
Pressure
(Ps) In. Hg.



'••





&


Stack
Temperature
 •
Barometric Pressure
Assumed Moisture, X
•<
Heater Box Setting
Probe Length, m.
Nozzle Diameter, In.
Probe Heater Setting
•
Schematic of Stack Cross Section
Velocity
Head
(AP8)
f,$^
^
1^
t>H
t>b
l*b
14
k*J
ttf

\>0
-&2~

Pressure-
Differential
Across
Orifice
Meter
(AH)
In. H20
I,/
/>#
4 Cf
( 2.
XI
2.V

X. f
3>/

Gas Sample
Volume.
(Vm) ftj
1*W(
'^iijx
*ffO'i(*j
IWST
n^^
ox

*
Gas Sample Temperature
at Dry Gas Meter
Inlet
(Tmln)°F
£0
<
n-g
t f
Avg.^7,
Avg.

Sample Box
Temperature
*-•




-.





„
Temperature
Leaving
Condenser or
Last Impinger
°F
TO
rP\'
Y& •

4*
r&*


r~v . •=
. gr-v


                                      **.
                                  VO
                                       4

-------

Plant
Location
-?,
Operator
Date
Run No. • /«i
Sample Box No. .

Traverse Point
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-------
                                         C-27
LABORATORY TEST SHEET
                                           LABORATORY
4NO-GEN- I I IB

-------
                                       C-28
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                                        LABORATORY
 4NO-GEN-I I 28
 TEST ENGINEER
  TEST EQUIPMENT
1
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                                OBSERVERS
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                                   D-l





SRL 1281 35 0472
                               APPENDIX D




                      STANDARD SAMPLING PROCEDURES




          The sampling procedures used during  the test  are  the same as




those published in the Federal Register, Volume  36, Number  247,  Thursday,




December 23, 1971.  These methods are as follows:  Methods  1,  2,  3, 4,  5,




and 7.  In addition,  the impinger catch was analyzed.
     SCOTT RESEARCH LABORATORIES, INC

-------
 method (s)  prescribed by the manufac-
 turer(s) of such Instrument, the Instru-
 ment shall be subject to manufacturers
 recommended zero adjustment calibra-
 tion procedures at least once per 24-hour
 operating  period unless the  manufac-
 turer^) specified or recommends cali-
 bration  at shorter intervals, hi  which
 case such specifications or recommenda-
 tions shall be followed.  The  applicable
 method specified in the appendix of this
 part shall be the reference method.
   (c) Production rate and hours of op-
 eration shall be recorded dally.
   (d) The owner or operator of any sul-
 furic acid production unit subject to the
 provisions of this  subpart shall maintain
 a  file of all measurements required by
 this subpart. Appropriate measurements
 shall be reduced to the units of the ap-
 plicable standard daily and summarized
 monthly. The record of any such  meas-
 urement and summary shall be retained
for at least 2 years following the date
 of such measurements and summaries.
 § 60.85  Test methods and procedures.
   (a) The provisions of this section are
 applicable to performance tests for deter-
 mining emissions of acid mist and sulfur
 dioxide from sulfuric acid production
 units:
   (b) All performance tests shall be con-
 ducted while the affected facility Is oper-
ating at or above  the  maximum acid
production  rate  at which  such facility
will be  operated  and under such other
relevant conditions as the Administrator
shall specify based on representative per-
formance of the affected facility.
   (c) Test methods set forth in the ap-
pendix to this part or equivalent methods
as approved by the .Administrator shall
be used as follows:
   (1) For  each repetition the add mist
and SO, concentrations shall be deter-
mined by using Method 8 and  traversing
according  to  Method 1.  The  mtnimn^n
sampling time shall be 2 hours, and mini-
mum sampling  volume shall  be 40 ft.'
corrected to standard conditions.
   (2) The volumetric flow rate  of the
total effluent shall  be determined by using
Method  2  and traversing  according to
Method 1.  Gas  analysis  shall be per-
formed by  using the integrated sample
technique of Method 3. Moisture content
can be considered to be zero.
   (d) Acid produced, expressed In tons
per hour of  100 percent sulfuric acid
shall  be determined during each 2-hour
testing period by suitable flow meters and
shall be confirmed by a material balance
over the production system.
   (e) For each repetition acid mist and
sulfur dioxide emissions, expressed In lb./
ton of 100 percent sulfuric acid shall be
determined by dividing the emission rate
in Ibi/hr.  by the  acid produced. The
emission  rate shall  be determined  by
the   equation,   lb./hr.=QsXc,   where
Qa=volumetric flow rate of the effluent
in ft.'/hr. at standard conditions, dry
basis  as determined In accordance with
paragraph  (c)(2)  of this section, and
c=acld mist and SO, concentrations in
Ib./ft.' as determined in accordance with
paragraph  (c)(l)  of this section, cor-
rected to standard conditions, dry  basis.
        APPENDIX—TEST METHODS
METHOD  1—OUIFZJI AND VELOCITY TRAVERSES
         1OB STATIONARY SOURCES
  1. Principle and Applicability.
  1.1  Principle.  A sampling site and the
number  of traverse points are selected to aid
in the extraction of a representative sample.
  1.3  Applicability.  This  method  should
be applied only when  specified by the test
procedures for determining compliance with
the New Source Performance Standards. Un-
less otherwise specified, this method  is not
Intended to apply to gas streams other than
those  emitted directly  to  the atmosphere
without  further processing.
  2. Procedure.
  2.1  Selection of a ^^nyiing site and mini-
mum number of traverse points.
  2.1.1   Select a sampling site that Is at least
eight stack or duct diameters downstream
and two diameters upstream from any flow
disturbance such as a bend, expansion, con-
traction, or  visible flame.  For rectangular
cross section, determine an equivalent diam-
eter from the following equation:
                      2.1.2  When  the  above  sampling,  site
                    criteria can be  met, the minimum number
                    of traverse points Is twelve (12).
                      2.1.3  Some sampling situations render the
                    above  sampling site  criteria  Impractical.
                    When this Is the case, choose a convenient
                    sampling location and use Figure 1-1 to de-
                    termine the minimum number of traverse
                    points. Under no conditions should a sam-
                    pling point be selected within 1 inch of the
                    stack wall. To obtain the number of traverse
                    points for stacks or ducts with a diameter
                    less  than 2 feet, multiply the number of
                    points obtained from Figure 1-1 by 0.67.
                      2.1.4  To use  Figure 1-1 first measure the
                    distance from the chosen sampling location
to the nearest upstream and downstream dis-
turbances.  Determine  the  corresponding
number of traverse points for each distance
from Figure 1-1.  Select the higher of the
two numbers of traverse points, or a greater
value, such that for circular stacks the num-
ber is a multiple  of 4, and for rectangular
stacks  the  number follows the criteria of
section 2.2.2.
  2.2  Cross-sectional layout and location of
traverse points.
  2.2.1   For  circular, stacks locate the  tra-
verse points on at least two  diameters ac-
cording to Figure 1-2 and Table 1-1.  The
traverse axes shall divide the stack cross
section Into equal  parts.
                                                 NUMBER OF DUCT DIAMETERS UPSTREAM'
                                                         (DISTANCE A)
                           0.5
                                  FROM POINT OF ANY TYPE OF
                                  DISTURBANCE [BEND. EXPANSION, CONTRACTION. ETC.)
equivalent diameter=2i
/(length) (width) \
\  length+width /
      equation 1-1
                                                NUMBER OF DUCT DIAMETERS DOWNSTREAM*
                                                           (DISTANCE B)
                                                                 FlfluraM. Minimum number of traverse points.
                                                  FEDERAL REGISTER, VOL.  36, NO. 247—THURSDAY, DECEMBER 23, 1971

-------
                                                                                        Tabla 1-1.  Location of traverse points in circular stacks
                                                                                      (Percent of stack diameter from inside wall to traverse point)
 Figure 1-2.  Cross section of circular stac'k divided Into 12 equal
 areas, showing location of traverse points at  centroid of each area.


O


..-—-.-

0

o
1
i
o .[ 9
i
_.. 	 i 	
r > i
i
O | " O
, 	 r- — --^
I
O | O
1


0




o
•~ — ~"

o
Figure 1-3.  Cross section of rectangular stack divided into 12 equal
areas, with traverse points at centrpid of each area.
Traverse
point
number
on a
diameter
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
Number of traverse points on a diameter* .
2
14.6
85.4





















4
6.7
25.0
75.0
93,3




















6
4.4
14.7
29.5
70.5
85.3
95.6


















8
3.3
10.5
19.4
32.3
67.7
80.6
89.5
96.7
















10
2.5
8.2
14.6
22.6
34.2
65.8
77.4
85.4
91.8
97.5














12
2.1
6.7
11.8
17.7
25.0
35.5
64.5
65.0
82.3
88.2
93.3
97.9












14
1.8
5.7
9.9
14.6
20.1
26.9
36.6
63.4
73.1
79.9
85.4
90.1
94.3
98.2










16
T.6
4.9
8.5
12.5
16.9
22.0
28.3
37.5
62.5
71.7'
78.0
83.1
87.5
91.5
95.1
98.4








18
1.4
4.4
7.5
10.9
14.6
13.8
23.6
29.6
33.2
61.8
70.4
76.4
81.2
85.4
89.1
92.5
95.6
93.6






20
1.3
3.9
6.7
9,7
12.9
16.6
20.4
25.0
30.6
38.8
61.2
69.4
75.0
79.6
83.5
87.1
90.3
93.3
96.1
98.7




22
1.1
3.5
6.0
8.7
11.6
14.6
18.0
21.8
26.1
31. 5
39.3
60.7
68.5
73.9
78.2
82.0
85.4
83.4
91.3
94.0
96.5
9S-.9


24
1.1
3.2
5.5
7.9
10.5
13.2
16.1
19.4
23.0
27.2
32.3
3.9.8
60.2
67.7
72.8
77.0
80.6
83.9
86.8
89.5
92.1
94.5
96.8
98.9
                                                                                                                                                      i
                                                                                                                                                      SO
                                                                                                                                                      m
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                                                                                                                                                      z
                                                                                                                                                      v>
      No. 247—Pt. H
                                              FEDERAL REGISTER, VOL. 36, NO. 347—THURSDAY, DECEMBER 23, 1971

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24884
      RULES AND  REGULATIONS
  2.2.2  For  rectangular  stacks  divide  the
cross section into as many equal rectangular
areas as traverse points, such that the ratio
of the length to the width of the elemental
areas Is between one and two.  Locate  the
traverse points at the centroid of each equal
area according to Figure 1-3.
  3. References.
  Determining Dust Concentration In a  Gas
Stream, ASME Performance  Test Code #27,
New Tort, N.Y.. 1957.
  Devorkln,  Howard,  et  al., Air  Pollution
Source Testing Manual, Air Pollution Control
District, Los Angeles, Calif.  November 1963.
  Methods for  Determination of  Velocity,
Volume, Dust  and Mist  Content of Gases,
Western Precipitation Division of Joy Manu-
facturing  Co.,  Los Angeles,  Calif. Bulletin
WP-50, 1968.
  Standard Method for Sampling Stacks for
Particulate Matter, In: 1971 Book of ASTM
Standards, Part 23, Philadelphia,  Pa. 1971,
ASTM  Designation D-2928-71.

METHOD  2—DETERMINATION  OP  STACK  GAS
  VELOCITY AND VOLUMETRIC PLOW RATE (TYPE
  B PITOT TUBE)

  1. Principle and applicability.

  1.1  Principle. Stack  gas velocity is deter-
mined from the gas density and from meas-
urement of the velocity head using a Type S
(Steuschelbe or reverse type) pitot tube.
  1.2  Applicability. This method should be
applied only when specified by the test pro-
cedures for determining compliance with the
New Source Performance Standards.

  2. Apparatus.
  2.1 Pitot tube—Type 8  (Figure 2-1), or
equivalent, with a coefficient  within ±6%
over the working range.
  2.2 Differential pressure gauge—Inclined
manometer, or equivalent, to measure velo-
city head to within  10%  of  the minimum
value.
  2.3 Temperature gauge—Thermocouple or
equivalent attached  to the pitot tube to
measure stack temperature to within 1.5% of
the  minimum  absolute stack temperature.
  2.4 Pressure gauge—Mercury-filled U-tube
manometer, or equivalent, to  measure stack
pressure to within 0.1. in. Hg.
  2.5 Barometer—To measure atmospheric
pressure to within 0.1 in. Hg.
  2.6 Gas analyzer—To analyze gas composi-
tion for determining molecular weight.
  2.7 Pitot  tube—Standard  type, to cali-
brate Type S pitot tube.

  3. Procedure.
  3.1 Set up the apparatus as  shown In Fig-
ure 2-1.' Make sure all connections are tight
and leak free. Measure the velocity head and
temperature at the traverse points specified
by Method 1.
  3.2 Measure  the static  pressure  in  the
stack.
  3.3 Determine  the stack gas molecular
weight  by gas analysis and appropriate  cal-
culations as Indicated in Method 3.
  4. Calibration.

  4.1 To calibrate the pitot tube, measure
the velocity head at some point in a flowing
gas stream with both a Type 8 pitot tube and
a standard type pitot tube with known co-
efficient. Calibration should  be done in the
laboratory and the velocity of the flowing gas
stream  should be  varied  over the normal
working range. It is recommended that the
calibration be repeated after use at each field
site.
  4.2 Calculate the pitot tube coefficient
using equation 2—1.
                              equation 2-1
where :
  CP ,,,„,= Pi tot tube coefficient  of Type  S
            pitot tube.
   Cp,,d=Pltot tube coefficient of standard
            type pitot tube (if unknown, use
            0.99) .
   Apsttd=Absolute pressure at standard conditions, 29.98
                                                    Inches Hg.
                                 FEDERAL REGISTER, VOL 36, NO.  247—THURSDAY, DECEMBER 23, 1971

-------
                          RULES AND  REGULATIONS
                                                                   24885
  6. References.

  Mark, L. S., Mechanical Engineers' Hand-
book, McGraw-Hill Book Co., Inc., New York,
N.Y., 1951.
  Perry, J.  H.,  Chemical  Engineers' Hand-
book, McGraw-Hill Book Co., Inc., New York,
N.T., 1960.
  Shigehara, R. .T., W.  P. Todd, and W. S.
Smith, Significance of Errors in Stack Sam-
             pling Measurements. Paper presented at the
             Annual Meeting of the Air Pollution Control
             Association, St. Louis, Mo., June 14-19, 1970.
               Standard Method for Sampling Stacks for
             Particulate Matter, In:  1971 Book of  ASTM
             Standards, Part 23, Philadelphia, Pa.,  1971,
             ASTM Designation D-2928-71.
               Vennard, J. K., Elementary Fluid  Mechan-
             ics, John Wiley & Sons,  Inc., New York, N.Y.,
             1947.
  PLANT.

  DATE
  RUN NO.
  STACK DIAMETER, in.
  BAROMETRIC PRESSURE, in. Hg.
  STATIC PRESSURE IN STACK (Pg), in. Hg.
  OPERATORS
                              SCHEMATIC OF STACK
                                 CROSS SECTION
          Traverse point
             number
Velocity head,
   in. H20
                                                              Stack Temperature
                                AVERAGE:
                        Figyra 2-2. Velocity traverse data.
         FEDERAL REGISTER, VOL. 36,  NO. 247—THURSDAY, DECEMBER 23, 1971

-------
 24886
                                           RULES  AND REGULATIONS
 METHOD 3	GAS ANALYSIS FOB CARBON DIOXIDE,
   EXCESS AIB, AND DRY MOLECULAE  WEIGHT

   1. Principle and  applicability.
   1.1  Principle. An Integrated or grab gas
 sample  Is extracted from a sampling point
 and analyzed for Its components  using an
 Great analyzer.
   1.2  Applicability. This method should be
 applied  only  when specified by the test pro-
 cedures for determining compliance with the
 New Source Performance Standards. The test
 procedure will Indicate whether a grab sam-
 ple or an Integrated sample is to be used.
   2. Apparatus.
   2.1  Grab sample (Figure 3-1),
   2.1.1   Probe—Stainless  steel  or  Pyrex1
 glass, equipped with a filter to remove partic-
 ulate matter.
   2.1.2  Pump—One-way  squeeze  bulb, or
 equivalent,   to  transport  gas  sample  to
 analyzer.
   i Trade name.
                                       2.2  Integrated sample (Figure 5-2).
                                       2.2.1  Probe—Stainless  steel  or  Pyrex1
                                     glass,  equipped with a filter to remove par-
                                     ticulate matter.
                                       222  Air-cooled condenser or equivalent—
                                     To remove any excess moisture.
                                       2.2.3  Needle valve-^To adjust flow rate.
                                       2.2.4  Pump—Leak-free,  diaphragm  type,
                                     or equivalent, to pull gas.
                                       2.2.5  Bate  meter—To  measure  a flow
                                     range from 0 to 0.035 cfm.
                                       2.2.6  Flexible bag—Tedlar,1 or equivalent,
                                     with a capacity of 2 to 3 cu. ft. Leak test the
                                     bag In the laboratory before using.
                                       2.2.7  Pltot  tube—Type S, or equivalent,
                                     attached to the probe so that the sampling
                                     flow rate can be regulated proportional to
                                     the stack gas velocity when velocity Is vary-
                                     ing with time or  a  sample  traverse  is
                                     conducted.
                                       2.3  Analysis.
                                       2.3.1 "Orsat analyzer, or equivalent.
                   PROBE
                                           FLEXIBLE TUBING
                                                                       TO ANALYZER
[ FUTE/HG
(GLASS WOOL)
                                          SQUEEZE BULB




                         Figure 3-1. Grab-sampling train.

                                              RATE I
    [  WOBE
                                    RIGID CONTAINER"
                , Figure 3-2. Integrated gas • sampling train.
  3. Procedure.
  3.1   Grab sampling.
  8.1.1  Set up the equipment as shown In
Figure 8-1, making sure all connections are
leak-free. Place the probe In the stack at a
sampling point and purge the sampling line.
  3.1.2  Draw sample Into the analyzer.
  3.2   Integrated sampling.
  3.2.1  Evacuate the" flexible bag. Set up the
equipment as shown In Figure 3-2 with the
bag  disconnected. Place  the probe In  the
stack and purge the sampling line. Connect
the bag, making sure that all connections are
tight  and that there are no leaks.
  3.2.2  Sample at a rate proportional to the
stack velocity.
  3.3   Analysis.
  3.3.1  Determine the CO2, O2, and CO con-
centrations as soon as possible. Make as many
passes as are necessary to give constant read-
ings. If more than ten parses are necessary,
replace the absorbing solution.
  3.3.2  For grab sampling, repeat the sam-
pling and analysis until three consecutive
samples vary no more than 0.5  percent by
volume for each component being analyzed.
 . 3.3.3  For integrated sampling, repeat the
analysis of the sample until three consecu-
tive -analyses vary no more than  0.2 percent
by  volume  for  each  component   being
analyzed.
  4. Calculations.
  4.1   Carbon dioxide. Average the three con-
secutive runs and report the result to the
nearest 0.1 % CO,.
  4.2  Excess air. Use Equation 3—1 to calcu-
late excess air,  and average the runs. Report
the result to the nearest 0.1%  excess air.

%EA =

         (%02)-0.5(%CQ)
0.264(% N2) - (% Oa) +0.5(% CO)

                             equation 3-1

where:
  %EA=Percent excess air.
   %O2=Percent oxygen by volume, dry basis.
   %Na=Percent  nitrogen  by volume,  dry
           basis.
  %CO=Percent  carbon  monoxide by  vol-
           ume, dry basis.
  0.264=Ratio of  oxygen to nitrogen  In air
           by volume.
  4.3  Dry molecular weight. Use Equation
3-2 to calculate  dry molecular weight  and
average the  runs. Report the result to tha
nearest tenth.

Ma=0.44(%CO.)+0.32(%02)
                        + 0.28(%NS+%CO)
                              equation 3-2

where:
     M*=3Dry molecular weight, Ib./lb-mole.
  %CO*=Percent carbon dioxide  by volume,
           •dry basis.
    %Os=Percent  oxygen  by  volume,  dry
           basis.
    %NiHPercent  nitrogen  by volume, dry
           basis.
    0.44=Molecular weight of carbon dioxide
           divided by 100.
    0.32=Molecular weight of oxygen divided
           by  100.
    0-28=Molecular weight of  nitrogen and
           CO divided by 100.
                                  FEDERAL REGISTER; VOL. 36, NO. 247—THURSDAY,  DECEMBER 23, 1971

-------
  5. References.
  Altshuller, A. P., et al.,  Storage  of Gases
and Vapors in Plastic  Bags,  Int.  J. Air &
Water  Pollution, 6:75-81, 1963.
  Conner, William D., and J. S. Nader, Air
Sampling with Plastic Bags,  Journal of the
American  Industrial Hygiene  Association,
25:291-297,  May-June 1964.
  Devorkin, Howard, et al.,  Air Pollution
Source Testing Manual, Air  Pollution  Con-
trol District, Los Angeles,  Calif., November
1963.

  METHOD 4	DETERMINATION OF MOISTURE
              IN STACK GASES

  I. Principle and applicability.
  1.1   Principle.  Moisture  is  removed  from
the gas stream, condensed, and determined
volumetrically.
  1.2   Applicability.  This method  is appli-
cable  for the  determination  of  moisture in
stack  gas only when specified by  test  pro-
cedures for determining  compliance with New
Source Performance  Standards. This method
does not  apply when liquid droplets are  pres-
ent in the gas stream* and the moisture is
subsequently used in the  determination of
stack  gas  molecular weight.
  Other  methods sxich  as drying tubes, wet
bulb-dry  bulb techniques, and  volumetric
condensation techniques may be used.
  2. Apparatus.
  2.1   Probe—Stainless  steel or Pyrex -  glass
sufficiently  heated to prevent condensation
  1 If liquid droplets are present in the gas
stream, assume  the stream to be saturated,
determine the average stack gas temperature
by  traversing according to  Method  1,  and
use a psychrometric chart to obtain  an ap-
proximation of  the moisture percentage.
  "Trade name.
and equipped with a filter to remove partlcu-
late matter.
  2.2  Impingers—Two  midget  impingers,
each with 30 ml. capacity, or equivalent.
  2.3  Ice  bath  container—To  condense
moisture In Impingers.
 • 2.4  Silica gel tube  (optional)—To protect
pump  and dry gas meter.
.  2.5  Needle  valve—To regulate gas  flow
rate.
  2.6  Pump—Leak-free, diaphragm type, or
equivalent, to pull gas through train.
  2.7  Dry gas meter—To measure to within
1% of the total sample volume.
  2.8  Rotameter—To measure a flow range
from 0 to 0.1  c.f.m.
  2.9  Graduated  cylinder—25 ml.
  2.10  Barometer—Sufficient  to  read  to
within 0.1 inch Hg.
  2.11  .Pitot tube—Type  8,  or  equivalent,
attached to probe so  that the sampling flow
rate can  be regulated proportional  to the
stack gas velocity when velocity is varying
with time or a sample traverse is conducted.
  3.  Procedure.
  3.1  Place exactly 5 ml.  distilled water in
each impinger. Assemble the apparatus with-
out the probe as shown, in Figure 4-1.  Leak
check  by plugging the inlet  to the first Im-
pinger and  drawing a  vacuum. Insure that
flow through the dry gas meter is less  than
1 % of the sampling rate.
  3.2  Connect  the probe and sample  at a
constant rate of 0.075 c.f.m. or at a rate pro-
portional to the stack gas velocity. Continue
sampling until the dry gas meter registers 1
cubic foot or until visible liquid droplets are
carried over from the  first impinger to the
second. Record temperature, pressure,  and
dry gas meter readings as required by Figure
4-2.
  3.3  After collecting the sample, measure
the volume Increase to the nearest 0.5 ml.
  4.  Calculations.
  4.1  Volume of water vapor collected.
                     Vwo =
                           (Vf-Vi)pH2oRTatd
                                                      ml.
                                                                          equation 4-1
 where:
    Vwc=Volume of  water vapor  collected
           (standard conditions), cu. ft.
     Vt=Final volume of impinger contents,
           ml.
     Vi=Initial volume  of  Impinger  con-
           tents, ml.
     R=Ideal  gas  constant,  21.83  Inches
          Hg—cu. ft./lb. mole-°R.
   pn'2o=:Density of water, 1 g./ml.
   Tstd=Absolute temperature at standard
          conditions, 530° R.
   Pstd=Absolute pressure  at standard con-
          ditions, 29.92 Inches Hg.
   MHOO=Molecular weight  of water, 18 lb./
          Ib.-mole.
      HEATED PROB1
FILTER'(GLASS WOOL)
                                                                           ROTAMETER
                                                          PUMP
                                                                     DRY GAS METER
            ICE BATH
                          Figure 4-1.  Moisture-sampling train.
            LOCATION.

            TEST
                                                           COMMENTS
            DATE
            OPERATOR
            BAROMETRIC PRESSURE
CLOCK TIME





GAS VOLUME THROUGH
METER, (Vm),
ft3





ROTAMETER SETTING
ft3/min





METER TEMPERATURE,
•r





V)
90
m
O

i
                           Figure 4-2. Field moisture determination.
                                                      FEDERAL  REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23,  1971
                                                                                                                                      1x5
                                                                                                                                      *»
                                                                                                                                      oo
                                                                                                                                      23

-------
24888
                 RULES AND  REGULATIONS
4.2  Gas volume.
       1771   CR
        '•"in. HgV. Tm     equation 4-2
•where:
  Vine =Dry gas  volume through meter at
          standard conditions, cu. ft.
  Vm =Dry gas volume measured by meter,
          co. ft
  Fm = Barometric pressure at the dry gas
          meter, Inches Hg.
  Pit«;=Pressure at standard conditions, 29.93
          Inches Hg.
  T.t«=Absolute  temperature  at standard
          conditions, 530* R.
  Tm —Absolute temperature at meter ( *F+
          460), *R.
4.3   Moisture content.
              -+8.,,,=
+ (0.025)
                        V^+Vm.

                              equation 4-3
 where:
   Bwo=Proportion by volume of water vapor
           In the gas  stream, dlmenslonless.
,   Vw« = Volume  of  water vapor  collected
:           (standard conditions), cu. ft.
'•   Vm« =Dry  gas  volume through  meter
           (standard conditions), cu. ft.
',   BWM=Approximate  volumetric proportion
;           of water vapor  in the gas stream
;.:          leaving the impingers, 0.025.
   6. References.
   Air Pollution Engineering Manual, Daniel-
 eon. J. A. (ed.), UJS.  DHEW, PHS, National
 Center for Air Pollution Control, Cincinnati,
 Ohio, PHS Publication No. 999-AP-40, 1967.
   Devorkln,  Howard,  et  al..  Air  Pollution
 Source Testing Manual, Air Pollution Con-
 trol District, Los Angeles, Calif., November
 1963.
   Methods for Determination of Velocity,
 Volume,  Dust and Mist Content  of  Oases,
 Western Precipitation Division of Joy Manu-
 facturing Co., Los Angeles, Calif., Bulletin
 WP-60, 1068.

 METHOD  E—DETERMINATION OF FABTICTTLATE
    EMISSIONS FBOM STATIONAET SOURCES

   1. Principle and applicability.
   1.1   Principle. Partlculate matter Is with-
 drawn  Isoklnetioally from the source and Its
 •weight Is determined gravimetrically after re-
 moval  of uncomlblned water.
   12   Applicability. This method is applica-
 ble for the determination of partlculate emis-
 sions  from  stationary  sources  only when
 specified  by the test procedures for determin-
 ing compliance  with  New Source Perform-
 ance Standards.
   2. Apparatus.
   2.1   Sampling train. The design specifica-
 tions of the partlculate sampling train used
 by KPA (Figure 5-1) are described  in APTD-
 0581. Commercial models of this  train are
 available.
   2.1.1 Nozzle—Stainless steel  (316)  with
 sharp,  tapered leading edge.
   2.1.2  Probe—Pyrex1 glass with  a heating
 system capable of maintaining a  minimum
 gas temperature of 250° F. at the exit end
 during sampling  to  prevent condensation
 from  occurring.  When  length limitations
 (greater than about 8 ft.)  are encountered at
 temperatures less than 600° F., Incoloy 825 *,
 or equivalent, may be used. Probes for sam-
 pling  gas streams at  temperatures in excess
 of 600° F. must have been approved by the
 Administrator.
   2.1.3  Pltot tube—Type  &, or equivalent,
 attached  to probe  to monitor stack gas
 velocity.
  3.1.4  Filter  Holder— Pyrex »  glass  with
heating system capable of maintaining mini-
mum temperature of 225' F.
  2.1.6  Implngers / Condenser — Pour Impln-
gers connected In series with glass ball joint
fittings. The first, third, and fourth Impln-
gers are  of the Oreenburg-Smlth  design,
modified by replacing the tip with a %-lnch
ID  glass  tube extending to one-half Inch
from the bottom of the flask. The second 1m-
plnger la of  the Greenburg-Smlth design
with the standard Up. A condenser may be
used In place of the Implngers provided that
the moisture  content of the stack gas can
still be determined.
  2.1.6  Metering  system — Vacuum  gauge,
leak-free  pump,  thermometers  capable of
measuring temperature  to within  6* F., dry.
gas meter with 2%  accuracy, and  related
equipment,  or equivalent,  as required to
maintain an isoklnetic sampling rate and to
determine sample volume.
  2.1.7  Barometer — To measure atmospheric
pressure to ±0.1 Inches Hg.
  2.2   Sample recovery.
  2.2.1  Probe brush—At least  as long as
probe.
  2.2.2  Olass wash bottles—Two.
  2.2.3  Olass sample storage containers.
  2.2.4  Graduated cylinder—250 ml.
  2.3  Analysis.
  2.3.1  Olass weighing dishes.
  2.3.2  Desiccator.
  2.3.3  Analytical balance—To  measure to
±0.1 mg.
  2.3.4  Trip  balance—300  g. capacity, tx>
measure to ±0.05 g.
  3. Reagents.
  3.1  Sampling.
  3.1.1  Filters—Glass fiber, MSA 1106 BH*.
or equivalent,  numbered for Identification
and prewelghed.
  3.1.2  Silica  gel—Indicating  type,   6-16
mesh, dried at 175° C. (350* F.)  for 2 hours.
  3.1.3  Water.
  3.1.4  Crushed Ice.
  3.2  Sample recovery.
 "3.2.1  Acetone—Reagent grade.
  3.3  Analysis.
  3.3.1  Water.

     IMPINGER TRAIN OPTIONAL MAY BE REPLACED
           BY AN EQUIVALENT CONDENSER
                                                   PROBE
                                             REVERSE-TYPE
                                              PITOT TUBE
                                                                       HEATED AREA  FILTER HOLDER / THERMOMETER   CHECK
                                                                                                                 ..VALVE
                                                                                                                  ..VACUUM
                                                                                                                     LINE
                                                        PITOT MANOMETER

                                                                 ORIFICE
                                                        THERMOHETI
                                                IMPINGERS            ICE BATH
                                                       BY-PASS,VALVE
                                                                                                       VACUUM
                                                                                                        GAUGE
                                                                                                MAIN VALVE
                                                                   DRY TEST METER
                                                     AIR-TIGHT
                                                       PUMP
                                                                     Figure 5-1. partlculate-sampling train.
                                              3.3.2 Desiccant—Drlerlte,1 Indicating.
                                              4. Procedure.
                                              4.1  Sampling
                                              4.1.1 After selecting the sampling site and
                                            the minimum number of sampling .points,
                                            determine the, stack pressure, temperature,
                                            moisture, and range  of velocity head.
                                              4.1.2 Preparation   of   collection  train.
                                            Weigh to the nearest gram approximately 200
                                            g. of silica gel. Label  a filter o'f proper diam-
                                            eter, desiccate* for at least  24 hours  and
                                            weigh to the nearest 0.5 mg. In a room where
                                            the relative humidity is less than 50%. Place
                                            100 ml. of water In each of  the  first  two
                                            Implngers, leave the  third  implnger empty,
                                            and place approximately 200 g. of prewelghed
                                            silica  gel in the fourth Impinger. Set up the
                                            train  without the probe as In Figure  5-1.
                                            Leak check the sampling train at  the sam-
                                            pling  site by plugging up the inlet to the fil-
                                            ter holder and pulling a 15 in. Hg vacuum. A
                                            leakage rate not in excess of 0.02 c.f.m.  at a
                                            vacuum of 15 In.  Hg is  acceptable. Attach
                                            the probe and adjust the  heater to  provide a
                                            gas temperature of about 250° F. at the probe
                                            outlet. Turn on the  filter heating system.
                                            Place  crushed ice around  the impingers. Add
  1 Trade name.
              1 Trade name.
              •Dry using Drlerlte1 at 70° F.±10° F.
                                            more ice during the run to keep the temper-
                                            ature of the gases leaving the last Implnger
                                            as low as possible and preferably at 70° F.,
                                            or less. Temperatures above 70° F. may result
                                            In damage to the dry gas meter from either
                                            moisture condensation or excessive heat.
                                              4.1.3  Particulate train operation. For each
                                            run, record the data required on the example
                                            sheet shown in Figure 5—2. Take readings at
                                            each sampling point, at least every 5 minutes,
                                            and when significant  changes in stack con-
                                            ditions  necessitate additional  adjustments
                                            In flow rate. To begin sampling, position the
                                            nozzle at the first traverse point with the
                                            tip pointing directly into the  gas  stream.
                                            Immediately start the pump and adjust the
                                            flow to  isokinetlc  conditions. Sample for at
                                            least 5 minutes at each  traverse  point; sam-
                                            pling time must be the  same for each point.
                                            Maintain isoklnetic sampling throughout the
                                            sampling  period. Nomographs are available
                                            which aid in the rapid adjustment of the
                                            sampling  rate without  other computations.
                                            APTD-0576 details the  procedure  for  using
                                            these nomographs. Turn oft the pump at the
                                            conclusion of each run  and record the final
                                            readings. Remove the probe and nozzle from
                                            the stack and handle  In accordance with the
                                            sample recovery process described in section
                                            4.2.
                                FEDERAL REGISTER, VOL.  36, NO.  247—THURSDAY, DECEMBER 23,  1971

-------
                                                   RULES AND  REGULATIONS
                                                                                 24889
       RUN NO	

       SAMPLE KK Nq_

       METER'BOX K0._

       HETERtHj	

       CFACIOB	
                                                                AMBIENT TEUPERA7URE_
                                                                                               Tm= Average dry gas meter temperature,
                   ASSUMED MOI$TME.*_
                   HUTES BOX S£TTINO_
                   ffiOBE LENGTH.*
                   NOZZLE aAMETO, !«._
                   PROBE Hf ATER SETT1NG_
                                  SCHEMATIC OF STACK CROSS SECTION
TRAVERSE POINT
NUU8QI












TOTAL
SAMPLING
TIME
lel.ria.













AVERAGE
STATIC
PRESSURE
[Psl. ta. Mj.














STACK
TEUPEUTUC
(TS'-*f














vEiocm
HEAD
I»PS>.














PHESSUKE
DIFFERENTIAL
ACROSS
ORIFICE
METER '
I«HJ.
la-HjO














GAS SAMPLE
VOLUME
(Vml. It3














GAS SAMPLE TEMPERATURE
AT DOT GAS UETtR
INLET
IT" ».!•*'












Avg.
OUTLET
"" ««"••'












AX.
Avg.
SAMPLE KM
TEMPERATURE.
"F














TE»PER»niRE
OF GAS
LEAVING
CONDENSER OR
LAST WPfflGER.
•t














                                          Figure 5-2. Parlici
  4.2  Sample recovery. Exercise care in mov-
ing the collection train from the test site to
the  sample recovery area  to minimize  the
loss of  collected  sample  or  the  gain  of
extraneous  paniculate matter.  Set aside  a
portion of the  acetone  used In the sample
recovery as a blank for analysis. Measure the
volume of water from  the first three 1m-
pingers,  then discard. Place the samples in
containers as follows:
  Container  No. 1. Remove the filter from
Its holder, place in this container,  and seal.
  Container  No.  2. Place  loose participate
matter   and  acetone  washings  from  all
sample-exposed surfaces prior to  the filter
in this container and seal. Use a razor blade,
brush, or rubber policeman to lose adhering
particles.
  Container  No.  3. Transfer the  silica gel
from the fourth Impinger to the original con-
tainer and seal. Use  a rubber policeman as
an  aid  in  removing silica gel  from  the
Impinger.
  4.3  Analysis. Record the data required on
the  example  sheet shown In  Figure 5-3.
Handle each sample container as follows:
  Container  No. 1. Transfer the  filter and
any loose participate matter from the sample
container to  a tared glass  weighing dish,
desiccate, and dry to a constant weight. Re-
port results to the nearest  0.5 mg.
  Container   No.  2.  Transfer  the  acetone
washings to a tared beaker and evaporate to
dryness  at ambient temperature  and pres-
sure. Desiccate and dry to a constant weight.
Report results to the nearest 0.5 mg.
  Container No. 3. Weigh the spent silica gel
and report to the nearest gram.
  5. Calibration.
  Use methods  and equipment which have
been  approved  by  the  Administrator  to
calibrate the  orifice  meter,  pltot  tube, dry
gas meter,  and probe  heater.  Recalibrate
after each test series.
  6. Calculations.
  6.1  Average dry  gas meter temperature
and average orifice pressure  drop.  See data
sheet (Figure 6-2).
  6.2  Dry gas volume. Correct  the sample
volume measured by  the dry gas  meter  to
standard conditions (70° F., 29.92 Inches Hg)
by using Equation 5-1.
                   /
     -V  fT.tJ\(
   ""-M^WV
"+13.6 1
__	 I =
                              equation 5-1
where:
  Vm>td= Volume of gas sample through the
           dry gas  meter (standard  condi-
           tions), cu/ft.
    Vm = Volume of gas sample through the
           dry  gas  meter   (meter  condi-
           tions) , cu. ft.
   TlU = Absolute temperature at  standard
           conditions, 530° R.
                                                                                               AH
         Barometric pressure at the orifice
           meter. Inches Hg.
         Average pressure drop across  the
           orifice meter, Inches H=O.
    13.6= Specific gravity of mercury.
    P.,4= Absolute pressure at standard con-
           ditions, 29.92 Inches Hg.
  6.3  Volume of water vapor.
                                                                                                                     ).0474
                                                                                                                           cu. :
                              equation 5-2

where:
  Vvr.ld= Volume of  water vapor In the gas
           sample  (standard   conditions),
           cu. ft.
    Vi0 = Total volume of liquid collected in
           Implngers and silica gel (see Fig-
           ure 5-3), ml.
    pay) = Density of water, 1 g./mL
   Maao=Molecular weight of water, 18 lb./
           Ib.-mole.
      R=Ideal  gas constant,  21.83  Inches
           Hg—cu. ft./lb.-mole-°R.
    T,td=Absolute temperature  at standard
           conditions,  530° R.
    P. td=Absolute pressure at standard con-
           ditions, 29.92 inches  Hg.

  6.4  Moisture content.

            „         *w»td
                              equation 5—3

where:
  Bwo =Proportion by volume of water vapor in the £as
         stream, dtmensionlcss.
  ^•«id=Volume of water in the gas sample (standard
         conditions), cu. ft.
  VmBtd = Volume of gas sample through the dry gas mot cr
         (standard conditions) , cu. ft.
  6.5  Total partlculate  weight. Determine
the total participate catch from the sum of
the  weights  on  the  analysis  data  sheet
(Figure 5-3).
  6.6  Concentration.
  6.6.1  Concentration In gr./s.c.f .
        c'.=  0.0154
                                                                  -^ n
                                                                  ing./ \

                              equation 5-4
where:
    0",= Concentration of participate matter In stack
         gas. gr./s.o,f., dry basis.
   M0 = Total amount of paniculate matter collected,
         mg.
  Vm.i
-------
 24890
RULES AND  REGULATIONS
                              PLANT.

                              DATE_
                              RUN NO.
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICULATE COLLECTED.
mg
FINAL 'WEIGHT

x
TARE WEIGHT

:^^
WEIGHT GAIN




FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME.
ml




SILICA GEL
WEIGHT.
9



9»| ml
  CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
  INCREASE BY DENSITY OF WATER.  (1 g ml):
                                                      = VOLUME WATER, ml
                       Figure5-3.  Analytical data.

  6.6.2  Concentration In lb./cu. ft.
                  Ci = V453i600mg^==2205><10_6M!,

                            Vm«td                     *mstd
                                                                           equation 5-5
where:
     
-------
necessary only If a sample  traverse la re-
quired, or It stack gas velocity varies with
time.
  2.2  Sample recovery.
                      2.2.1  Glass wash bottles—Two.
                      2.2.2  Polyethylene  storage   bottles—To
                    store Implnger samples.
                      2.3  Analysis.
PROBE (END PACKED
WITH QUARTZ OR
PYREX WOOL]
  TVPESP1TOT
STACK WALL
           MIDGET BUBBLER MIDGET IMPINGERS
    GLASS WOOL
                                       SILICA GEL DRYING TUBE
                           TOEJWOHETER
                                                                       'UMP
                               DRY GAS METER   BOTAMETER
                             Figure 6-1.  SOj sampling train.
  2.3.1  Pipettes—Transfer type, 5 ml. and
10 ml. sizes  (0.1  ml. divisions) and  25 ml.
size  (0.2 ml. divisions).
  2.3.2  Volumetric flasks—50  ml., 100 ml.,
and  1,000ml.
  2.3.3  Burettes—5 ml. and 50 ml.
  2.3.4  Erlenmeyer flask—125 ml.
  3.  Reagents.
  3.1 Sampling.
  3.1.1  Water—Delonlzed, distilled.
  8.1.2  Isopropanol, 80%—Mix 80 ml. of Iso-
propanol with 20 ml. of distilled water.
  3.1.3  Hydrogen peroxide, 3%—dilute 100
ml. of 30% hydrogen peroxide to 1 liter with
distilled water. Prepare fresh daily.
  3.2 Sample recovery.
  3.2.1  Water—Deionized, distilled.
  3.2.2  Isopropanol, 80%.
  3.3 Analysis.
  3.3.1  Water—Deionized, distilled.
  3.3.2  Isopropanol.
  3.3.3  Thorin indicator—l-(o-arsonophen-
ylazo) -2-naphthol-3,6-disulfonlc  acid, dlso-
dium salt (or equivalent). Dissolve 0.20 g. in
100 ml.  distilled water.
  3.3.4  Barium perchlorate  (0.01 N)—Dis-
solve   1.95  g.  of   barium   perchlorate
[Ba(ClO4)a.3H3O] In 200  ml. distilled water

      No. 247—Pt. II	3
                    and dilute to 1 liter with isopropanol. Stand-
                    ardize with sulfurlc  acid. Barium  chloride
                    may be used.
                      3.3.5  Sulfurlc  acid standard  (0.01 N) —
                    Purchase  or  standardize  to  ±0.0002  N
                    against 0.01N NaOH which  has previously
                    been  standardized' against potassium  acid
                    phthalate (primary standard grade).
                      4. Procedure.
                      4.1   Sampling.
                      4.1.1  Preparation of collection train. Pour
                    15 ml. of 80% isopropanpl Into the midget
                    bubbler and 15 ml. of 3% hydrogen peroxide
                    into each of the first two midget Implngers.
                    Leave the final midget impinger dry. Assem-
                    ble the train  as shown in Figure 6-1. Leak
                    check the sampling  train at the sampling
                    site by plugging the probe Inlet and pulling
                    a 10 Inches Hg vacuum. A leakage rate not
                    In excess  of 1% of the sampling rate Is ac-
                    ceptable.  Carefully release the probe Inlet
                    plug and  turn off the pump. Place  crushed
                    ice around the implngers. Add more  Ice dur-
                    ing the run to keep the temperature of the
                    gases  leaving the last Implnger at 70° P. or
                    less.
                      4.1.2  Sample collection. Adjust the sam-
                    ple flow rate  proportional to the stack  gas
velocity.  Take  readings  at  least every  five
minutes  and  when significant changes in
stack conditions  necessitate additional  ad-
justments In flow rate. To  begin sampling,
position  the tip  of the probe  at  the first
sampling point and start the pump. Sam-
ple proportionally  throughout the run.  At
the conclusion of  each run, turn off  the
pump and record the final readings. Remove
the probe from the stack and disconnect it
from the train. Drain the ice bath and purge
the remaining  part of the train by drawing
clean ambient air through the system for 15
minutes.
  4.2  Sample  recovery. Disconnect the  1m-
pingers  after purging. Discard the contents
of the midget bubbler. Pour the contents of
the midget Impingers into a polyethylene
shipment bottle. Rinse the three midget  Im-
pingers  and the connecting tubes with  dis-
tilled water and  add these  washings to  the
same storage container.
  4.3  Sample analysis. Transfer the contents
of the storage container to a 50 ml. volu-
metric flask. Dilute to the mark  with  de-
ionized,  distilled  water.  Pipette  a  10  ml.
aliquot of this solution into a 125 ml. Erlen-
meyer flask. Add 40 ml. of  Isopropanol  and
two to four drops of thorln Indicator.  Titrate
to a  pink endpolnt using 0.01 N barium
perchlorate. Run a blank with each series
of samples.
  5.  Calibration.
  5.1 Use standard methods and equipment
                      which have been approved by the Adminis-
                      trator to calibrate the rotameter, pilot tube,
                      dry gas meter, and probe heater.
                        5.2  Standardize the  barium  perchlorate
                      against 25 ml. of standard sulfurie acid con-
                      taining 100 ml. of Isopropanol.
                        6. Calculations.
                        6.1  Dry  gas  volume. Correct  the sample
                      volume  measured by the dry gas meter to
                      standard conditions  (70° P. and  29.92 Inches
                      Hg) by using equation 6-1.

                           _   /T.td\ /Pb.,
                           -
                                                                                                                                         1
                                        vmp
                                in. Hg\   T
                                                                                                                                    ..\
                                                                                                                                      /
                                                                                                                                                                 equation 6-1
                                                                                                            where:
                                                                                                              Vmlltd= Volume of gas sample through the
                                                                                                                       dry gas meter (standard condi-
                                                                                                                       tions) , cu. ft.
                                                                                                              •  Vra= Volume of gas sample through the
                                                                                                                       dry  gas  meter  (meter  condi-
                                                                                                                       tions) , cu. ft.
                                                                                                               Tata = Absolute temperature at standard
                                                                                                                       conditions, 530' R.
                                                                                                                Tm= Average dry gas meter temperature,
                                                                                                                       °R.
                                                                                                               Pbmr= Barometric  pressure at the orifice
                                                                                                                       meter, Inches Hg.
                                                                                                               P,ta= Absolute pressure at standard con-
                                                                                                                       ditions, 29.92 Inches Hg.
                                                                                                              6.2   Sulfur dioxide concentration.
eoj
                           (7.05X10-'— \-
                           V          g.-ml.
where:
       Cso3= Concentration of sulfur dioxide
              at  standard conditions,  dry
              basis, Ib./cu. ft.
 7.05 x 10-"= Conversion factor, including the
              number of grams per gram
              equivalent of  sulfur  dioxide
              (32 g./g.-eq.), 453.6 g./lb., and
              1,000 ml./l., Ib.-l./g.-ml.
        V,= Volume  of  barium  perchlorate
              titrant used for the sample,
              ml.
       Vtb = Volume  of  barium  perchlorate
              titrant used for the blank, ml.
         W=Normality of barium perchlorate
              titrant, g.-eq./l. ,
      Vaoln = Total solution volume of sulfur
              dioxide, 50 ml.
        V, = Volume  of  sample  aliquot  ti-
              trated, ml,
     Vmltd= Volume  of gas sample  through
              the  dry gas  meter (standard
              conditions), cu. ft., see Equa-
              tion 6-1.
                                                                                                                                                                                 c.
                                                                                                                                                                                 m
                                                                                                                                                                                 to
                                                                                                                                                                                 O
                                             O

                                             I
                             equation- 6-2   ij

                                             Z
  7.  References.    ,                          *"
  Atmospheric Emissions from Sulfurlc Acid
Manufacturing Processes, U.S. DHEW,  PHS,
Division of Air Pollution, Public Health Serv-
ice Publication No. 999-AP-13,  Cincinnati:,
Ohio, 1965.
  Corbett,  P.  F., The Determination of SO2
and  SO, in Flue Gases, Journal of the Insti-
tute of Fuel, 24:237-243, 1961.
  Matty, R. E. and E.  K.  Dlehl, Measuring
Flue-Gas SO2  and SO3, Power 101:94-97, No-
vember, 1957.
  Patton,  W.  F.  and J. A. Brink, Jr., New
Equipment  and  Techniques for Sampling
Chemical Process Gases, J. Air Pollution Con-
trol Association, 13, 162  (1963).

METHOD 7—DETERMINATION OP NITROGEN  OXIDE
   EMISSIONS  FROM STATIONARY  SOURCES

  1.  Principle  and applicability.
  1.1 Principle.  A grab sample  la collected
In an evacuated  flask  containing a  dilute
sulfurlc acid-hydrogen  peroxide absorbing
solution, and  the nitrogen  oxides, except   10
                                                      FEDERAL REGISTER, VOL.  35,  HO. 257-  7i;:j5;OAY, DKEiV.DIil 23, 1971

-------
24892

nitrous oxide,  are  measure  colorlmetrtcally
using  the   phenoldlsulfonlc  acid   (PDS)
procedure.
  1.2   Applicability. This method IB applica-
ble for the  measurement of nitrogen oxides
from  stationary sources only when specified
by the test  procedures for determining com-.
pllance  with   New  Source  Performance
Standards.
  2. Apparatus.
  2.1   Sampling. See Figure 7-1.
  2.1.1  Probe—Pyrex1  glass,  heated, with
filter  to remove particulate matter. Heating
Is unnecessary  If the probe remains dry dur-
ing the purging period.
  2.1.2  Collection  flask—Two-liter,  Pyrex,1
round bottom with short neck and  24/40
standard  taper opening,  protected  against
Implosion or breakage.

  1 Trade name.
                       RULES  AND REGULATIONS

                   2.1.3  Flask valve—T-bore stopcock  con-
                 nected to a 24/40  standard taper joint.
                   2.1.4  Temperature gauge—Dial-type ther,
                 mometer, or equivalent,  capable  of measur-
                 ing 2° F. Intervals from 28" to 125° F.
                   2.1.5  Vacuum  line—Tubing   capable  of
                 withstanding a vacuum of 3 Inches Hg abso-
                 lute pressure, with "T" connection and T-bore
                 stopcock, or equivalent.
                   2.1.6  Pressure  gauge—TJ-tube manometer,
                 36  Inches,  with   0.1-lnch  divisions,  or
                 equivalent.
                   2.1.7  Pump—Capable  of producing a vac-
                 uum of 3 Inches Hg absolute pressure.
                   3.1.8  Squeeze bulb—Oneway.
                   2.2   Sample recovery.
                   2.2.1  Pipette or dropper.
                   2.2.2  Glass storage containers—Cushioned
                 for shipping.         «
                                                                      - SQUEEZE BULI
        PROBE
                                - FLASK VALVI
      FILTER


  GROUND-GLASS
      § NO. 12/5
   8-WAY STOPCOCKr
   T-BORE. I. PYREX.
  2-irmBORE, 8-mmOO
       FLASK
                              .FLASK SHIEltX. .\
          GROUND"
          STANDARD TAPER,
          3 SLEEVE NO. 24/40
GROUND-GLASS
SOCKET, S NO. K/6
PYREX
                                                                    0AM ENCASEMENT
                                                              •BOILING FLASK •
                                                              2- LITER. ROUND-BOTTOM. SHOOT MECX.
                                                              WITH { SLEEVE NO. 24/40
                          Figure 7-1. Sampling train, flask valve, and llask.
   2.2.3  Glass wash bottle.
   2.3  Analysis.
   2.3.1  Steam bath.
   2.3.2  Beakers  or casseroles—260 ml.,  one
 for each sample and standard (blank).
   2.8.3  Volumetric pipettes—1, 2, and 10 ml.
   2.3.4  Transfer pipette—10 ml. with 0.1 ml.
 divisions.
   2.3.5  Volumetric flask—100  ml.,  one for
-each sample, and 1,000 ml. for the standard
 (blank).
   2.3.6  Spectrophotometer—To measure ab-
 eorbance at 420 nm.
   2.3.7  Graduated cylinder—100  ml.  with
 1.0 ml. divisions.
   2.3.8  Analytical balance—To measure to
 0.1 mg.
   3. Seagents..
   3.1  Sampling.
   3.1.1  Absorbing solution—Add  2.8 ml. of
 concentrated H2SO4 to 1  liter of  distilled
 water. Mix well  and add 6  ml. of 3 percent
 hydrogen  peroxide. Prepare a fresh, solution
 weekly and do not expose to extreme heat or
 direct sunlight.
   3.2  Sample recovery.
   3.2.1  Sodium  hydroxide  (12V)—Dissolve
 40 g. NaOH in distilled water and dilute to 1
 liter.
   3.2.2  Red litmus paper.
                   3.2.3  Water—Delonlzed, distilled.
                   3.3  Analysis.
                   3.3.1  Fuming sulfuric acid—15 to 18% by
                 weight free sulfur trloxide.
                   3.3.2  Phenol—White solid reagent grade.
                   3.3.3  Sulfuric acid—Concentrated reagent
                 grade.
                   3.3.4  Standard solution—Dissolve 0.6495 g.
                 potassium nitrate (KNO8) in distilled water
                 and dilute to 1 liter. For the working stand-
                 ard  solution, dilute 10 ml. of the resulting
                 solution to 100 ml. with distilled water. One
                 ml.  of the  working' standard  solution  IB
                 equivalent to 25 /ig. nitrogen dioxide.
                   3.3.5  Water—Delonlzed, distilled.
                   3.3.6  Phenoldlsulfonlc  acid   solution—;
                 Dissolve 25 g. of pure white phenol In 150 ml.
                 concentrated sulfuric acid on a  steam bath.
                 Cool, add 75 ml. fuming sulfuric acid, and
                 heat at 100° C. for 2 hours. Store In a dark,
                 stoppered bottle.
                   4. Procedure.
                   4.1 Sampling.
                   4.1.1  Pipette 25 ml. of absorbing solution
                 into a  sample flask. Insert the flask valve
                 stopper Into the flask with the  valve In the
                 "purge"  position.  Assemble the  sampling
                 train as shown In  Figure 7-1 and place the
                 probe at  the sampling point. Turn the  flask
                 valve and the pump valve to their "evacuate"
positions. Evacuate the flask  to at least 3
Inches Hg absolute pressure. Turn the pump
valve to its "vent" position and turn off the
pump. Check the manometer for any fluctu-
ation In the mercury level. If there is a visi-
ble change over the  span  of one minute,
check for leaks. Record the Initial volume,
temperature, and  barometric pressure.  Turn
the flask valve to  Its  "purge" position, and
then  do  the  same with  the pump valve.
Purge the probe and the vacuum tube using
the squeeze bulb. If condensation occurs  In
.the probe and flask valve area, heat the probe
and purge until the condensation disappears.
Then turn the pump valve to Its "vent" posi-
tion.  Turn  the flask  valve  to Its "sample"
position and allow sample to enter the flask
for about 15 seconds. After collecting the
sample,  turn  the  flask valve to Its "purge"
position and  disconnect the flask from the
sampling  train.   Shake the  flask  for  5
minutes.
   4.2  Sample recovery.
   4.2.1   Let the flask  set for a minimum  of
16 hours and then shake the contents for 2
minutes. Connect the  flask to  a  mercury
filled  U-tube  manometer,  open the  valve
from the flask to the manometer, and record
the  nask  pressure and temperature  along
with the barometric pressure. Transfer the
flask contents to a container for shipment
or to a 250 ml. beaker for analysis. Rinse the
flask with  two portions of 4 distilled  water
 (approximately 10 ml.)  and add  rinse  water
to the sample. For a blank use 26 ml. of ab-
sorbing solution and the same volume of dis-
tilled water as used In rinsing the flask. Prior
to shipping or analysis, add sodium hydrox-
ide (IN) drop-wise into both the sample and
the  blank  until  alkaline  to  litmus  paper
 (about 25 to 35 drops In each).
   4.3  Analysis.
   4.3.1  If the sample has  been shipped  In
a container, transfer  the  contents to  a 250
ml. beaker using a small amount of distilled
water. Evaporate the solution to dryness on a
steam bath and then cool. Add 2 ml. phenol-
dlsulfonlc acid solution to the dried residue
and triturate thoroughly with  a glass rod.
Make sure the solution contacts all the resi-
due. Add 1 ml. distilled water and four drops
of concentrated sulfuric acid. Heat the solu-
tion on a steam bath  for 3 minutes with oc-
casional stirring.  Cool, add 20 ml. distilled
water, mix well by stirring,  and  add concen-
trated ammonium hydroxide drbpwlse with
constant stirring  until alkaline to litmus
paper.  Transfer  the solution to a  100  ml.
volumetric flask and wash the beaker three
times with 4 to  6 ml. portions  of distilled
water.  Dilute  to  the  mark and mix  thor-
oughly. If the sample contains solids, trans-
fer a portion of the solution to a clean, dry
centrifuge tube, and centrifuge, or filter a
portion of the solution. Measure the absorb-
ance of each sample at 420 nm. using the
blank solution as a zero.  Dilute the sample
and  the blank with  a suitable  amount of
 distilled water If absorbance falls outside the
range of calibration.
   5.  Calibration.
   5.1   Flask volume. Assemble the flask and
flask valve and fill with water to the stop-
 cock.  Measure the volume of water to ±10
ml.  Number and  record the volume on the
flask.
   6.2   Spectrophotometer. Add 0.0 to 16.0 ml.
 of standard solution to a series of beakers. To
 each beaker add 25 ml. of absorbing solution
 and  add sodium  hydroxide (IN)  dropwlse
 until alkaline to  litmus paper (about 25 to
 35 drops).  Follow the analysis procedure of
 section 4.3 to collect enough data to draw a
 calibration curve of concentration In pg. NOa
 per sample versus absorbance.
   6.  Calculations.
   6.1   Sample volume.
                                 FEDERAL  REGISTER, VOl. 36, NO.  247—THURSDAY, DECEMBER 23, 1971

-------
                                                  RULES  AND  REGULATIONS
                                                                                                                            24893
where:
   V,c=Sample  volume  at  standard condi-
          tions (dry basis), ml.
  Tala= Absolute temperature at  standard
          conditions, 530° R.
  P,tJ — Pressure  at  standard   conditions,
          29.92 Inches  Hg.
   Vf = Volume of flask and valve, ml.
   Va = Volume of absorbing solution, 25 ml.
                                                Pt—Final  absolute  pressure  of flask,
                                                      inches Hg.
                                                P, = Initial  absolute  pressure  of flask,
                                                      Inches Hg.
                                                T, = Final absolute temperature of (flask,
                                                      °R.
                                                T, = Initial absolute temperature of flask,
                                                      °R.
                                              6.2  Sample concentration. Read /ig.  NO2
                                            for each  sample from  the plot of ng.  NOa
                                            versus absorbance.
                    Ci
                  = I ^7—

                             1.6X10'^
                                     ml./
where:
    C = Concentration  of  NOX as NOa (dry
         basis), Ib./s.c.f.
   m=Masf of NO2 In gas sample, /ig.
  Vac = Sample volume at  standard condi-
         tions (dry basis), ml.
  7. References.
  Standard Methods  of Chemical Analysis.
6th ed. New York, D. Van Nostrand Co., Inc.,
1962, vol. 1, p. 329-330.
  Standard Method of Test  for Oxides of
Nitrogen In  Caseous Combustion Products
(Phenoldlsulfonlo Add Procedure), In: 1968
Book of ASTM Standards, Part 23, Philadel-
phia, Pa. 1968, ASTM Designation D-1608-60,
p. 725-729.
  Jacob, M. B., The Chemical Analysis of Air
Pollutants, New York, N.Y., Interscience Pub-
lishers, Inc., 1960, vol. 10, p. 351-356.

METHOD 8—DETERMINATION OF SULFTTRIC ACID
  MIST AND SULFTJB DIOXIDE  EMISSIONS FROM
  STATIONARY SOURCES

  1. Principle and applicability.
  1.1 Principle.  A gas sample  Is  extracted
from a sampling point In the stack and the
acid mist including sulfur  trloxide (s sepa-
rated from sulfur dioxide. Both fractions are
measured separately  by the  barlum-thorln
tltration method.
  1.2 Applicability. This method Is applica-
ble  to determination of sulfuric acid mist
(Including sulfur trloxide)  and sulfur diox-
ide  from stationary sources only when spe-
cified by the test procedures for determining
                                                                         equation 7-2

                                            compliance  with the New Source  Perform-
                                            ance Standards.
                                              2. Apparatus.
                                              2.1   Sampling. See Figure  8-1.  Many of
                                            the design  specifications of  this  sampling
                                            train are described in APTD-0581.
                                              2.1.1  Nozzle—Stainless steel   (316)  with
                                            sharp,  tapered leading edge.
                                              2.1.2  Probe—Pyrex1 glass  with a heating
                                            system to prevent visible condensation dur-
                                            ing sampling.
                                              2.1.3  Pltot tube—Type 8,  or equivalent,
                                            attached  to  probe  to  monitor stack gas
                                            velocity.
                                              2.1.4  Filter holder—Pyrex1 glass.
                                              2.1.5  Implngers—Four as shown  in Figure
                                            8-1. The first and third are of the Greenburg-
                                            Smith  design with standard tip. The second
                                            and fourth  are of the Greenburg-Smlth de-
                                            sign, modified by replacing the  standard tip
                                            with a %-inch ID glass tube extending to
                                            one-half Inch  from  the bottom of the im-
                                            pinger  flask.  Similar   collection   systems,
                                            which  have been approved by the  Adminis-
                                            trator, may be used.
                                              2.1.6  Metering  system—Vacuum  gauge,
                                            leak-free  pump, thermometers  capable of
                                            measuring temperature to within 5° F., dry
                                            gas meter with  2% accuracy,  and related
                                            equipment,  or  equivalent,  as  required to
                                            maintain an isoklnetic sampling  rate and
                                            to determine sample volume.
                                              2.1.7  Barometer—-To measure atmospheric
                                            pressure to ±0.1 Inch Hg.
                                              1 Trade name.
                       STACK
                                           FILTER HOLDER
                                                                       THERMOMETER

                                                                               CHECK
                                                                               VALVE
  REVERSE-TYPE
   PITOTTUBE
                                         ICE BATH      IMPINQERS
                                              BY-PASS VALVE
                                                                              VACUUM
                                                                               LINE
                                                                           VACUUM
                                                                             GAUGE
                                                            •AIR-TIGHT
                                                             PUMP
                       DRY TEST METER

                          Figure 8-1. Sulfuric acid mist sampling train.
  2.2  Sample recovery.
  2.2.1  Wash bottles—Two.
  2.2.2  Graduated cylinders—250 ml.,  500
ml.
  2.2.3  Glass sample storage containers.
  2.2.4  Graduated cylinder—260 ml.
  2.3  Analysis.
  2.3.1  Pipette—25 ml., 100ml.
  2.3.2  Burette—50ml.
  2.3.3  Erlenmeyer flask—260 ml.
  2.3.4  Graduated cylinder—100ml.
  2.3.5  Trip  balance—300 g.  capacity, to
measure to ±0.05 g.
 •2.3.6  Dropping bottle—to  add  Indicator
solution.
  3. Reagents.
  3.1  Sampling.
  3.1.1  Filters—Glass fiber,  MSA type 1108
BH, or equivalent, of a suitable size to fit
in the filter holder..
  3.1.2  Silica  gel—Indicating  type,  6-16
mesh, dried at 175° C. (350°  F.)  for 2 hours.
  3.1.3  Water—Delonized, distilled.
  3.1.4  Isopropanol,  80%—Mix  800  ml. of
Isopropanol with 200 ml.  of deionlzed,  dis-
tilled water.
  3.1.5  Hydrogen peroxide, 3%—Dilute 100
ml. of 30% hydrogen peroxide to 1 liter with
delonized, distilled water.
  3.1.6  Crushed ice.
  3.2  Sample recovery.
  3.2.1  .Water—Deionized, distilled.
  3.2.2  Isopropanol, 80%.
  3.3  Analysis.
  3.3.1  Water—Deionlzed, distilled.
  3.3.2  Isopropanol.
  3.3.3  Thorin indicator—l-(o-arsonophen-
ylazo)-2-naphthol-3, 6-disulfonlc  acid, di-
sodlum salt (or equivalent). Dissolve 0.20 g.
In 100 ml. distilled water.
  3.3.4  Barium  perchlorate  (0.01N)—Dis-
solve  1.95  g.  of  barium perchlorate [Ba
(CO,).,3 H,O] In 200 ml. distilled water and
dilute to 1 liter with Isopropanol. Standardize
with sulfuric acid.
  3.3.5  Sulfuric acid  standard  (0.01AT) —
Purchase or standardize to ± 0.0002 N against
0.01 N NaOH which  has previously  been
standardized against primary standard po-
tassium acid phthalate.
  4. Procedure.
  4.1  Sampling.
  4.1.1  After selecting the sampling site and
the  minimum number  of sampling points,
determine the stack pressure,  temperature,
moisture, and range of velocity head.
  4.1.2  Preparation  of   collection   train.
Place 100 ml. of 80% Isopropanol In the first
implnger, 100 ml. of 3% hydrogen peroxide in
both the second and third impingers, and
about 200 g. of silica gel  In the fourth 1m-
plnger.  Retain a portion of the  reagents for
use  as  blank solutions. Assemble  the  train
without the probe as shown in Figure 8—1
with the  filter between the first and second
Implngers. Leak check  the sampling  train
at the sampling site by plugging the  Inlet to
the  first Impinger and  pulling a 15-inch Hg
vacuum. A leakage rate not in excess of 0.02
c.f.m. at  a vacuum  of 15 Inches Hg is ac-
ceptable.  Attach the probe and  turn on the
probe  heating system.  Adjust  the probe
heater  setting during  sampling to  prevent
any visible condensation. Place crushed Ice
around the Implngers.  Add more Ice during
the run to keep the temperature of the gases
leaving the last Implnger at 70° F.  or less.
  4.1.3  Train  operation.  For  each run, re-
cord the data required  on the example sheet
shown  In Figure 8-2. Take readings  at  each
sampling point at least every 5 minutes and
when significant changes In stack conditions
necessitate  additional  adjustments  In  flow
rate. To begin sampling,  position the nozzle
at the first traverse point with the tip point-
ing  directly  Into the gas stream. Start the
.pump and immediately adjust  the  flow to
isoklnetic conditions.  Maintain  Isoklnetic
sampling throughout the sampling period.
Nomographs are available which aid in the
                                 FEDERAL REGISTER, VOL.  36, NO. 247—THURSDAY, DECEMBER 23, 1971

-------
                                     E-l




SRL 1281  35  0472
                                 APPENDIX E




                            LABORATORY REPORT
     SCOTT RESEARCH LABORATORIES, INC

-------
                                   E-2





SRL 1281 35 0472
                            LABORATORY REPORT




E.I  ON-SITE HANDLING AND TRANSFER, PARTICULATE




          After the completion of a test run, the probe and nozzle were




disconnected from the impinger train and all open ends sealed immediately




to avoid contamination.  At the laboratory facility, the nozzle was




disconnected from the probe and very carefully washed with acetone, using




a fine bristled brush.  All acetone washings were collected in a clean




glass jar, the jar itself being placed on a large piece of clean aluminum




foil.  The probe was then washed using a long handled brush rotated




through it under a continuous stream of acetone.  The brush was also




carefully cleaned, and all washings collected in the glass jar.  The




probe was finally checked visually for any residue.




          The impinger train was initially wiped clean on the outside




and all glassware connectors, including the filter, removed carefully




and all exposed surfaces wiped clean.  All the connectors were placed




on a piece of aluminum foil ready for washing.  The first three impingers




were then analyzed for water collection by transferring the water through




the outlet port into a graduated cylinder and noting the volume.  The




impingers were not dismantled and all transfers and washings were




performed through the inlet and outlet ports.  All of the glassware in




the back half of the filter, up to the fourth impinger was then carefully




washed with distilled water and the washings collected.  This was




followed by an acetone wash which was again collected in a separate jar.
     SCOTT RESEARCH LABORATORIES, INC

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                                   E-3





SRL 1281 35 0472






          Acetone washings from the glassware in the front half of the




filter were collected in the same jar as the probe and nozzle wash.




The filter was carefully removed from the holder and placed in a




plastic dish which was then sealed with tape.  Silica gel in the fourth




impinger was weighed in a previously tared glass jar using a triple-




beam balance.




          All acetone jars had aluminum lined lid , or aluminum foil




was used before screwing on the lids.  The following designations were




used for labeling the containers:




          Container #1:  Filter




          Container #2:  Acetone wash front half from filter




          Container #3:  Water wash back half from filter




          Container #4:  Silica gel




          Container #5:  Acetone wash back half from filter






E.2  LABORATORY HANDLING AND ANALYSIS, PARTICULATE




     E.2.1   Filter Transfer



          Clean plastic dishes were desiccated for 24 hours, labeled




and tared on an electronic balance.  The filter containers were unsealed




and desiccated for 24 hours before carefully transferring the filters




to the tared dishes using a fine pair of tweezers.  Care was taken to




place a piece of aluminum foil under the transfer operation.  A




"staticmaster" brush was used to brush any fine particles adhering to




the container or foil.  All transfers were performed near the balance




and the weight reported to the nearest 0.1 mg.  The plastic dishes were




then sealed  for shipment.
     SCOTT RESEARCH LABORATORIES, INC

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                                   E-4




SRL 1281 35 0472






     E.2.2  Acetone Washes




          The 250 ml. beakers to be used for the acetone wash transfers




were leached for 24 hours in 50% nitric acid, washed thoroughly and oven




dried overnight.  These were then desiccated for 24 hours and tared.




Once tared, the beakers were sealed with "parafilm" and handled with




tongs or "Kimwipes".




          The jars containing the acetone washes were left loosely




covered in a hood until the acetone was evaporated.  Once the acetone




was evaporated, the glass jar was rinsed with acetone, using a rubber




policeman, and the washings collected in the tared beaker.




          After the acetone had evaporated, the beakers were desiccated




for 24 hours and weighed to a constant weight.  Where water was present




in the acetone wash, it was evaporated in an oven at 90 C after the




acetone had all evaporated.




     E.2.3  Water Washes




          The level of water in the collection bottles was marked for




later volume measurement.  Each water wash was then transferred into




a 2000 ml. separatory funnel and extracted three times with 25 ml.




portions of chloroform.  Often where a large volume of water was collected




(above 500 ml.), a fourth extraction was used.  The chloroform extracts




were collected directly in a tared beaker prepared in the same manner




as described in the previous section.




          Extraction with three 50 ml. portions of ether followed,




collecting the water portion in the original jars.  The ether extracts




were combined with the chloroform extracts.  These were then washed
     SCOTT RESEARCH LABORATORIES, INC

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                                                   E-5




                SRL 1281 35 0472






                with distilled water in the separatory funnel and returned to the




                tared beaker for evaporation in the hood.  The residues were desiccated




                and weighed.




                          The water portion was transferred to tared beakers, oven  dried




                at 90 C, desiccated, and weighed.  All beakers were "parafilm" sealed for




                shipment.  Particle size analysis was not performed per instruction




                from the Project Officer.  A summary of weight measurements is shown




                in Table E-l.
                     SCOTT RESEARCH LABORATORIES. INC
1

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                                                   TABLE  E-l  -  SUMMARY  OF  WEIGHT  MEASUREMENTS
30
n
po
20
n

t-
oo
O
ao

I
so
H
O
                                                   Run 1
                                    Final
            Tare    Gross  Blank   Net
            (g)      (mg)   (mg)    (nig)
         Container #1
         (Filter)

         Container #2
         (Acetone wash front half)

         Container "3a
         (Organic excract)

         Container #3b
         (Water after extraction)

         Container US
         (Acetone wash back half)
  8.1710     8.0790    92.0    -     92.0


 88.0860    87.9135   172.5    3.0    169.5


 99.5340    99.5290     5.0    0.0     5.0


100.5075   100.4465    61.0    0.0    61.0


 94.5905    94.5805    10.0    0.5     9.5
                                  Probe, cyclone, filter, mg.       261.5

                                                   Total, mg.       337.0
                                                                                          Run  2
 Final    Tare    Gross  Blank   Net
  (g)      (g)    (mg)    (mg)    (mg)
                                                                            8.2030    8.1015   101.5
                                                                        101.5
93.8415  93.7345  107.0   2.0   105.0


99.5090  99.5000    9.0   0.0     9.0


99.4915  99.4375   54.0   0.0    54.0


98.3490  98.3370   12.0   1.0    11.0


Probe, cyclone, filter, mg.      206.5

                 Total, mg.      280.5
                                                                                                                                  Run 3
                                                                                                                  Final      Tare    Gross  Blank   Net
                                                                                                                   (g)       (g)     (gm)   (mg)   (mg)
                                                                                                                                                          00
                                         8.2085    8.1145   94.0
                                                                                                                                                    94'°
 91.8990   91.7500  149.0   1.0   148.0


 96.5790   96.5710    8.0   0.0  -   8.0


 97.9745   97.9240   50.5   0.0    50.5


101.6575  101.6430   14.5   1.0    13.5


Probe, cyclone, filter, mg.       242.0

                 Total, mg.       314.0
                                                                      Run 4
                                                        Final     Tare    Gross  Blank   Net
                                                         (g)        (g)    (mg)   (mg)   (mg)
                            Container  //I
                            (Filter)
                     7.7760   7.7120    64.0
              64.0
                            Container  #2               96.0070  95.8995   107.5   2.0   105.5
                            (Acetone wash  front half)
                            Container  #3a
                            (Organic Extract)

                            Container  #3b
                            (Water  after extraction)

                            Container  //5
                            (Acetone wash back half)
                    97.3620  97.3530     9.0   0.0     9.0


                    98.1750  98.1425    32.5   0.0    32.5


                    95.5405  95.5300    10.5   1.0     9.5


                    Probe, cyclone, filter,  mg. .     169.5

                                     Total,  mg.      220.5
                                                                                                               Run 5
                                                             Final    Tare     Gross   Blank   Net
                                                              (g)       (g)      (mg)    (mg)    (mg)
                                                             7.7905   7.7125     78.0
                                                      78.0
                   93.4980  93.4020    96.0    1.0    95.0


                   99.3770  99.3690     8.0    0.0      8.0


                   98.5585  98.5280    30.5    0.0    30.5


                   98.5695  98.5550    14.5    1.0    13.5


                   Probe, cyclone, filter, mg.       173.0

                                    Total, mg.       225.0

-------
                                   E-7





SRL 1281 35 0472






E.3  NO  ANALYSIS
       x


          Immediately after each NO  flask sample was taken, the flask
                                   X


containing the absorbing solution and the gas sample was shaken for



five minutes.  The flask was then allowed to sit until the following



morning when it was shaken again for two minutes.  Following this final



shake, the flask pressure was measured with a mercury manometer.  Each



flask was then carefully wiped off and the stopcocks removed.  The



absorbing solutions were then transferred to glass shipping bottles



with two 10 ml. washes of distilled water.  Just prior to shipping,



the samples were neutralized with 1.0 N sodium hydroxide (approximately



40 drops).  At this time solution blanks were made for each set of samples.



The blanks contained 25 ml. of NO  absorbing solution and 20 ml. of
                                 X


distilled water and were neutralized with 1.0 N. sodium hydroxide.  At



the end of the test period all samples were transported to the laboratory



for analysis.



          All NO  samples were analyzed by the Phenoldisulfonic acid
                X


procedure.  Prior to analysis, a calibration curve was established for



a suitable range of NO  concentrations.  From a standard potassium nitrate
                      X


solution with an equivalent concentration of 25 pg N0« per ml. four



aliquots of 4, 8, 12 and 16 ml. were added to respective 250 ml. beakers.



Twenty-five ml. of NO  absorbing solution was added to each of these
                     X


beakers and the analysis procedure described below was followed.  These



solutions were read against a blank containing no standard solution and



a calibration curve of % absorbance versus ug N0« was plotted.
     SCOTT RESEARCH LABORATORIES. INC

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                                   E-8




SRL 1281 35 0472






          Upon arrival at the laboratory, each sample was transferred




to a 250 ml. beaker and evaporated to dryness on a steam bath.  After




cooling, 2 ml. of phenoldisulfonic acid was added and each sample was




triturated thoroughly with a glass stirring rod.  One ml. of distilled




water and four drops of concentrated sulfuric acid were added and the




samples were returned to the steam bath for three minutes.  The samples




were then cooled and 20 ml. of distilled water was added.  Concentrated




ammonium hydroxide was then added dropwise until each sample was alkaline




to litmus paper.  The samples were transferred to 100 ml. volumetric




flasks with distilled water and portions of each solution were read at



420 my on a Bausch and Lomb Spectronic 20 Colorimeter.  The solution




blanks run with each set of samples were used for a colorimeter zero




reference.  The absorbances read for each sample were then converted




to yg N09 via the previously established calibration curve.  NO  con-
        Z.                                                      X.


centrations were calculated as ppm N0_ following the procedure described




in Appendix B.  The laboratory data recorded for each analysis is included



as Table E-2.






E.4  ORSAT ANALYSIS



          A total of five integrated bag samples were analyzed by Orsat




during the three day test period.  Each five liter Tedlar sample bag




was equipped with a Teflon sample tube fitted with an airtight syringe




cap.  Prior to sampling, each bag was flushed with pure, dry nitrogen



and sealed with the syringe cap.
     SCOTT RESEARCH LABORATORIES, INC

-------
                                   E-9
SRL 1281 35 0472
                      TABLE E-2 - NO  ANALYSIS DATA
Run
No.

 1
 Date
3/20/72
           3/22/72
           3/22/72
           3/23/72
           3/23/72
Sample
Number

  1
  2
  3

  1
  2
  3

  1
  2
  3

  1
  2
  3

  1
  2
  3
Absorbance
 @ 420 my

  0.160
  0.227
  0.205

  0.242
  0.240
                               0.170
                               0.208
                               0.050

                               0.256
                               0.037
                               0.230

                               0.93
                               0.260
                               0.199
     NOX
Concentration
      N02)

    119.7
    169.8
    153.3

    181.0
    179.5
                                                    (lost)
                      127.1
                      155.6
                      37.4

                      191.5
                      27.7
                      172.0

                      69.6
                      194.4
                      148.8
     SCOTT RESEARCH LABORATORIES, INC

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                                  E-10





SRL 1281 35 0472







          At the end of each sampling day the sample bags were returned




to the field laboratory where they were analyzed for CO, CCL and 0?




by Orsat.




          Each bag was connected to the Orsat analyzer by carefully




removing the syringe cap and inserting the Teflon tube securely into




the Orsat sample tube.  The Orsat analyzer was then purged by squeezing




the Tedlar bag and forcing the sample through the Orsat bypass.  Successive




100 ml. samples were drawn into the Orsat sample burette and then passed




through each of the three absorbing solutions (potassium hydroxide - CO-,




alkaline pyrogallate - 0~, and acid cuprous chloride - CO).  Repetitive




passes were made through each absorbing solution until good duplication




of results occurred.  At least three 100 ml. samples were analyzed from




each Tedlar sample bag.  The data recorded for each Orsat analysis is




included in Table E-3.






E.5  TOTAL HYDROCARBON ANALYSIS




          Immediately following each Orsat analysis the remainder of the




sample contained in each Tedlar bag was analyzed for hydrocarbons via




a Beckman Model 108-A Total Hydrocarbon Analyzer.  This instrument




utilized a flame ionization detector and the following operating




conditions were maintained during each analysis:




                    Sample Backpressure:      2.50 psi




                    Fuel Pressure:           23.0  psi




                    Oxidant Pressure:        11.0  psi




                    Range:                  100    X
     SCOTT RESEARCH LABORATORIES. INC

-------
                                    E-ll
SRL 1281  35  0472
                      TABLE  E-3 - ORSAT ANALYSIS  DATA
Run Sample
No. Date Number Component
1 3/20/72 1 C02

°2

CO

2 C02

°2

CO

3 C02

°2

CO

2 3/22/72 1 C02

°2

CO

2 C0_

°2

CO

3 C0_

°2

CO

Analysis
Number
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
Bunette Volume (ml)
Initial
100.0

99.8

81.6

1100.0

99.8

81.7

100.0

99.8

81.6

100.0

99.7

80.1

100.0

99.8

80.1

100.0

99.7

80.1

Final
99.8
99.8
81.6
81.6
81.6
81.6
99.8
99.8
81.7
81.7
81.7
81.7
99.8
99.8
81.6
81.6
81.6
81.6
99.7
99.7
80.1
80.1
80.1
80.1
99.8
99.8
80.1
80.1
80.1
80.1
99.7
99.7
80.1
80.1
80.1
80.1
Difference
0.2
0.2
18.2
18.2
0.0
0.0
0.2
0.2
18.1
18.1
0.0
0.0
0.2
0.2
18.2
18.2
0.0
0.0
0.3
0.3
19.6
19.6
0.0
0.0
0.2
0.2
19.7
19.7
0.0
0.0
0.3
0.3
19.6
19.6
0.0
0.0
     SCOTT RESEARCH LABORATORIES, INC

-------
                                  E-12
SRL 1281 35 0472
                     TABLE  E-3  -  ORSAT ANALYSIS DATA

                                (continued)
Run
No.
Date
Sample
Number
 3   7/22/72    1
 4   7/23/72    1
Component
   co2

   °2
   CO
   co2

   °2
   CO
   co2

   °2
   CO

   co2

   °2
   CO
   co2

   °2
   CO
   co2

   °2
   CO
Analysis
Numb er
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
Bunette Volume (ml)
Initial
100.0

99.8

80.4

100.0

99.8

80.4

100.0

99.7

80.3

100.0

99.7

79.9

100.0

99.6

79.9

100.0

99.7

99.9

Final
99.8
99.8
80.4
80.4
80.4
80.4
99.8
99.8
80.4
80.4
80.4
80.4
99.7
99.7
80.3
80.3
80.3
80.3
99.7
99.7
79.9
79.9
79.9
79.9
99.6
99.6
79.9
79.9
79.9
79.9
99.7
99.7
79.9
79.9
79.9
79.9
Difference
0.2
0.2
19.4
19.4
0.4
0.0
0.2
0.2
19.4
19.4
0.0
0.0
0.3
0.3
19.5
19.5
0.0
0.0
0.3
0.3
19.8
19.8
0.0
0.0
0.4
0.4
19.7
19.7
0.0
0.0
0.3
0.3
19.8
19.8
0.0
0.0
    SCOTT RESEARCH LABORATORIES. INC

-------
                                    E-13
SRL 1281 35 0472
                      TABLE E-3 - ORSAT ANALYSIS DATA
                                 (continued)
Run Sample Analysis Analysis
No. Date Number Component Number
5 3/23/72 1 C02
°2
CO

2 C0_

°2
CO

3 CO
.
°2
CO

1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
Bunette Volume (ml)
Initial
100.0
99.6
79.8

100.0

99.6
79.8

100.0

99.5
79.7

Final
99.6
99.6
79.8
79.8
79.8
79.8
99.6
99.6
79.8
79.8
79.8
79.8
99.5
99.5
79.7
79.7
79.7
79.7
Difference
0.4
0.4
19.8
19.8
0.0
0.0
0.4
0.4
19.8
19.8
0.0
0.0
0.5
0.5
19.8
19 . 8
0.0
0.0
     SCOTT RESEARCH LABORATORIES, INC

-------
                                  E-14




SRL 1281 35 0472





The Scott compressed gases used during each analysis were:



               Fuel:  40% hydrogen in nitrogen



               Oxidant:  Blended Air



               Zero:  Hydrocarbon Free Air (<0.1 ppm-C)



               Span:  99.9 ppm propane (±2.0% analysis) in nitrogen



          Just prior to introducing each sample into the analyzer,



the instrument was zeroed and spanned on range 100.  The Tedlar sample



bag was then connected to the analyzer via a Teflon tube and the sample



was drawn into the analyzer until a stable reading was recorded on the



meter.  The bag was then disconnected and resealed with the syringe cap.



The instrument zero and span points were rechecked to insure that the



calibration had not changed during the analysis.  The complete analytical



procedure was then repeated until good duplication of results were obtained.



All meter readings recorded for each sample are included as Table E-4.



          The meter readings were then converted to parts per million



carbon by the following formula:




                                99.9 ppm-C3HR     3 ppm-C
          ppm-C = meter units x -r^— .	~  — x 	rr, „
          vv                    100 units-Span   ppm-C-Hg




The final data with example calculations are included in Appendix B of



this report.
     SCOTT RESEARCH LABORATORIES, INC

-------
                                   E-15
SRL 1281 35 0472
                   TABLE  E-4 - TOTAL HYDROCARBON DATA
Run
No.
 Date

3/20/72


3/22/72


3/22/72


3/23/72


3/23/72
Sample
 No.

  1
  2

  1
  2

  1
  2

  1
  2

  1
  2
Range
                                          100
                                          100

                                          100
                                          100

                                          100
                                          100

                                          100
                                          100

                                          100
                                          100
                                               Meter Units
Sample

 69.5
 69.5

 35.0
 33.0

 16.0
 16.0

 10.5
 10.5

  5.0
  7.0
Span
                            100.0
                            100.0

                            100.0
                            100.0

                            100.0
                            100.0

                            100.0
                            100.0

                            100.0
                            100.0
     SCOTT RESEARCH LABORATORIES, INC

-------
                                      F-l




SRL 1281  35 0472
                                 APPENDIX F




                                  TEST LOG
     SCOTT RESEARCH LABORATORIES. INC

-------
                                    F-2





SRL 1281 35 0472





                                TEST LOG



          On Monday, March 20, 1972, the Scott test team arrived at



the Wentz Plant of Westmoreland Coal Company in Stonega, Virginia,



and began to set up the test equipment.   Upon arrival at the site it



was learned that a wildcat strike had just started, but that there



was enough Osaka coal to continue processing for 8 or 9 hours.  The



process was switched to Osaka coal around noon by which time Scott was



set up and prepared to start testing.  Preliminary  velocity and



temperature traverses were performed and a nozzle size selected.



The first run was started at 1523.  Twenty-four points were traversed



in each port for a period of 2% minutes each.  The pitot line became



clogged with water at one point and had to be blown out.  The first run



was completed at 1825.  An Orsat and total hydrocarbon sample was



collected from 1512 to 1607.  NO  samples were collected at 1540, 1628,
                                X


and 1807.  During the test a brownish plume was observed trailing off



from the stack.



          The sample train was dismantled and the spare system was



assembled for the second run.  A leak test was performed and found to be



satisfactory.  When the pump was turned on to start the test, all of the



power went off.  Apparently the plant had turned on night lights between



the tests and the circuit was not large enough to carry everything.



Several attempts were made to supply alternate power but with no success.



Thus, it was decided to be ready for a test early the next morning.  The



samples were returned to the motel where all sample transfers were



performed and a new system, as well as a backup unit were prepared.  The



Orsat and hydrocarbon samples were analyzed and the NO  samples trans-
                                                      X


ferred to sample bottles.



     SCOTT RESEARCH LABORATORIES, INC.

-------
                                    F-3




SRL 1281 35 0472




          It was believed that there would be enough coal to perform a



run first thing Tuesday morning even if the strike continued.  Thus,



the Scott team arrived at the plant early and began setting up for a



test run.  It was soon learned that the entire plant was now striking



and that no testing could be performed.  The strike was settled late



in the afternoon and preparations were made to test on Wednesday.



          Wednesday the Scott team arrived at the plant and prepared



to run a test while the plant was processing Osaka coal.  A leak test



was performed and the filter holder was found to leak slightly, but it



was acceptable.  The run was started at 940 and continued to 1142.



The Orsat and hydrocarbon sample was collected from 935 to 1030.  NO



samples were collected at 950, 1025, and 1115.  The sample train was



disassembled and the second system was set up and leak tested.



          The third run was then started at 1305 and ran until 1515.



The Orsat and hydrocarbon sample was collected from 1304 to 1404.



The first sample for NO  was collected at 1325.  Other NO  samples
                       X                                 X


were taken at 1430 and 1520.  During both tests a slight brownish



plume was observed trailing off from the stack.



          The sample train was dismantled and taken back to the motel



where both sample trains were cleaned and the samples transferred to



sample bottles.  During the cleanup and transfer, it was noted that the



filters were being torn by the gasket in the filter holder.  This did



not affect the test, but made the cleanup procedure difficult.   The



Orsat and hydrocarbon samples were analyzed while the NO  samples were
                                                        X


transferred.  The sample trains were then prepared for more tests.
     SCOTT RESEARCH LABORATORIES, INC.

-------
                                   F-4
SRL 1281 35 0472

          On Thursday the Scott team arrived at the plant and set up to
perform tests while the plant was processing Wentz coal.  The sample
train was put in place and a leak test performed.  It was found to be
satisfactory and the test was started at 925 and ran until 1130.  It
was snowing and very windy during the test.  At 1045 the wind blew over
the manometer being used to measure the draft.  Thus, no readings were
taken after 1045.  The Orsat and hydrocarbon sample was collected from
925 to 1025.  The NO  samples were collected at 950, 1020, and 1115.
                    X
The sample train was disassembled and the second unit prepared to start
testing.
          A leak test was performed and found to be satisfactory.  The
test was started at 1144.  It had to be stopped at 1254 because of a
coal blockage in the plant operation.  The test was restarted at 1336
and continued until 1430.  The Orsat and hydrocarbon sample, was collected
from 1138 to 1238.  The NO  samples were taken at 1205, 1340, and 1415.
                          X.
Because of the weather conditions it was difficult to obtain a good
visible description of the stack plume.
          The sampling train was disassembled and all of the test
equipment was removed from the test site.  Back at the motel the sample
transfer and analyses were performed.  The Scott team traveled home on
Friday.
         Figure F-l illustrates the test program schedule.
     SCOTT RESEARCH LABORATORIES, INC.

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FIGURE F-l  SUMMARY OF TEST PROGRAM
®
M 1500
S
H
90
n
en
tn
ft
SB
» 0925
o
90
O
90


M
ft
1300






0900





1125





15*12 1607 °rSat & HC Sample
Change
1523 1620 X*~\ Ports 1725
1701 1704

1540 1628

933 1025
Change
940 • 104o'"1fortS 1042 1142


• • *
950 1025 1115

1304 1404
Change

1305 1405 °rtS 1415 1515
» • «
1325 1430 1520

925 1025
Change
09*^ -"'""i* O T t S^
J^ 1025 1030 1130
• • •
950 1020 1115

1138 1238
Change
1144 /forfcs "\ ' .
1244 1246 1254 1336
• • • •
1205 1340
RUN 1 - 3/20/72

1825


• NO
1807 x
RUN 2 - 3/22/72
1220



NO
X
RUN 3 - 3/22/72
1555


NO
*
RUN 4 - 3/23/72

1155


NO
X
RUN 5 - 3/23/72
1445

1430
• NO-
1415 X
UJ
P
1845 g
	 'Particulate i—
w
Ui
o
Ni
Particulate






Particulate





Particulate





Particulate





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                                     G-l
SRL 1281 35  0472
                                APPENDIX G




                      PROJECT PARTICIPANTS AND TITLES
     SCOTT RESEARCH LABORATORIES, INC

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                                    G-2
SRL 1281 35 0472
                     PROJECT PARTICIPANTS AND TITLES
          The personnel taking part in the project include:
Thomas Ward

Charles Sedman

Larry Jones

Norman Troxel

Joseph Wilson

Jyotin Sachdev

William Scott

Zenophon Tomaras

Margaret Husic

Louis Reckner
Project Officer - EPA

Project Engineer - EPA

Project Engineer - EPA

Senior Engineer - SRL

Field Team Leader - SRL

Engineer - SRL

Technician - SRL

Chemist - SRL

Technician - SRL

Manager, Atmospheric Chemistry &
Industrial Emissions Dept.
     SCOTT RESEARCH LABORATORIES. INC

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