TEST NUMBER 72-CI-16
INTERNATIONAL MINERALS AND CHEMICALS
       SUPER PHOSPHORIC ACID
          BARTOW, FLORIDA
      February 28-March 1, 1972

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                   PEDCo-EN VIRON MENTAL
                        SUITE 8  •  ATKINSON SQUARE
                             CINCINNATI. OHIO 45246
                                        513 /77 1-4330
        TEST NUMBER 72-CI-16

 INTERNATIONAL MINERALS AND CHEMICALS
        SUPER PHOSPHORIC ACID
           BARTOW, FLORIDA
       February 28-March 1, 1972
             Prepared by
     .Richard W. Gerstle, P.E.
                 By
PEDCo-Environmental Specialists, Inc,
          Cincinnati, Ohio

   Contract No. 68-02-0237, Task 2

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                     TABLE OF CONTENTS

                                              Page Number

  I.   INTRODUCTION	 .      1

 II.   SUMMARY OF RESULTS 	      4

III.   SAMPLING PROCEDURES 	      8

 IV.   ANALYTICAL PROCEDURES 	     13

  V.   APPENDIX 	     14

      Part A - Emission Calculations and
               Results

      Part B - Field Data

      Part C - Standard Analytical Procedures

      Part D - Test Log

      Part E - Project Participants

      Part F - Recommendations

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I.   INTRODUCTION




     Stack emission tests were conducted, and related process



samples were taken during the period February 28 to March 1,




1972, at the international Mineral and Chemical Company's




superphosphoric acid plant in Bartow, Florida.






     According to the terms of PEDCo's contract with EPA,




only stack gas measurements, selected feed and product




samples, and scrubber water samples were to be taken by PEDCo,




Stack gas samples were taken at points designated by EPA.




All process data and operating procedures were obtained by




EPA personnel.  Sample analyses and emission calculations




were also to be performed by EPA staff.






     Three tests were made to determine total fluoride




emissions before and after the scrubber serving the super-




phosphoric acid plant.  In this process, fumes from the



plant's acid recycle tank, and the vent serving the product




storage tank and barometric seal tank are directed into a




combination venturi scrubber and packed bed scrubber in




series before entering the atmosphere.  Samples were taken




simultaneously in the two lines entering the scrubber system,




and in the single duct leaving the scrubber.  Figure 1 shows




the equipment layout and the locations of the sampling sites.

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Detail of Outlet
 Sampling Site
    Point E
                              o
                              C7	
                        Detail of Inlet
                       Sampling Site from
                       Recycle Acid  Tank
                            Point C.,
                                                      Detail of Inlet
                                                     Sampling Site from
                                                    Barometric Seal Tank
                                                          Point CU
 ro
4-
 m
  Fan
         12-1/4"  exit line
          x-Outlet Sampling Port, E

           Access Flange
            Venturi
            Scrubber
          TPacked
          Bed
          Scrubber
       Recycle
        Acid
        Tank
90"
-  Sampling Site

       Cl
                       4-7/8" Vent Line
                            Product
                            Storage
                              Tank
                                                       —Vs
                                                8-7/8".
                                              Vent Line
                                                          24"

                                                          ~Sampling Site

                                                                 C2

                                                          74"
                                      Barometric
                                      Seal Tank
      FIGURE 1  DUCTWORK AND SAMPLING SITES AT IMC  SUPERPHOSPHORIC
                ACID PLANT

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Three sets of samples were taken to determine total fluoride



content of the gas streams.  Moisture, carbon dioxide, and



oxygen contents of the gas streams were also measured; velocity,



temperature and total gas flow were determined for each test.



Samples of feed, product, and recycle acid were taken during



each run, as well as scrubber water samples.  Each stack gas



sample extended over a two hour period.

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II.  SUMMARY OF RESULTS



     During the first two runs, the plant was operating under



normal process conditions.  However, during the third test



some puffing of gases was noticed at the inlet ducts and the



flow rates were slightly lower indicating that the scrubber



could have been partially plugged up.






     Tests on the vent leading to the scrubber from the



recycle acid tank were characterized by extremely high fluoride



concentrations.  This high concentration of what was apparently



silicon tetrafluoride caused plugging problems in the sampling



train.  In addition, reactions between HF, SiF. , and H_0



in the impinger depleted the water in the impingers, formed a



white precipitate, and caused a reduced fluoride collection



efficiency for this train.





     A fume was exiting from the sample train pump.  For this



reason fluoride concentrations reported for the recycle tank



inlet to the scrubber are probably lower than the true values.






     Total measured vent gas flows were greater on the scrubber



outlet as compared to the two inlet lines.  This is partly due



to the leaks around the scrubber which caused ambient air to



leak into the scrubber and connecting duct work.






     A complete summary of stack gas conditions and emission



levels for each test run are given in Tables 1-3.

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                                     Table  1
                               Summary  of Results
                              Inlet  - Recycle Tank
Run Number
Date
Stack pressure, inches Hg
Stack gas moisture,  % volume
Average stack gas temperature,  °F.
Stack gas flow rate  0 S.T.P.*.  SCFM
Vol. Gas Sampled @ S.T.P.*,  SCF
Fluoride, water soluble,  mg
Fluoride, total, mg
Fluoride, water soluble,  gr/SCF
Fluoride, total, gr/SCF
Fluoride, water soluble,  gr/CF  stfc.  cond,
Fluoride, total, gr/CF stk.  cond.
Fluoride, water soluble,  Ib/hour
Fluoride, total, Ib/hour
Fluoride, water soluble,  Ib/ton P?0j.  Fed.
Fluoride, total, Ib/ton P    Fed.
1
2/29/72
30.2
15.8
206
165
37.9
115000
115033.4
46.7
46.7
31.3
31.3
66.1
66.1
2.9
2.9
2
2/29/72
30.2
8
225
146
24.7
30200
30210.5
18.9
18.9
13.4
13.4
23.6
23.6
1.1
1.1
3
3/1/72
30.2
9.7
207
138
16.2
171000
171099
162.1 .
162.2
118.6
118.7
192.3
192.4
8.7
8.7
* Dry, 70°F., 29.92 inches  Hq.

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                                Table 2
                          Summary of Results
                          Inlet - Seal  Tank
Run No.                                           123

Date                                           2/29/72   2/29/72    3/1/72

Stack pressure,  inches  Hg                        30.2      30.2       30.2

Stack gas moisture,  % volume                      2.7       2.5        2.0

Average stack gas temperature,  °F.               161       170        154

Stack gas flow rate  @ S.T.P.,  SCFM               319       357        288
                        *
Vol. gas sampled @ S.T.P.,  SCF                  74.4      77.0       62.9

Fluoride, water soluble, mg                     3900      2100       5400

Fluoride, total, mg                              3921      2103       5416

Fluoride, water soluble, gr/SCF                 0.81      0.42       1.32

Fluoride, total, gr/SCF                         0.81      0.42       1.33

Fluoride, water soluble, gr/CF stk.  cond.        0.67      0.34       1.12

Fluoride, total, gr/CF stk. cond.                0.68      0.35       1.12

Fluoride, water soluble, Ib/hour                2.2       1.3        3.3

Fluoride, total, Ib/hour            _           2.2       1.3        3.3

Fluoride, water soluble, Ib/ton P205 Fed.        0.10      0.06       0.15

Fluoride, total, Ib/ton P0  Fed.                0.10      0.06       0.15
*Dry, 70°F., 29.92 inches Hg.

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                                Table  3
                          Summary  of Results
                                Outlet
Run No.

Date

Stack pressure, inches  Hg

Stack gas moisture,  % volume

Average stack gas temperature,  °F.

Stack gas flow rate  @ S.T.P.,  SCFM

Vol. gas sampled @ S.T.P. ,  SCF

Fluoride, , water soluble,  mg

Fl uoride, total , mg

Fluoride, water soluble,  gr/SCF

Fluoride, total, gr/SCF

Fluoride, water soluble,  gr/CF stk.  cond.

Fluoride, total, gr/CF stk.  cond.

Fluoride, water soluble,  Ib/hour

Fluoride, total, Ib/hour

Fluoride, water soluble,  Ib/ton P
                                     Fed
Fluoride, total , Ib/ton P205 Fed.

Scrubber efficiency, %
1
2/29/72
30.2
3
87
812
92.5
309
309
0.05
0.05
0.05
0.05
0.36
0.36
0.02
0.02
99.5
2
2/29/72
30.3
3
94
779
90.8
471
472
0.08
0.08
0.07
0.07
0.53
0.53
0.02
0.02
97.9
3
3/1/72
30.2
2.3
90
586
71.2
404
405.7
0.09
0.09
0.08
0.08
0.44
0.44
0.02
0.02
99.8
*Dry, 70°F., 29.92 inches Hg.

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III.  SAMPLING PROCEDURES
              A


     All gas  streams were  sampled isokinetically by using


 a modified EPA particulate sampling train and following


 the sampling  procedures  described in Method  5 of the Federal


 Register of December 23, 1971.  The sampling train as shown


 in  Figure 2 consisted of a stainless steel button-hook


 nozzle, a heated Pyrex glass probe contained in a steel


 sheath, a Greenburg-Smith  impinger without a tip, a second


 impinger with a tip, a third impinger without a tip, an


 80  millimeter Whatman No.  1 paper filter, and a final


 impinger containing approximately 200 grams  of indicating


 type silica gel.  The first and second impingers contained


 100 ml each of distilled water at the beginning of each


 test.  The third impinger  was initially dry.  All impingers


 were contained in an ice-water bath and the  temperature of


 the gases leaving the fourth impinger was in the 65 to 70°F


 range.  The filter was not heated.  An air tight vacuum


 pump, dry gas meter, orifice, and associated valves, connectors,


 thermometers, and manometers completed the train.




     Due to the high fluoride content of the gases from the


 acid recycle  tank, the train used here was further modified


 during the last two runs by adding another straight tip


 impinger before the filter and adding 50 ml. of water to


 this impinger.

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                                                THERMOMETER
            HEVERSE-TYPE
            PI TOT TUBE
             STACK
                                                        CHECK
                                                        ~VALVE
                                      BY-PASS VALVE   VACUUM

                                        MAIN .VALVE GAUGE
                         DRY TEST METER
FIGURE 2.   SAMPLING  TRAIN USED  TO  DETERMINE
              FLUORIDE  CONCENTRATIONS

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     A type 'S1 pitot tube was attached to the probe to


measure the velocity head of the stack gas.  The sampling


rate was continually adjusted to maintain isokinetic sampl-


ing rates by means of a nomograph which related the pressure


drop across the orifice after the meter with the velocity


head measured by the pitot tube.  Stack gas temperatures


were measured with long stem dial thermometers.



     In a typical run to determine fluoride concentrations,


the train was assembled and checked for leaks by plugging


the first impinger and drawing a vacuum of 15" Hg.  The


probe and nozzle assembly was then attached to the impinger


and the train positioned at the first sampling point.  Each


point along the stack diameter was sampled for ten minutes.
                                          •    -    -        /-T •

A two hour sampling period was used, except at the inlet


site from the recycle tank where a 60 minute sampling period


was used because of heavy fluoride concentrations.  This period


was extended over a two hour period by running the train in


15 minute on-off cycles.  At each point the velocity head,


stack gas temperature, final impinger temperature, meter


temperatures, meter reading, and pump suction pressure drop


were measured and recorded.  All data sheets for these tests


are attached in Part B of the Appendix.
                          10

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     Upon completion of sampling, the train was completely



disassembled, the condensate volume measured, and the



silica gel weighed on a triple beam balance at the site.



The water in the impingers was poured into plastic  (Nalgene)



wide mouth bottles.  The paper filter and all washings  from



the probe and all glassware were also placed in this same



container.  When necessary the probe was also brushed to



remove solid matter.  All train components were then dried



with acetone and the train reassembled  for the next run.



Each container was immediately labeled.  Much of the white



precipitate in the inlet train on the recycle tank line



could not be removed from the_inside__ of;„ _thei irnpj.nger	



stems.





     Feed, product, and scrubber water  samples were also



placed in plastic bottles and labeled.  All samples were



submitted to Mr. J. Rom of EPA for future analysis.








     Moisture content of the gas stream was determined  by



making a preliminary run with this same train without a



filter.   This was accomplished by running the train at  a



sampling rate of approximately 0.75 cfm for 30 minutes  and



measuring the moisture condensed and the weight gain of the



silica gel.
                           11

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     Carbon dioxide and oxygen content of the gas stream



were measured with a standard Orsat apparatus by drawing



samples from the stack directly into the Orsat apparatus



through a one-quarter inch diameter stainless steel probe.



The probe was carefully purged with stack gas before taking



the sample.  This procedure was deemed sufficiently accurate



to determine the molecular weight of the stack gases.
                           12

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IV.  ANALYTICAL PROCEDURES




     Water soluble fluorides were determined by a sulfuric




acid distillation followed by the SPADNS - Zirconium Lake




Method.  Water insoluble fluorides were first fused with




NaOH followed by a sulfuric acid distillation then by the




SPADNS - Zirconium Lake Method.






     P-O- analysis of the stack effluent was done by the




Molybdovanadophosphate Colorimetric Method.






     For more details of exact methods used, see Appendix,




Part C.
                          13

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V.  APPENDIX
     14

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           APPENDIX A




Emission Calculations and Results

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                              NOMENCLATURE


   PB - Barometric pressure,  inches  Hg
   PS - Stack pressure,  inches Hg
   As - Stack area, sq.  ft.
   TS - Stack temperature, °R
   TM - Meter temperature,   R
   H_  - Average square root  of velocity  head,  /inches  HpU"
   AH - Average meter orifice pressure differential, inches H20
   AN - Sampling nozzle  area, square feet
   CP - S-type pitot tube correction factor
   VM - Recorded meter volume sample, cubic  feet  (meter  conditions)
   VC - Condensate and silica gel  increase in  impingers,  milliliters
   Po - Pressure at the  dry  test meter orifice,   PB +  TT~^ inches Hg
  STP - Standard conditions,  dry,  70°F,  29.92  inches Hg
  VWV - Conversion of condensate in  milliliters  to  water  vapor  in  cubic feet  (STP)
VSTPD - Volume sampled,  cubic feet (STP)
   VT - Total  water vapor volume and dry  gas  volume samples,  cubic feet (STP)
    W - Moisture fraction of stack gas
  FDA - Dry gas fraction
   MD - Molecular weight of stack gas,  Ibs/lb-mole  (dry conditions)
   MS - Molecular weight of stack gas,  lbs/lb/-mole (stack  conditions)
   GS - Specific gravity of stack gas,  referred  to  air
   EA - Excess air, %
    U - Stack  gas velocity, feet per minute
   OS _ Stack  gas flow rate, cubic feet per minute  (stack conditions)
   OD - Stack  gas flow rate, cubic feet per minute  (dry conditions)
OSTPD - Stack  gas flow rate, cubic feet per minute  (STP)
 PISO - Percent isokinetic volume sampled (method described in  Federal Register)
 Time - Total  sample time, minutes

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              EQUATIONS FOR CALCULATING  FLUORIDE EMISSIONS
   VWV =



 VSTPD =



    VT =



 '.   W =




   FDA =



FMOIST =



    MD =



    MS =



    GS =



    EA




     £



    QS



    QD



 QSTPD



  PISO
13.6
         - TM
(0.0474) x (VC)



(17.71 x (VM) x  (PB +



(VWV) + (VSTPD)                 e




(VWV)-5;(VT)   '  .          ,,  .  .                              •



(1.0) - (W)                                    •>•_'.



Assumed moisture fraction                               ,    '



(0.44 x % CO  ) + (0.32  x % 02) + (0.28 x % N2) +  (0.28  x % CO)




(MD x FDA) +  (18 x W)




(MS) '-5- (28.99)
             02  -
             x % N2) -
                                                  0   -
=  [(100) x



=  (174) x (CP) x  (H)  x V(TS x 29.92)-v-(GS x PS)




=  (U) x (AS)                                                  ,   •
                      • •                                  r   •     .



=  (QS) x  (FDA)




=  (530) x (QD)-T-(TS) X (PS) f (29.92)



= Qo.oo267 x VC  x  TS) -}- (PQ x TS x VM ^ TM)]  -7- [[(Time  x U x PS x AN)]
Fluoride Emissions:      -  '




       MG = Milligrams of fluoride from lab analysis




       Grains/SCF =  (0.01543) x (MG).-i- VSTPD
                               »                .          t



       Grains/CF, Stack Cond.  = (17.71) x  (PS) x  (FDA)  x  (Grains/SCF)




       Lbs/l^our  = (Grains/SCF) x (0.00857) x  (QSTPD)  .




       ?2®5 ^e^  ~ Tons/hour,  determined from  plant  data

                             G   •                        €

       Lbs/ton P2P  Fed = (Ibs/hour) -^- (Tons/hour P205 Fed)
                                                                   (TS)

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               EMISSION DATA
             I.M.C. SUPER ACID
                  OUTLET
1) Run Number
2) Date
3) Time Began
4 ) Time End
5) Barometric Pressure, In Hg
6) Meter Orifice Pressure Drop, in H»0
7) Vol Dry Gas, Meter Cond. Cubic Feet
8) Average Gas Meter Temperature, Deg F
9) Vol Dry Gas, S.T.P., Cubic Feet
10) Total H20 Collected, Ml
11) Vol H20 Vapor Collected, S.T.P., Cu.Ft.
12) Stack Gas Moisture, Percent Volume
13) Assumed Stack Gas Moisture, Pet Vol
14) Percent C02
15) Percent 02
16) Percent CO
17) Percent N->
' £.
18) Percent Excess Air
19) Molecular Weight of Stack Gas, Dry
20) Molecular Weight of Stack Gas, Stk Cond.
21) Stack Gas Specific Gravity
22) Avg. Square Root (Vel Head) , in H2O
23) Average Stack Gas Temperature, Deg F
24) Avg. Square Root (Stk Temp x Vel Head)
25) Pitot Correction Factor
26) Stack Pressure, in Hg , Absolute
27) Stack Gas Vel, Stack Cond, F.P.M.
28) Stack Area, Sq . Feet
29) Effective Stack Area, Square Feet
30) Stack Gas Flow Rate, S.T.P., SCFMD
31) Net Time of Test, Minutes
32) Sampling Nozzle Diameter, Inches
33) Percent Isokinetic
34) Fluoride - Water Soluble, MG
35) Fluoride - Total, MG
36) Fluoride - Water Soluble, GR/SCF
37) Fluoride - Total, GR/SCF
38) Fluoride - Water Sol., GR/CF,STK CND.
39) Fluoride - Total, GR/CF,STK CND.
40) Fluoride - Water Soluble, LB/HOUR
41) Fluoride - Total, LB/HOUR
43) Fluoride - Water Sol., LB/TON P205 FED
44) Fluoride - Total, LB/TON P20s FED
1
2/29/72
12:12
14:12
30.2
1.69
99.1
115.5
92.488
59.8
2.83
3
3.5
0.1
20.8
0.1
79
7860
28.85
28.53
0.98
0.309
87
7.236
0.83
30.2
1052.1
0.82
0.82
812
120
0.375
101.3
309
309
0.0514
0.0514
0.0485
0.0485
0.3579
0.3579
0.0158
0.0158
2
2/29/72
16:00
18:00
30.3
1.61
98.28
123.5
90.756
59
2.8
3
4
0.1
20.8
0.1
79
7860
28.85
28 .52
0 .98
0 .298
94
7 .017
0.83 .
30.3
1020.3
0.82
0.82
779
120
0.375
103.9
471
472
0 .0799
0.0801
0.0743
0.0745
0.5332
0.5344
0.0238
0.0239
3
3/1/72
8:57
10 :57
30.2
0.89
75 .15
106
71.183
35
1.66
2f\
. 3
4
0.1
20 .8
0 .1
79
7860
28 .85
o o a
£ o • D
Or\ r\
. yy
0 .222
90
5 .214
0.83
30.2
757.1
0.82
0.82
586
120
0.375
108.2
404
405.7
0.0874

0.0878 !
6.0825
0.0828 1
0.4391 '
0.4400 '
0.0190
Q. 0190 i

***S.T.P.
,  70 DEGREES F, 29.92 INCHES MERCURY***

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                              EMISSION DATA
                            I.M.C. SUPER ACID
                            INLET - SEAL TANK
1) Run Number
2) Date
3) Time Began
4) Time End
5) Barometric Pressure, In Hg
6) Meter Orifice Pressure Drop, in H~0
7) Vol Dry Gas, Meter Cond. Cubic Feet
8) Average Gas Meter Temperature, Deg F
9) Vol Dry Gas, S.T.P., Cubic Feet
10) Total H20 Collected, Ml
11) Vol H20 Vapor Collected, S.T.P., Cu.Ft.
12) Stack Gas Moisture, Percent Volume
13) Assumed Stack Gas Moisture, Pet Vol
14) Percent C02
15) Percent 02
16) Percent CO

17) Percent No
18) Percent Excess Air
19) Molecular Weight of Stack Gas, Dry
20) Molecular Weight of Stack Gas, Stk Cond.
21) Stack Gas Specific Gravity
22) Avg. Square Root (Vel Head) , in H20
23) Average Stack Gas Temperature, Deg F
24) Avg. Square Root (Stk Temp x Vel Head)
25) Pitot Correction Factor
26) Stack Pressure, in Hg , Absolute
27) Stack Gas Vel, Stack Cond, F.P.M.
28) Stack Area, Sq . Feet
29) Effective Stack Area, Square Feet
30) Stack Gas Flow Rate, S.T.P., SCFMD

31) Net Time of Test, Minutes

32) Sampling Nozzle Diameter, Inches
33) Percent Isokinetic
34) Fluoride - Water Soluble, MG
35) Fluoride - Total, MG
36) Fluoride - Water Soluble, GR/SCF
37) Fluoride - Total, GR/SCF
38) Fluoride - Water Sol., GR/CF,STK CND.
39) Fluoride - Total, , GR/CF,STK CND.
40) Fluoride - Water Soluble, LB/HOUR
41) Fluoride - Total, LB/HOUR
43) Fluoride - Water Sol., LB/TON P205 FED
44) Fluoride - Total, LB/TON P2®5 FED
1
2/29/72
11:30
13:30
30.2
1
76.879
94.5
74.35
43
2.04
2.7
3.5
0.1
21
0.1
7Q Q
/ o • o
193981
28.86
28.57
n QQ
U • -/ -/
0.246
161
_[_ \J -J_
6.136
n R •}
U . O ~J
30.2
891.6
n 43
\j • rr _J .
0 43
\J • T *J
319

120

0 .375
108 .8
3900
3921
0.8078
0.8121
0.6723
0.6759
2.2085
2.2204
0.0977
0.0982
2
. 2/29/72
15:55
17:55
30.2
1.25
81.146
105.5
76.997
41.8
1.98
2.5
3.5
0.1
21
0.1
•70 o
/ o . o
193981
28.86
28.58
OQQ
• .7 _7
0.277
170
-U / \J
6.942
083
\J • O J
1008.3
0.43
0 43
\J • ^ *J
357
•*J -J 1
T O f\
] S ll
_L £* \J
0*\ *-t p"
^ / s
• -*J / «J
100 9
J- \J \J • J
2100
2103
0.42
0.4206
0.3451
0.3456
1.2834
1.2852
0.0573
0.0574
3
3/1/72
9:05
11:05
30.2
0.85
65 .014
94
62.909
26 .8
1.27

3.5
0 .1
21
0.1
78 8
/(_)•'-'
193981
28.86
28.64
On o
• ,/ -7
0.218
154
J. ~J T
5.437.
0 83
\J • O — t
30 2
•j \j • &*
788.9
0.43
0 . 43
288
£* \j \j
^ *\ f\
i / n
J_ £M \J
OT "7 C*
T / T
• -J 1 -J
102.1
C A f\ A
b40U
5415.6
1.3219
1.3257
1.1206
1.1238
3.2602
3.2696
0.1469
0.1473
***S.T.P. «~>DRY, 70 DEGREES  F,  29.92 INCHES MERCURY***

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                              EMISSION DATA
                            I.M.C.  SUPER ACID
                           INLET  -  RECYCLE TANK
1) Run Number
2) Date
3) Time Began
4) Time End
5) Barometric Pressure, In Hg
6) Meter Orifice Pressure Drop, in H~0
7) Vol Dry Gas, Meter Cond . Cubic Feet
8) Average Gas Meter Temperature, Deg F
9) Vol Dry Gas, S.T.P., Cubic Feet
10) Total H20 Collected, Ml
11) Vol H20 Vapor Collected, S.T.P., Cu.Ft.
12) Stack Gas Moisture, Percent Volume
13) Assumed Stack Gas Moisture, Pet Vol
14) Percent C02
15) Percent 02
16) Percent CO
17) Percent N->
' £
18) Percent Excess Air
19) Molecular Weight of Stack Gas, Dry
20) Molecular Weight of Stack Gas, Stk Cond.
21) Stack Gas Specific Gravity
22) Avg. Square Root (Vel Head) , in H2O
23) Average Stack Gas Temperature, Deg F
24) Avg. Square Root (Stk Temp x Vel Head)
25) Pitot Correction Factor
26) Stack Pressure, in Hg , Absolute
27) Stack Gas Vel, Stack Cond, F.P.M.
28) Stack Area, Sq. Feet
29) Effective Stack Area, Square Feet
30) Stack Gas Flow Rate, S.T.P., SCFMD
31) Net Time of Test, Minutes
32) Sampling Nozzle Diameter, Inches
33) Percent Isokinetic
34) Fluoride - Water Soluble, MG
35) Fluoride - Total, MG
36) Fluoride - Water Soluble, GR/SCF
37) Fluoride - Total, GR/SCF
38) Fluoride - Water Sol., GR/CF,STK CND.
39) Fluoride - Total, GR/CF,STK CND.
40) Fluoride - Water Soluble, LB/HOUR
41) Fluoride - Total, LB/HOUR
43) Fluoride - Water Sol., LB/TON 'P2°5 FED
44) Fluoride - Total, LB/TON P205 FED
1
2/29/72
12:00
13:45
30.2
0.64
38.745
87.5
37.917
150.6
7.14
15.8
13.9
1
20
0.1
78.9
1923
28.96
27.22
0.94
0.494
206
12.753
0.83
30.2
1898.1
0.13
0.13
165
80
0.25
109
115000
115033.4
46.7078
46.7214
31.3398
31.3489
66.133
66.1522
2.9262
2.9271
2
2/29/72
16:10
18:10
30.2
0.45
25.67
97.5
24.659
45.1
2.14
8
13.9
1
20
0.1
78.9
1923
28.96
28.09
0.97
0.412
225
10.782
0.83
30.2
1579.9
0.13
0.18
146
60
0.25
108.9
30200
30210.5
18.8604
18.8669
13.4539
13.4586
23.6302
23.6384
1.0549
1.0553
3
3/1/72
9:00
11:00
30.2
0.43
16.65
89
16.2.41
36.7
1.74
9 .7
13.9
1
20
0.1
78.9
1923
28.96 	
^"tr^ fl
&7z3L —
0.96
0.391
207 .
10.092
0.83
30.2
1483.7
0;13
0.13
138
60
0.25
74 .4
171000
171099
162.1434
162 .2373
118 .5943
118.6618
192.3198
192 .4312
8.6631
8.6681
***S.T.P.. «-->-DRY,  70 DEGREES F,  29.92 INCHES MERCURY***

-------
Run 1


    2


    3
Flow:
Total Fluoride:
319 (DSCFM)
2.2 (#/HR)

357
1.3
288
3.3
                                                 I.M.C.  Super Acid
                                                Scrubber Efficiency
                         Seal Tank
                     Recycle Tank
Run 1


    2


    3
   Flow:
   Total Fluoride:
   165  (DSCFM)
   66.1(#/HR)

   146
   23.6

   138
   192.4
                                                  68.3  '
                                                  24.9
                                                 195.7
                                                               Scrubber
Efficiency:   99.5


             97.9


             99.8
Flow:
Total Fluoride:
                                                                                                       Outlet
812 (DSCFM)
0.36 (#/HR)

779
0.53

586
0.44

-------
APPENDIX B




Field Data

-------
     This section contains all field data collected during

these tests.   Data sheets are arranged in the following

order:


     Preliminary Pitot Traverse - Inlet on Recycle Tank Line

     Preliminary Pitot Traverse - Inlet on Barometric Seal Tank Line

     Preliminary Pitot Traverse - Scrubber Outlet

     Moisture Run-Meter Data - Inlet on Recycle Tank Line

     Moisture Run-Meter Data - Inlet on Barometric Seal Tank Line

     Moisture Run-Meter Data - Scrubber Outlet

     Meter Data Sheet, Line from Recycle tank-Scrubber Inlet Test 1

     Meter Data Sheet, Line from Barometric Seal-Scrubber Inlet
       Test 1

     Meter Data Sheet, Vent from Scrubber Outlet Test 1

     Meter Data Sheet, Line from Recycle tank-Scrubber Inlet Test 2

     Meter Data Sheet, Line from Barometric Seal-Scrubber Inlet
       Test 2

     Meter Data Sheet, Vent from Scrubber Outlet Test 2

     Meter Data Sheet, Line from Recycle tank-Scrubber Inlet Test 3

     Meter Data Sheet, Line from Barometric Seal-Scrubber Inlet
       Test 3

     Meter Data Sheet, Vent from Scrubber Outlet Test 3

     Orsat Analyses

-------
                                   GAS VELOCITY AND VOLUME DATA
       VELOCITY  TRAVERSE DATA
Point
1
2
3
4
5
6


















Position
Inches3
0.2
e>.7
1,5
3,5
-f.z.
4-. 7


















Total
Average
Reading, Ap
"H2°
o. \°>
. 12.
, /5
.)(«
,ie>
.10


















-
—
VAP
0.43^
.346
•3fl7
.4dO
.424-
.316


















2.3£X>
5-sas
T °F
S
IfiO




1 '



















ISO
                                    Test No.
                                    Location
                                                                                        PRELSM
                                                                                        IMC
Stack Inside Dimensions   4
                                                                         I,D.
                                                                  SCRUBBER \NL_ET
                                                                   RECYCLE TANK
                                          Stack Area, A  = 	.	
                                                       S         -r "'•-'
                                          Barometric Pressure, P, =
                                          Stack Gage Pressure =
                                          Stack Abs. Pressure, P  =
                                                                S
                      Stack Gas Temp., T^ -
                         ecula
                         = 174
      J3J.£     "Hg
         	 "H20
         *3T  "H20 -
              13.6
   |-7Q   °F + 460 =
                                            Pb =
                                                                                              >R
                                          Molecular Weight of Stack Gas, M  =
                                          V
                                          Vs -
              Cp V T  x 29.92 x  29^  ft/min.
                                                                          M
                              Xl

                                          Q,  Volume =
ft/min. x
                                                             sq.  ft.  =
                                                        cfm
                                            r, Standard Volume at 70°F and 29.92  "Hg(Wet Basis)=
                                                Q x 530  x Ps    = 17.7 x    154   x   -30. i ^  =
                                                    T      29.92
                                          Qs = Qw x (100-W)/100 =
a) From outside of port  to  sampling  point.
   Pitot tube     s	
   Manometer 	
   Thermometer
                                J4  WALL THICKNESS
                                   BUILD-UP
   Data Recorder
   Date       £-
R.A.
                       PEDCo- ENVIRONMENTAL
                            SUITE S •  ATKINSON  SQUARE
                                  CINCINNATI. OHIO 45246
                                            513 / 77 1-4330

-------
                           GAS  VELOCITY AND VOLUME DATA
VELOCITY TRAVERSE DATA
                                                                      Test No.
Point
1
z.
3
4
5
(a
-7
P>
















Position
Inches3
0.3
1,0
1,7
3,ft
6>.o
7,2.
•7.*>
8.5
















Total
Average
Reading, Ap
"H2°
• II
,<3P>
.14
.Ok
.07
.O.n
.Q-5
.03
















-

V/AP
0.332.
-3OO
.374
• ZAf
.e&5
.£2.4
.za4
-\73
















2.137
0.267
T °F
S
l<^0
1




I
t

















/(/,0
                                                                              Location -. j
                                          Stack Inside Dimensions   Q^/s" I.D.
                                                              . 43O|    sq.  ft.
                                                                           :     "Hg
                                                                           — "H2°
                                                                                SCRUBBER INLET
                                                                                BAR. SEAL
                                   Stack Area,  A  =
                                                S
                                   Barometric Pressure, P,  = _
                                   Stack Gage Pressure = 	-2.Q
Stack Abs. Pressure, P  =
                      S
Stack Gas Temp., T  = 	[
                                                                       "H0 + P. =   "o,
                                                                               "H20  +
                                                                               13.6
                                                                          F +  460  =
                                                                                        R
                                  Molecular Weight of Stack Gas, M  =
                                  V   =  174  \/Ajp  Cp V T  x 29.92 x 29"* ft/min.
                                                                   M
                                  Q, Volume  =
                                                                ft/min. x
                                        sq.  ft.  = 422   cfm
                                  Q  ,  Standard Volume at 70°F and 29.92 "Hg(Wet Basis)=
                                         Q  x  530   x Pg	  = 17.7 x
                                             TS      29.92
                                   Qs  =  Qw  x  (100-W)/100 = 	
                                                                            42.2.
                                          X  -50.
                                                                                        6ZO
a) From outside of port to  sampling  point,
   Pitot tube 	^	
   Manometer 	o-l"
   Thermometer
             C-r.F.
   Data Recorder
   Date         2. -2°>-~??
                                                                    VERTICAL
                                                                    '/4" WALL THICKNESS
                                                                    ~3/4" BUILD -up
                       PEDCo- ENVIRONMENTAL
                             SUITE 8 •  ATKINSON  SQUARE
                                  CINCINNATI. OHIO 4524-6
                                            513 /771-433O

-------
                                   GAS VELOCITY AND VOLUME DATA
       VELOCITY TRAVERSE  DATA
Point
1
2.
3
4-
.5"
'&
V
8
<£
10
II
\2.












Position
Inches3
0,2.4
0. 8Z
1 .+5
?-. 15
3.IO
4^35
7- "50
9.2
10.0
10. A
n-.i
\\A












Total
Average
Reading, Ap
"H2°
O.Oft
0. 10
0. IO
o,/l
•3,11
f).l\5
0,\\
$.11
f*.O°>5
0,05
o .oe>
•:?< ,07












- •
-
\/Ap
£.28:3
.31k
.-3/6
•33Z
,332.
.33^
-3.^2.
,332
.30S
,3oo
-3OO
-2^5"












•3.7-5S
a. 3/3
Ts°F
S5
/
1
/








-------
                               PARTICULATE FIELD SAMPLING METER  DATA
Plant
MC
                                                      Filter No.
Run Number   MOISTURE
Location  RECYCLE - INLET SCRUBBER
Date  2--2.5-7Z. Time   IO'.3OA.M.
Operator   R.S.A. •/ Gr.F.	
Sample Train Number   3	
Meter Number 	4.	
AH@
Barometric Pressure,  in.' Hg 3O,z
Assumed Moisture,  % _ ^ _ __
Assumed Meter Temp.,  °F    _
Stack Gage Pressure _ ---
                                                      Probe Tip Diameter, in.    — -
                                                      Condensate Collected, ml.   3
                                                      'C'  Correction Factor    . —
                                                                                     "H2°
Point
3"/*/

















Total
Avg.
Time
Min.
10
10
10















30

Dry Gas Meter
^Volume
ft3
Vm
38.Z.O
43,41
4-8. &l















\G,bl

Inlet
Temp.
oF
0^
ft?
B&















•2.S^>
8(*
Outlet
Temp.
°F
80
8Z.
82.















244
a i
Velocity
Head Ap
"H2°




















Orifice AH
"H2°




















Pump
Vacuum
"Hg
3.5"
4.0
4.0

















Filter
Temp.
oF




















Impinger
or
Condenser
Temp. , °F




















Stack Gas
Temp . , ° F
Ts
/ -70
I -70
170












•




Leakage Rate @ (5- "Hg =  Q'.Q\~7   cfm
                                 - 10
                                                      PEDCo-ENVIRONMENTAL
                                                           SUITE 8  «  ATKINSON SQUARE
                                                                CINCINNATI. OHIO  45346
                                                                           5 1 3 I 7 7 1-433O

-------
 Plant
PARTICULATE FIELD  SAMPLING METER DATA
                         Filter No.
Run  Number_
Location SCRUBBER IN|LE=T -
Date 2--Z.t?)-7Z-  Time  <>,', 45  A.M.
.Operator  R.S.A. 2* G-.FI	
Sample  Box Number	|	
Meter Box Number     -x
                                                     Barometric Pressure, in. Hg
                                                     Assumed Moisture, %
                                                     Assumed Meter Temp., °F
                                                     Stack Gage Pressure	
                                                     Probe Tip Diameter, in.
                                                     Condensate Collected, ml.
                                                     'C'  Correction Factor
                                                                  -"H2°
                                                        'Z..9
Point
t
3"/W.
\















Total
,AV8















267
6?
Outlet
Temp.
oF
~75
-7X
82.















235-
S>3.7
Velocity
Head Ap
"H2°




















Orifice AH
"H20




















Pump
Vacuum
"Hg
4
5
.5

















Box
Temp.
op




















Impinger
or
Condenser
Temp. , °F




















Stack
Temp.
°F
\(aO '
1 6cj
t / ^^
1 wtj
















160
Leakage Rate  @ |5"Hg =
    CF/M
                             3O.2.
                                                               PEDCo - EN VIRON M ENTAL
                                                                     SUITE S •   ATKINSON  SQUARE
                                                                          CINCINNATI. OHIO 45346

-------
 Plant   IMC
PARTICULATE FIELD SAMPLING METER DATA
                        Filter No.
 Run Number  MOISTURE.
 Location SUPER PH^OS. OUTLET
 Date 2.-Z9-7Z  Time /Q.-QoA.M.
 Operator   L..E, '	
 Sample Box Number    2.  	
 Meter Box Number%-
                        Barometric Pressure,  in.  Hg
                        Assumed Moisture,  %    	
                        Assumed Meter Temp.,  °F
                        Stack Gage Pressure	
                        Probe Tip Diameter,  in.
                        Condensate Collected, ml.
                        'C1 Correction Factor
                              -"H2°
Point

6" IN

















Tnt^l
Avq-
Time
Min.
10
10
















2. £3

Dry (
Volume
'ft3
IZ-7.332
133. "5O
I5-|. 0215















23.7(9

3as Mett
Inlet
Temp.
OF
110
I2.Z

















Mfe
sr
Outlet
Temp.
°F
8>^»
&•&

















ec*
Velocity
Head Ap
"H2°




















Orifice AH
"H2°




















Pump
Vacuum
"Hg
2.0



















Box
Temp .
OF




















Impinger
or
Condenser
Temp., °F
S--7
57

















5~7
Stack
Temp.
oF
80
&(D

















60
Leakage Rate @ 15 "Hg =
   CFM
                                 = 22.4
PEDCo-ENVIRONMENTAL-
           S  •  ATKINSON SQUARE
          CINCINNATI. OHIO  45346

-------
                               PARTICULATE FIELD SAMPLING METER DATA
Plant
              TMC
                                                                 Filter No.
Run Number
Location IMUET- UgC^CLE.
Date  2--zcl.-T7Z.  Time  \1\co~
Operator  RSfr k
                                                                 Barometric Pressure,  in.  Hg "56,
                                                                 Assumed Moisture,  %       13. *•}
                                                                 Assumed Meter  Temp.,  °F
                                                                 Stack Gage Pressure  —  C
                                                                                                -"H2°
Sample Train Number _
Meter Number 	<-j-_
AH@
       1.40
                  fl.TS"
                                                                 Probe Tip Diameter,  in.
Condensate Collected, ml.
'C1 Correction Factor
0/5-r
tf-3
/. 2.
2.7-
-?.^r
Point
\
'L
3
+














Total
Avg.
Time
Min.
2.0 *
20
2.O
-LO **














SO

Dry Gas Meter
Volume
ft3
Vm
M-S.fB^S
51 . °i'00
01. ''no
1^. A^O
Al. GM-0
'












35.T4£

Inlet
Temp.
oF
e^
9^
^6?
SI














35^
q^
Outlet
Temp.
oF
fit,
SM-
Sk
/?^














3m
«^
Velocity
Head Ap
"H2°
O.-27
<5,7.0
0.2. S
O.Z6*
















Orifice AH
"H2°
/5.T3.
5,53
0,^5
tf,t*T














12. 51
0,^4
Pump
Vacuum
"Hg
IH
\(*
11
^^-5 "














6-5.0
13,^
Filter
Temp.
OF
—
—
—















—
—
Impiricfer
or|'
Condenser
Temp . '/ ° F
&^
^0
4»a
^
.-:*!
;'v -
i, •
.,J .
\
fe?-








inc.
6^
*S tack -Gas
|cemp|J;;j.|
>-!S ' ' ni i-,'%-sS
#£' •'•'•*-& *»
3 U
IRQ
aio
220
ZlS",
>">t . ' ,C ri--'' " 'i'Ji "^ T«f","
•••n/ •:* .y.f.*J
§J': •..•i-'v^f-H
•j-j/ •.•'.'• T ^.*si'
.,U' -| :i rl
££• '•f-r*ii
aiv --'.1^4^








9^5"
20C9
Leakage Rate @  15 "Hg =
                                 cfm
                                                                 PEDCo-ENVIRONMENTAL
                                                                      SUITE S •  ATKINSON SQUARE
                                                                            CINCINNATI. OHIO 45246
                                                                                      51 3 / 77 1-433O

-------
                              PARTICULATE FIELD SAMPLING METER DATA
Plant
           TKAC
                                                                Filter No.
Run Number
                 I
Location JWUET - 8i - \'-3o
Operator   RSA
Assumed Meter Temp., °F 	
Stack Gage Pressure 	o
Sample Train Number 	
Meter Number 	3_
AH@    |.S"   0    0,ns C
                                                                                               -"H2°
                                                                Probe Tip  Diameter,  in.
                                                                Condensate Collected, ml.
                                                                'C' Correction Factor
                                                                                             M-3
pisr.
£,












6, .01
LOO
Pump
Vacuum
"Hg
5
M-
^
4
M-
4












2S
M.
Filter
Temp.
oF
-
_
-
-
—
—












—
—
Impinger
or
Condenser
Temp . , ° F
(tl
(tft
^
(si
10
m.












41 (o
^
StaclC Gas
Temp/J, •: °F
•. "'
-------
                               PARTICULATE FIELD SAMPLING METER DATA
Plant
             Iv\C
Run Number
Location Qin LET -
Date  1--i<\-~\ 2.  Time
Operator   t> E\-fev
Sample Train Number
Meter Number
AH@    i. 3^  g>    6,i
Filter No.
                        PHOSPHOR 1C
Barometric Pressure,  in.  Hg 36.
Assumed Moisture,  %      5, g
                                                                 Assumed Meter Temp.,  °F    | (&
1.6
x^.o
//• 7
Point
I
2
S
"4
5
&












Total
Avg.
Time
Min.
•2.0
20
Ze>
•2-0
2rt
2C












J2-0

Dry Gas Meter
Volume
ft3
Vm
151. 1*70
1^4.100
IRQ.^OO
^ft.flOO
e is. RO
2.3Z.&60
ZSd. 2T<5











q'l.ioo

Inlet
Temp .
oF
\OA
l^a
131
nz
H43
m3












-7^1
I3Z.
Outlet
Temp .
oF
8*1
^i
°i^
IOZ
fofo
I0t»












S^l
^1
Velocity
Head Ap
"H2°
6,0(^
6. 10
0, ID
0, >7_
Q. 16
0,10














Orifice AH
"H2°
1.10
i.ns
),n^
2./9^
l.lr
l.Ti












16. /C
l.(.°f
Pump
Vacuum
"Hg
7.0
16. £
n.o
VZ.A
13.0
l^.^












6-t.s
II. 0
Filter
Temp.
op
—
^
^.
-
--
—












—
—
Impinger
or
Condenser
Temp . , ° F
57
£(*
5*7
Sto
S^«
J5A












340
•^T
Stack Gas
Temp., °F
Ts
SO
85
6£
^O
RO
°I6












5ZO
ftl
Leakage Rate @  15 "Hg =
6
                                 cfm
PEDCo-ENVI RON MENTAL
     SUITE  B  •  ATKINSON  SQUARE
          CINCINNATI. OHIO 45346
                     513 l~7~7 1-4330

-------
                              PARTICULATE FIELD SAMPLING METER DATA
Plant
IMC
Run Number
Location
Date TA
               r BM^.
               Time 3; Sg" P.m.
Operator   6, P. \
Sample Train Number
Meter Number       3
                                                                Filter No.
                                                      Barometric Pressure, in. Hg
                                                      Assumed Moisture, %      3.S"
                                                      Assumed Meter Temp., °F
                                                      Stack Gage Pressure
                                                                                              -"H2°
                                                      Probe Tip Diameter, in.  . 3*1
                                                                Condensate Collected, ml.
                                                                'C' Correction Factor
                                                                                   . 8
Point
I
1
3
4-
£
(j>












Total
Avg.
Time
Min.
•2.0
1-0
•ZQ
zo
1£>
2.0












IZO

Dry Gas Meter
Volume
ft3
Vm
2^,n\\
ans. \oo
2 £8. -730
£T 1 . Q°tO
28M-. M-50
^l, MO
311, ftSl











filJ^t?

Inlet
Temp.
OF
100
1 \0
\\(o
HA
\-20
llfi












&8Z
)l>f
Outlet
Temp .
oF
P>3
&4
10fo
\OU-












SfiS
^7
Velocity
Head Ap
"H2°
o,nR
0, 6fe
0,07
0,07
0,G~I
6.0&














Orifice AH
"H2°
I.4S
l,^0
1, IT
l.iC
1. 11?
1,30












1,96
I.ZS
Pump
Vacuum
"Hg
£
g
-7
^?
ft
>5












M«4
n,3
Filter
Temp.
op
—
—
—
—
—
—












—
-
Impinger
or
Condenser
Temp . , ° F
L>-L
0-3
(*£
t>Z
ien
6>i












3^
(.S
Stack Gas
Temp . , ° F
Ts
l(*6
1^.0
IP)6
IG.O
no
no












IOZO
no
Leakage Rate @ 15 "Hg =
                      cfm
                                                                PEDCo-ENVIRONMENTAL
                                                                     SUITE 8 •  ATKINSON  SQUARE
                                                                           CINCINNATI. OHIO 45246
                                                                                     51 3 I-7-7 1-433O

-------
                               PARTICULATE FIELD SAMPLING METER DATA
Plant
          TMC
Run Number
Location I\MLET-
Date  2-7. ^-HZ  Time 14: \09\y\- k;>Q?.Nv\-
Operator   R. S. A •	
Sample Train  Number    3
Meter Number  	^£	
AH@
Filter No.
                                                                 Barometric  Pressure, in. Hg  "30.2-
                                                                 Assumed  Moisture,  % 	I 3. ^	•
                                                                 Assumed Meter Temp.,  °F
                                                                 Stack Gage  Pressure  - C>.
                               -"H2°
                                                                 Probe Tip Diameter,  in.   . 2S C
                                                                 Condensate  Collected,  ml.   t-4-5". )
                                                                  *C' Correction  Factor    0,
Point



3-
-

3


M








Total
Avg.
Time
Min.
(5-


IS


IS *'


15"








fe>O

Dry Gas Meter
Volume
ft3
Vm
^'S.O'ifl
^.ObO

^.o&o
\6^^30

lflcl.^0
1 n . a^

L 1 1 1 , 0 "30
)l?j ,lt->0







ZS.010

Inlet
Temp.
oF
loo
^^

4-
-------
Plant
                              PARTICULATE  FIELD SAMPLING METER DATA
                                                                 Filter No.
Run Number
Location
Date  -3-'
                                                                 Barometric Pressure, in._Hg
                                                                 Assumed Moisture, % 	t-4-
               Time ^',00- k'.op V-vw
                                Assumed Meter Temp., °F   (| Q
Operator
Sample Train Number
Meter Number _ 3.,
AH@
                                                                 Stack Gage Pressure   4- . Q 3>    "H2°
                                                                 Probe Tip Diameter, in. __
                                                                 Condensate Collected, ml. 	
                                                                 'C'  Correction Factor     ,Q
Point
i
7.
3
M
£
L












Total
Avg.
Time
Min.
26
to
•zo
20
20
10












IZO

Dry Gas Meter
Volume
ft3
Vm
ZS6 - QQO
-nA.u^o
2£>(. 000
"23=1.366
•2,1^7, 300
3^3,UOO
•2^^, 1 U,(D











^8,Z8O

Inlet
Temp.
oF
\2+
IH-6
14A.
|5~0
lM-0
1^-5












SH-1
IM-0
Outlet
Temp.
OF
^6=
IOP
lo?
10?
IIM-
m-












(t+2.
\CFl
Velocity
Head Ap
"H20
to.Ote
0,t)°l
6, 1 1
0, 12
(5,0?
0,<5^














Orifice AH
"H2°
1. 10
1.76
2,00
-i, Os
I.M-A
I,i40












°l.kS"
l,(«l
Pump
Vacuum
"Hg
L,,$
)4,o
IS.O
M'.S
IS.-0
1^, tf












S3,0
13,8
Filter
Temp.
op
—
—
-
—
—
—












—
—
Impinger
or
Condenser
Temp . , ° F
SA
ST.












3(^1
to
Stack Gas
Temp . , ° F
Ts
q.T
QC
*»<
^C
^r
^0












S^S"
PM>
Leakage Rate @  IS" "Hg =    fl.Q
cfm
                                                                 PEDCo- ENVIRONMENTAL
                                                                      SUITE 8  •  ATKINSON SQUARE
                                                                           CINCINNATI. OHIO  45246
                                                                                      513 / 77 1-4330

-------
                               PARTICULATE FIELD SAMPLING METER  DATA
Plant
ItAC
Run Number
Location
Date \
"IT. Time
   6-. F,
Operator _
Sample Train Number
Meter Number _ 3
AH@
                         - Ji.'o^'/l.
                                                                 Filter No.
                                                      Barometric Pressure,  in.  Hg
                                                      Assumed Moisture,  %      "3.S"
                                                                                                  . 2.
Assumed Meter Temp.,  °F
Stack Gage Pressure    -
                                                                                                -"H2°
                                                      Probe Tip Diameter,  in.
                                                      Condensate Collected, ml.  z. 6>, 6
                                                      'C1 Correction Factor    £>,°\ £>
Point
l
z
3
M-
r
la












Total
Avg.
Time
Min.
-20
•26
zo
Z-^0
ZO
ZO












IZL0

Dry Gas Meter
Volume
ft3
Vm
•3\Z,01 1
374, £30
331.^710
345. 4°f 0
3S9. ISO
3^.710
3H H. iD8^











^S,OI4-

Inlet
Temp.
oF '
fVS
0|ft
I02_
lOb
I5S
m^












&OZ
loo
Outlet
Temp.
oF
1°l
ft3
ea
^z
^3
^5*












530
fi8
Velocity
Head Ap
"H2°
o.oft
0,6k
0.6S"
fl,0^
o.oq-
6,0 3-














Orifice AH
"H20
1,30
^5,q-7
fl.T7
<^,-7T
6,^M-
tf,k>3












S-.OB
0,ft^"
Pump
Vacuum
"Hg
S
•+
«4
4-
3
3












23
4
Filter
Temp.
OF
—
—
—
—
—
—












—
—
Impinger
or
Condenser
Temp . , ° F
n&
TZ_
in
/*ft
fc^
6sft












^\^
(o^
Stack Gas
Temp . , ° F
T
1*50
Ife0
Ue3
1^0
iss-
ISS"












^Z3
ISU-
Leakage Rate @  15  "Hg =
                      cfm
                                                                 PEDCo-ENVIRONMENTAL
                                                                       SUITE 8 •  ATKINSON SQUARE
                                                                            CINCINNATI. OHIO 45246
                                                                                      513 IT7 1-433O

-------
                               PARTICULATE FIELD SAMPLING METER DATA
Plant
           IVAC
Run Number
Location  IN L.ET -
Date 2.-3Q--T2.  Time ST.oO- \V.Q6A-W\-
Operator      Pv.S ft .	
Sample Train  Number     3
Meter Number  	4-    	
AH@
       1.4-0
                       CPW\
                                                                 Filter No.,
                                                                 Barometric  Pressure, in. Hg
                                                                 Assumed Moisture,  %     l~3'/
                                                                 Probe Tip Diameter,  in.
                                                                 Assumed Meter  Temp.,  °F   tOO
                                                                 Stack Gage  Pressure 	O	
                                                                                                ."H2°
Condensate Collected,  ml.
"C1 Correction Factor
Point
1


z.


3


4-








Total
Avg.
Time
Min.
IS


\S *


IS"


\&








(*O

Dry Gas Meter
Volume
ft3
Vm
I2fo,u.6*0
rZS'.klO

\ttUlO
1-33JTO

133,110
138, "230

138,230
ms. n D







I(»,U?A

Inlet
Temp.
oF
&6
80

es
8R

90
^0

S65
°/U







TOB
S't
Outlet
Temp .
op
ft6
00

as
ft8

&B
A3

^8
^8







nofi
6=1
Velocity
Head Ap
"H2°
fl.lO
a* 10

0, 15"
0,|S"

6,17
5,n

6,1<5
/3,"Z-0









Orifice AH
"H2°
6,Z^
O.-Z-Co

6.14.0
O^Q

0,^-d>
(0,U^

S<\
201
Leakage Rate @  |S"Hg =   0.6^"    cfm
                                 TO
                                                                 PEDCo - ENVIRONMENTAL
                                                     /&  m,«
                                                                                      SI 3 IT7 1-433O

-------
                               PARTICULATE FIELD SAMPLING METER DATA
Plant
                                                                 Filter No.
Run Number
Location
                                                                 Barometric  Pressure,  in. Hg 3Q.Z.
                                                                 Assumed Moisture,  % 	L}-	
Date  -5-1--) 3-  Time  &'S~l- IP'S"!
Operator  L. ELFggs 4 3. 6-
Sample Train Number    2.
Meter Number 	2.
AH@
                                                                 Assumed Meter Temp.,  °F    | ( Q	
                                                                 Stack Gage  Pressure  -V- Q. flZ- "H2°
                                                                 Probe Tip Diameter, in.
                                                                 Condensate  Collected, ml.   3b.Q
                                                                 "C1 Correction Factor    O,
Point
1
2
3
4-
S
b












Total
Avg.
Time
Min.
20
ZO
20
ZO
T-0
£o












120

Dry Gas Meter
Volume
ft3
Vm
3>4.*t. 386
36>l. -260
3ia,8MO
3S5", 0^6
?fn. (s&Q
M-l 1.730
^^u,53o











ns~.\^o

Inlet
Temp.
OF
^^
US'
\\4
MS
l"ZC
IZ2












foH3
life
Outlet
Temp .
op
£fi
^&
Re>
^te
9&
°lb












5^n
^^
Velocity
Head Ap
"H2°
0.65"
^>,0(o
(?.03
6, OS"
<3,
6»A
-7^











M-M-0
(/3
Stack Gas
Temp . , ° F
Ts
°IO
aa
M
^16
^0
90
qo











6>T-7
^6
Leakage Rate @  I? "Hg =   Q, 0
                                 cfm
PEDCo-EN VI RON MENTAL
     SUITE  B  •  ATKINSON  SQUARE
          CINCINNATI. OHIO -4524C
                     513 /77 1-4330

-------
PEDCo- ENVIRONMENTAL
     SUITE 8  •  ATKINSON SQUARE
          CINCINNATI. OHIO  45246
                     513 /771-4330
                        COMBUSTION GAS ANALYSIS
               Plant
               Operator  /f
            Comments
               Location  &A#~fo»J    ft •• A ,
               Date
Test
No. Time
/ to: &>
I /o: 10
1 /o: \£





%(co2)
o





%(CO)
n

-------
          APPENDIX C




Standard Analytical Procedures

-------
                         ENVIRONMENTAL PROTECTION  AGENCY

                     Research Triangle Park,  North Carolina   27711

Reply to
 Atln of:                                                            -   n
                                           •  .            .      .     Date: 12-21-72
 Subject:   Summary of Fluoride Analysis        • ,                                   ,

   T*
    "'   R* Neul'icht,  EMB, IRL                                                   !
             This  memorandum is in response to your request for a brief
        summary of our SPADNS-Zirconium Lake procedure for determination
        of fluoride in stack emission samples.

             Samples received in our laboratory are filtered through
        fluoride free paper filters to yield water soluble and water insoluble
        portions.   The water insoluble particulate collected on the filter
        is rinsed throughly to be sure that all water soluble fluoride is
        rinsed through.   The water soluble fraction is distilled from sul-
        furic acid to a maximum temperature of 180 C.   If chloride is suspected
        in the sample Ag So  is added to the still. . SPADNS solution is added
        to an aliquot of the distillate and the absorbance is read at 570 nm.
        The concentration of the sample is determined from a calibration curve
        prepared from standard fluoride solutions.  It is very inroortant that
        the temperature of the samples be the same as that of the standards
        when absorbances are recorded.                 I

             The water insoluble fraction of the sample is evaporated to dry-
        ness in the presence or a siurry ox ^^0, cuiu Uien luo^J "wlLli IT^CII.  The
        fusate is  dissolved with distilled water, neutralized with dilute H So ,
        distilled and analyzed as described for the soluble portion.

             Paper filters containing particulate are cut into small pieces,
        suspended in a slurry of CAO, evaporated to dryness and ashed prior
        to the alkali fusion and distillation.

             If you have any questions about this procedure, let me know.
                                             Howard L. Crist
                                 Chief, Source Sample Analysis Section
                                              SSFAB, QAEML
        cc:   R.  E.  Lee

-------
          Phosphorus Pentoxide Determination



       Colorimetric Molybdovanadophosphate Method






     An aliquot of sample is hydrolyzed in the presence of



HC1 and HMO., acids by boiling almost to dryness.






     The sample is cooled to room temperature, transferred



to a 250 ml. volumetric flask and diluted to volume with



distilled water.  A 20 ml. aliquot is transferred to a 100 ml



volumetric flask, 20 ml. of molybdovanadate reagent is added



and the flask is diluted to volume.





     The absorbance of the yellow color is determined after



ten minutes at 400 nm.  The concentration of phosphorus



pentoxide is determined from a calibration curve prepared



with standard solutions.

-------
APPENDIX D




 Test Log

-------
     February 28, 1972



A.M.



9:00-10:00     At request of I.M.C. and C.F.  Industries all



               members of sampling team attended meeting to



               review safety rules at super phosphoric acid



               plant.  Attendees were PEDCo-Environmental:



               R. Gerstle, L. Elfers, R. Amick, J.  Geiger,



               G. Forte.  EPA: J. Rom.  I.M.C./C.F. Industries



               Bill Harwood, Bob Riddle, Bob Hearon, Richard



               Gonzales, Pat Peterson, J. Cox, Gene Lewis.






10:00-11:00    Plant is shutdown today for weekly cleanout.



               Therefore look over sampling sites and make



               requests for electrical outlets, sampling



               platform changes, etc. and make physical



               measurements of sites.





12:00          Leave plant.






     February 29, 1972



A.M.
7:50           Arrive at plant and begin set up.  Two trains



               on inlet-one on recycle tank and one on



               combined barometric seal tank and product



               storage tank.  One train on single outlet stack



               after scrubber.

-------
9:00           Make Pitot traverses at all sites.   Fumes very



               bad at all sites due to lack of wind.






10:00-10:30   .Make moisture runs at all three sites.  NOTE:



               Inlet train on recycle tank vent became coated



               with white material after only a few minutes,



               but still able to run for 30 minutes @ 0.3



               cfm.





11:30          Begin inlet run on barometric seal line.





11:45          Orsat



P.M.



12:00          Begin first test run on recycle tank vent.



               Stopped after four minutes to change from 3/8



               to 1/4" nozzle and change filter.  Filter had



               brownish color.





12:12          Begin outlet run.



               NOTE:  Process somewhat upset during this run



               due to hole in barometric condenser seal line.



               This was repaired at 1:00 and increased vacuum



               in evaporator.  Sampling train on recycle tank



               vent is emitting a white visible highly irritating



               fume - apparently a fluoride.  Impingers are



               heavily coated with white gelatinous material



               which has consumed most of the water in the



               train.  Glass in train is heavily etched.

-------
1:00           Scrubber inlet water sample  pH = 1.0,  Temp. 75°F.



               Bill Harwood getting product and feed samples.






1:15           Opacity <10%






1:30-2:15      Complete first series of tests.






2:15           I.M.C. started tests using their equipment.



               Their train on recycle tank vent also plugged



               up.   (This was the first time they had sampled



               inlet.)






2:30-4:00      Clean-up trains.   Inlet train on recycle tank



               is very difficult to clean and white material



               cannot be completely removed.  Use copious



               amounts of water  to wash out fluorides.  Silica



               gel bleached white.  Decide to make second run



               with this train over a one hour period (on



               fifteen minutes-off fifteen minutes) and use



               four straight tip impingers with 150cc, 150cc,



               50cc, and Occ of  water before filter and then



               silica gel impinger.  Use 1/4" nozzle for entire



               run.






4:00           Start run No. 2 at all locations.  This run



               routine except for plugging problems on inlet-



               recycle train. This train again completely



               coated with white precipitate and is not



               collecting all fluorides as evidenced by fume




               leaving train's meter.

-------
5:00           Take scrubber water, and product and feed



               samples.  Opacity = 10-20% somewhat heavier



               than this morning.






6:15           Complete test work and begin train cleanup.






7:30           Leave plant






     March 1, 1972



A.M.
7:45           Arrive at plant and begin setting up equipment.



               Notice that inlet ducts are puffing out gases,



               i.e. ducts are under slight positive pressure



               and flow is somewhat less than yesterday.



               Appears that scrubber is partially plugged up.





9:00           Begin sampling.  Use same set-up as second run



               yesterday.





9:15           Operator uncovers inlet plate to scrubber and



               pokes around inside venturi section to loosen



               cake buildup.  Uncovered duct for 3-5 minutes.



               This appeared to increase vent gas flows for a



               while.






9:18           Inlet train at recycle is plugged-washed out



               probe and nozzle.



10:00          Orsat

-------
10:30          Scrubber water and process samples taken.



               Scrubber outlet water temperature = 84°F






11:15          Complete sampling.  Inlet train on recycle line



               is again completely filled with white material



               and difficult to clean out.  Absorption



               efficiency of this type of train under these



               conditions of high F~*concentration is very



               questionable but is certainly well under 90%



               after the first 5 or ten minutes of sampling.



               In addition much of the precipitate in train



               cannot be removed.





11:15-1:00     Clean up trains and pack equipment.  Elfers



               in lab dividing samples: 1/2 to I MC 1/2 to



               EPA.






1:00           Leave plant and go to Farmland Industries.

-------
     APPENDIX E




Project Participants

-------
Project Participants

Richard W. Gerstle, P.E.
 Engineer in charge of sampling

Larry A. Elfers, Chemist

Robert S. Amick, Engineer

Gene Forte, Technician

Joseph Geiger, Technician


EPA

J. Rom - In, charge of sampling

J. Reynolds - In charge of process
 operations liaison

-------
  APPENDIX F




Recommendations

-------
Recommendations

            K\'•':•; .' "im-;:;^;        fc-f :•-:*•.•-?*•%.'*'-$
     The sampling train used during  these  tests  was  apparently

not capable of absorbing high concentrations  of  fluorides.

This was evident at the inlet sampling  site  from the recycle

tank line where visible emissions were  emitted from  the dry gas

meter and the silica  gel became very white jLn_cql_6r_ and/jwas	'

apparently affected by fluorides passing into this impinger.

We recommend a strong reducing agent such  as  sodium  arsenite

and/or a strong basic solution be used  in  the impingers whenever

high concentrations of fluorides and free  fluorine are suspected

In addition, more liquid should be used in the train and

sampling volumes should be decreased to avoid saturation.   As

used in these tests,  the collection  efficiency of the sampling

train is probably less than 95%.  Further  studies of sampling

fluorides in percentage quantities appear  necessary.

-------