TEST  NO.  72 - CI  -  18
                          ROYSTER  COMPANY
                 RUN  OF PILE TRIPLE SUPERPHOSPHATE
                         MULBERRY, FLORIDA

                   FEBRUARY 29  -  MARCH  1, 1972
                                                      .  n<:
2324 S. W.  34th STREET  /  GAINESVILLE, FLORIDA 32601 / PHONE 904/372-3318

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      TEST NO. 72 - CI - 18
         ROYSTER COMPANY
RUN OF PILE TRIPLE SUPERPHOSPHATE
        MULBERRY, FLORIDA

   FEBRUARY 29 - MARCH 1, 1972
       Test Conducted By:

 Environmental Engineering, Inc.

      Contract # 68-0.2-0232.  -

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                          TABLE OF CONTENTS

                                                                Page
List of Figures                                                 iii
List of Tables                                                  iii
Introduction                                                      1
Sumnary of Results                                                1
Process Description                                               8
Process Operation                                                 8
Location of Sampling Points                                       9
Sampling and Analytical Procedures                               14
Appendix
           A., Emission Calculations and Results
           B.  Field Data
           C.  Standard Analytical Procedures
           D.  Project Participants           •

                                 ii

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                          LIST OF FIGURES
                                                 Page
1.  Flow Diagram and Sampling Locations             3
2.  Port Location - Scrubber Inlet                10
3.  Port Location - Mixing Cone                   11
4.  Port Location - North Stack                   12
5.  Port Location - South Stack                   13
6.  Moisture Sampling Train                       17
7.  Fluoride Sampling Train                       18

                         LIST OF TABLES
1.  Summary of Results - Scrubber Inlet             4
2.  Summary of Results - Mixing Cone               5
3.  Summary of Results - North Stack               6
4.  Summary of Results - South Stack               7
                             lit

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INTRODUCTION
     Under the direction of the Environmental  Protection Agency,  Environmental
Engineering, Inc. conducted emission tests at the Royster Company Triple Super-
phosphate plant in Mulberry, Florida.  Three test runs were conducted  on
February 29- March 1, 1972.  The purpose of the tests was to obtain data for
the use of both the Industrial Studies Branch and the Performance Standards
Branch of the Environmental Protection Agency.

     Measurements for total fluorides were made at the scrubber inlet  duct and
at the two outlet stacks to the scrubber.  The emissions from the mixing cone
were also measured.  Grab samples of the scrubbing liquid, the process reactants,
and the process product were analyzed for fluoride and P205 content.  A schema-
tic flow diagram of all sampling locations is given in Figure 1.   Complete test
results are given in Appendix A.
SUMMARY'OF RESULTS
     All process and scrubber operating conditions were normal during  the three
test runs.  No major sampling problems were encountered; the only irregularity
occurred at the scrubber inlet duct.  Since entrained water was present at this
sample point, the percent stack gas moisture,was calculated using a psychrome-
tric chart.
     For the third test run both the percent stack gas moisture and the fluoride
concentration  for the North and the South outlet stacks are extremely low com-
pared to the other two test runs.  No explanation is available for this anomolyV

 v   A summary of stack gas conditions, fluoride emission levels, and  scrubber

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 efficiencies for each test run are given in Tables 1 - 4.
\

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   Stack Sample Location
Rock  Acid
  v
   cone
     V
 Curing Den
                              Pond Water
                                  V
 Scrubbers
                                                                To    Atmosphere
North
Stack

South
Stack
                                                                 t       t

                                                        	|
                                                   To Pond
Storage
                                         Figure 1
                                 Schematic Flow Diagram
                                     Royster Company

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                                   TABLE 1
                             SUMMARY OF RESULTS
                                  FLUORIDES

                               SCRUBBER INLET
Run No.
Date
Barometric pressure, inches Hg
Stack pressure, inches Hg
**
Stack gas moisture, % volume
Average stack gas temperature, °F.
Stack gas flow rate @ S.T.P.t SCFM
Vol. dry gas P 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 stk. cond.
Fluoride, total, gr/CF stk. cond.
Fluoride, water soluble, Ib/hour
Fluoride, total, Ib/hour
Fluoride, water soluble, Ib/ton P20r Fed.
Fluoride, total, Ib/ton PpCt Fed.
Scrubber efficiency, %
1
2/29/72
30
29.62
3.2
77
105575
65.408
1600
1600.36
0.3767
0.3768
0.323
0.323
340.8
340.9
21.8
21.8
—
2
2/29/72
30
29.62
2.9
75
95245
60.21
1800
1801.5
0,4604
0.4608
0.385
0.3853
375.8
376.1
23.5
23.5
— .
3
3/1/72
30
29.62
2.9
74
136147
114.133
2100
2101
0.2834
0.2835
0.2523
0.2524
330.7
330.8
20.0
20.0
—
**
Dry, 70°F., 29.92 inches Hg.

Saturated gas;  % moisture calculated from psychrometric chart

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                                TABLE  2

                          SUMMARY  OF RESULTS
                               FLUORIDES
                         MIXING CONE PICKUP
Run No. •
Date
Barometric pressure, inches Hg
Stack pressure, inches Hg
Stack gas moisture, % volume
Average stack gas temperature, °F.
Stack gas flow rate @ S.T.P., SCFM
Vol. dry gas @ 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 stk. cond.
Fluoride, total, gr/CF stk. cond.
Fluoride, water soluble, Ib/hour
Fluoride, total , Ib/hour
Fluoride, water soluble, Ib/ton P00r Fed.
£ 0
Fluoride, total, Ib/ton P205 Fed.
Scrubber efficiency, %
1
2/29/72
30,
30
0.1
90
246
51.169
46.8
405.8
0.0141
0.1221
0.0136 •
0.1178
0.0297
0.2579
0.0019
0.0165

2
2/29/72
30
30
1.5
90
239
48.482
61
408
0.0194
0.1296
0.0184
0.1233
0.0397
0.2654
0.0025
0.0166

3
3/1/72
30
30
2.2
80
292
61.457
11.1
778.1
0.0028
0.195
0.0027
0.1875
0.007
0.488
0.0004
0.0296

Dry, 70°F., 29.92 inches  Hg.

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                                TABLE   3

                          SUMMARY OF RESULTS
                               FLUORIDES

                            OUTLET NORTH
Run No.
Date
Barometric pressure, inches Hg
Stack pressure, inches Hg
Stack gas moisture, % volume
Average stack gas temperature, °F.
Stack gas flow rate G> S.T.P.* SCFM
Vol. dry gas @ 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 stk. cond.
Fluoride, total, gr/CF stk. cond.
Fluoride, water soluble, Ib/hour
Fluoride, total, Ib/hour '
Fluoride, water soluble, Ib/ton Pp05 Fed.
Fluoride, total, Ib/ton P,>05 Fed.
Scrubber efficiency, %
V
1
2/29/72
30
30
3
88
64741
95.346
34.4
34.46
0.0056
0.0056
0.0052
0.0052
3.08
3.09
0.197
0.198
98.5
2
2/29/72
30
30
2.8
89
65060
96.426
24.8
24.8
0.004
0.004
0.0037
0.0037
2.21
2.21
0.14
0.14
99.0
3
3/1/72
30
30
0.4
86
63591
94.688
6
6
0.001
0.001
0.0009
0.0009
0.53
0.53
0.03
0.03
99.8
Dry, 70°F., 29.92 inches  Hg.

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                                TABLE  4
                          SUMMARY OF RESULTS
                               FLUORIDES

                             OUTLET  SOUTH
Run No.
Date
Barometric pressure, inches Hg
Stack pressure, inches Hg
Stack gas moisture, % volume
Average stack gas temperature, °F.
Stack gas flow rate @ S.T.P.* SCFM
Vol. dry gas @ 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 stk. cond.
Fluoride, total, gr/CF stk. cond.
Fluoride, water soluble, Ib/hour
Fluoride, total, Ib/hour
Fluoride, water soluble, Ib/ton P^Og Fed.
Fluoride, total , Ib/ton P205 Fed.
Scrubber efficiency, %
1
2/29/72
30
29.91
2.9
89
42317
71.375
24.5
24.59
0.0053
0.0053
0.005
0.005
1.9
1.9
0.12
0.12
—
2
2/29/72
30
29.91
3.1
90
40952
66.89
17.8
17.8
0.0041
0.0041
0.0038
0.0038
1.4
1.4
0.09
0.09

3
3/1/72
30
29.91
-0.2
87
43090
68.094
0.52
0.52
0.0001
0.0001
0.0001
0.0001
0.04
0.04
0.003
0.003
—
Dry, 70°F., 29.92 inches Hg.

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Process Description
     ROP triple superphosphate is  made by reacting 32-34 percent
PpOg rock with phosphoric acid in  a TVA cone-type continuous  mixer
to yield a product containing 46%  P205.  Tne principal  reaction
is as follows:
     Ca3(P04)2 + 4 H  P04 + 3H20 —->• 3 Ca H4 (P04)2°H20
     The cone discharges to a slowly moving belt called the "den"
on which the reactions continue until the slurry solidifies and is
discharged to the storage pile. The reactions go to near completion
in the pile where after sufficient curing the product is ready for
shipment.
Process Operation
     Run #1 was conducted from 12:40 p.m. to 3:20 p.m.  on
February 29, 1972.  The second test was completed at 7:04 p.m. the
same day.  Run #3 was carried out  from 9:08 a.m. to 11:12 a.m. on
March 1.  Process and scrubber conditions were normal throughout
the three tests.
                                    8

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    LOCATION OF SAMPLING POINTS

          The sampling sites and number of traverse points  were
selected as per "Method I - Sample and Velocity Traverses  for Sta-
tionary Sources, Part 60, Subchapter C, Chapter 1,  Title 40," Federal
Register. No. 247-Pt. II-l.
          The above method suggests using two perpendicular diameters
of traverse points per sampling station, however,  on-site  conditions
necessitated the use of only one traverse diameter in some cases.   The
suggested number of traverse points per diameter was used  where possible
without sampling within one inch of the inner wall.
           Figures 2 through 5 are schematic diagrams of the stack con-
figurations near the sampling location, and the sampling points traversed
during the emission tests.

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          LET
TRAVERSE:
POHMT NQ
i
2
3
4-
5"
G
7
8
9
10
ii
12.
13
!4-
15
1G
17
l&
DISTANCE"
FROM PORT
( INCHES)
( 5/3Z
3 25/32.
G 7/IG
9 3/Q
12- 9/1G
IG 5/3Z
^0 5"/l6
2.5 15/32
3 2- 27/3 2.
S3 5132.
GO 9/16
65^ 23/32
G9 27/3Z
"73 7/IG
76 sye
79 9/16
62 7/32.
84- I3/I€»
n
     86" I.D
FIGURE 2



  10
A-A'

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1X1NG   CONE  PICK-UP
                        TRAVERSE:
                         POINT NO.
                            i
                            Z
                            <3
                            4-
Di STANCE
FROM PORT
 ( INCHES)
   1/4
   f 3/4"
   4 1/8"
   5"
       6» '
                          Not sampled - too close
                         'to stack wall
            A'-A'
              FIGURE 3
                11

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                          OUTLET    NORTH
A'
A'
             60'
   \

TRAVERSE
POINT NCX
t*
2
3
4-
iD
G
7
8
9
IO
ii
12.
13
14-
15
16
DISTAIMCE"
i=RGiVl PORT
CINCHES)
I 5/3Z
3 17/32
G 1/8
9
12. 5T/3Z
15" 2T/3Z
20 3/&
2T
4-5
Si 5V©
5& 5-/3Z.
F9 27/32
Gl 1/2.
OS 7/8
Ge I5/3Z
~10 2.7/32.
                            Not sampled
                                 PORT 2.
                   7Z" I.Q
 BLOWER
                                               PORT
                                  A'- Ax
               FIGURE 4
                 12

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                         OUTLET _  SOUTH
        A'
A'
                   CO'
              N
\
TRAVERSE
POINT NO
*
I
2,
3
4-
5"
G
7
8
9
»O
11
12.
13
11-
IG
DISTANCE-
FP\OM PORT
I 6V3Z
3 I7/3Z
G t/8
9
1 2. 573Z
IS" 27/3Z
ZO 3/&
27
4-S
s"t 4>ve
5G 573Z
5*9 Z7/32
Gl I/2.
C>5 7/8
TO 27 /3Z
                              Not sampled
                                  PORT 2.
                       7Z" J.D.
                 BLOWER
                             PORT i
                    FIGURE 5
                      13
                                   A-A"

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SAMPLING AND ANALYTICAL PROCEDURES

A.  Preliminary Moisture Determination
           The preliminary moisture content of the stack gases at each
sampling site was determined by Method 4 of the Federal Register
(Volume 36, Number 247, Part II, December 23, 1971).
           The only significant difference between F.R. Method 4 and
the method used was the configuration of the sampling train (see
Figure 6 ).-  The sampling train used in these tests consisted of the
first two midget impingers with 5 grams of distilled-deionized water
followed by two dry midget impingers in place of a silica gel  cartridge.
           At sampling sites where liquid entrainment was a problem, the
preliminary and final moisture contents were determined from wet and
dry bulb thermometry.  See Appendix B  for the data used in determining
the preliminary moisture content of the stack gases.
           After completing the moisture run, the total impinger liquid
plus water rinsings of the probe tip thorough the fourth impinger were
placed in an 8 ounce polyethylene container.  The samples were held by
EPA personnel for further analyses.

B.  Preliminary Velocity Determination
           Method 2 of the above mentioned Federal Register was used as
a guide in determining the preliminary stack gas velocity for each source
tested.  The major difference was that only the maximum and minimum
 *
   Scrubber Inlet
                                  14

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velocity heads across each stack area were determined so that a proper
nozzle size could be selected.   During each of the three fluoride
emission tests, velocity head readings were taken at points selected
by using Method 1 of the Federal Register.
           Stack pressure and temperature measurements were also made
during the preliminary velocity determinations.

C.  Sampling for Fluoride Emissions
           The sampling procedure used for determining fluoride emissions
was similar to Method 5 of the Federal Register.  The major difference
between the two methods was the configuration of the sampling train.
The sampling train described in the Federal Register has a heated box
containing the filter holder directly following the glass probe.  The
sampling train used in these tests contained no heated box and the filter
holder was placed between the third and fourth impingers (between dry
impinger and silica gel impinger) to  prevent sample carry-over.  Figure   '..
7 is a schematic diagram of the sampling  train used.
           After the selection of the sampling site and the minimum number
of sampling points per Method 2 of the above mentioned Federal Register,
three separate test runs were performed.  For each run, the required
stack and sampling parameters were recorded on field data sheets.  They
are .included in Appendix  B.  Readings were taken at each traverse point
at least every five minutes, and when significant changes in stack para-
meters necessitated additional adjustments to maintain an isokinetic flow
rate.  Nomographs were used to aid in the rapid adjustment of the sampling
                                  15

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  rate.  The traverse points were selected to maintain at least one inch
  from the inner stack wall.                                    .
             After each run, the liquid volume in the first three impingers
  was measured volumetrically and the silica gel was reweighed.  The im-
  pinger liquid, the filter, plus the water washings of the probe and other
  sampling train components up to the silica gel were placed into poly-
  ethylene containers.
   D.   Liquid  and  Product  Grab Samples
              Periodically,  during each  test  run,  grab samples  of the raw
   materials,  finished  product, and  scrubber  liquid  were  taken, and  the
   temperature  and  pH were determined at the  site.   On some  occasions,
   the  samples  were split  with the plant personnel so that comparative
   analyses could  be  performed.

   E.   Laboratory Analysis Procedures
              Water soluble  fluorides were  done  by a sulfuric acid distilla-
   tion followed by the  SPADNS-ZIRCONIUM LAKE METHOD.  Water insoluble
   fluorides were first  fused with NaOH  followed by  a sulfuric  acid  distilla-
   tion then by the SPADNS-ZIRCONIUM LAKE METHOD.
              ?2^>^  analysis  of the stack effluent  was done by EPA personnel.
   All  other PpOj.  analyses were done by  plant personnel.
              For more details of exact  method used, see  Appendix C.
\
                                    16

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  1.   Heated Glass Probe
  2.   Glass Connector
  3.   Ice Bath
  4.   Midget Impinger With
  5.   Midget Impinger With
  6.   Midget Impinger,  Dry
  7.   Midget Impinger,  Dry
  3.   Flexible Sample Line
  9.   Vacuum Gauge
 10.   Main Control  Valve
_!!.   By-Pass Control  Valve
!12.   Air Tight Vacuum  Pump
 13.   Dry Test Meter
.14.   Thermometer
 15. '  Calibrated Orifice
 16.   Inclined Manometer
 17.   S-Type Pitot Tube
                                                        Figure ''6

                                                 MOISTURE SAMPLING TRAIN

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 1.
 2.
 3.
 4.
 5.
 6.
 7.
 8.
 9.
10.
11.
12.
 s.
16.
17.
18.
19.
Stainless Steel Nozzle
Heated Glass Probe
Glass Connector
Irnpinger,with 100 ml' H»0 (Modified Tip)
Irnpinger with 100 ml H^O (Standard Tip)
Impinger, Dry (Modified Tip)    '
Impinger with 180 grams Silica Gel (Modified Tip)
Filter Holder with No. 1 Whatman Filter
Flexible Sample Line
vacuum Gauge
Main Control Valve
By-Pass Control Valve
Air Tight Vacuum Pump
Dry Test Meter
Calibrated Orifice
Inclined

           nometer
S-Type Pi tot Tube

3




=a$%
10
T"
;»U.
i|U-
•a
ciM' (\W

1


1 1
j i
| (
:i

T" '

, '
i *


- 1
i !
i
i
»
S!
i '-T •-
i! tl-
J ^
• 7
8
— ^
-/-]


;!
i »•
i "'I
._]
                                                                                                           11
                                                                <~ntj>*—'
13
O
-^M-
IXM
©
I n
it
                                                        Figure 7

                                                  FLUORIDE SAMPLING TRAIN

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APPENDIX

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          APPENDIX  A
Emission Calculations  & Results

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              E.E.I. SOURCE SAMPLING NOMENCLATURE SHEET
  PB - Barometric pressure, inches Hg
  PS - Stack pressure, inches Hg
  As - Stack area, sq. ft.
  AS'- Effective area of positive stack gas flow, sq. ft.
NPTS - Number of traverse points where the pitot velocity head was greater than zei
  TS - Stack temperature, °R
  TM - Meter temperature, °R
  II  - Average square root of velocity head, Vinches
.  AJH - 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 impringers, milliliters
  Po - Pressure at the dry test meter orifice, [PB +A H~) inches Hg
                                               L   -13.6J
 STP - Standard conditions, dry, 70°F, 29.92 inches Hg
       Conversion of condensate in milliliters to water vapor in cubic feet (STP)
       Volume sampled, cubic feet (STP)
       Total water vapor volume and dry gas volume sampled, cubic feet (STP)
       Moisture fraction of stack gas              -
       Dry gas fraction
       Molecular weight of stack gas, Ibs/lb-mole (dry conditions)
       Molecular weight of stack gas, Ibs/lb-mole (stack conditions)
       Specific gravity of stack gas, referred to.air
       Excess air, %
       Average square root of velocity head times stack temperature
       Stack gas velocity, feet per minute
       Stack gas flow rate, cubic feet per minute (stack conditions)
       Stack gas flow rate, cubic feet per minute (dry conditions)
       Stack gas flow rate, cubic feet per minute (STP)
       Percent isokinetic volume sampled (method described in Federal Register)
       Total Sample Time (minutes)                             "

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                  EQUATIONS FOR CALCULATING FLUORIDE EMISSIONS





       VWV = (0.0474) x (VC)


     VSTPD = (17.71 x (VM) x  (PB +  AIL.  )-^ TM
                                    13.6

        VT = (VWV) + (VSTPD)


         W = (VWV)-j-(VT)


       FDA = (1.0) - (W)                                   ,


    FMOIST = Assumed moisture fraction


        MD = (0.44 x % C0£) + (0.32 x %  02)  + (0.28 x % N2)  + (0.28 x % CO)


        MS = (MD x FDA) +  (18 x W)


        GS = (MS)-j- (28.99)


    .    EA = [(100) x (% 02 - ^j^-i-fjo. 266.x % NZ) - (% 02 - %.,CO) ~]


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


;        QS = (u) x (AS)


        QD = (QS) x  (FDA)


     QSTPD = (QD) x  (  53°) x (i8-)
                     29.92     TS


      PISO =   (o.oo267 x VC x TS) + (PQ  x TS x VM-^-TM)  -~   (Time x 2 x  PS  x



    Fluoride Emissions:          -


           MG = Milligrams of fluoride from  lab  analysis


           Grains/SCF = (0.01543) x (MG)~ VSTPD


           Grains/CF,  Stack Cond.  = (17.71) x (PS)  x (FDA)  x (Grains/SCF) -7- (TS)


           Lbs/hour = (Grains/SCF)  x (0.00857) x (QSTPD),


\         P2°5 Fed = Tons/hour, determined  from plant  data


           Lbs/ton P205  Fed =  (Ibs/hour)  -^ (Tons/hour ,P2°5 Fed)

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FLUORIDE EMISSIONS

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                            r-n nr> n n  71 P <-' c1  n / 

i 28.J50 1 °-98 10 815 1 77 J_ 1 8 W8 8 Q 10 83 J. 29 . G2 1 2767.1 J_ 40. 34 J_ 40.34 1 105575 .J_ 126 J_ 0.25 1 58.3 j_TSlfd".TG J_ 0.37 67- J_ 0 . 3 7 G 8 \TrM- — - | 34078 |~3?() . 9' i -L _ i"^T 55 — ^X . o 1 2 1 __3.._ _ 1 1 2Z22./.7-0 1 2L/JL/_7_2_ 1 I_lli-S.a L OJLi-SJi 1 1_30 _ _ i__30 1 1 G 2 _Za.R 1 115 ^3_2 5 1 1 R ^ «.4 1 7 1_ 2 | l_§.Q.t.21. 1_ 114 J.3_3 _J 1-10^37 1 _JULJ7JL J J. 10 J. 2_^9 j i _„_ i __ ^ 1 1 1 1 1 1 j 1 ° 1 ° j[ 2 8 . 8 5 _[ 2 3_, 8 5 l^j>.5_4_ 1 _2£L54 ll'j.iS- 1 JL32 10.732 1 0.031 J_ 7 4 . 8 _[ 7 4 _! ' 1 G . 9 2 0 J_ 19.207 J_ 0 . 8 3 . J_ 0 . t; 3 J_29.G2 _| 29. G 2 1 24_7_8_,5_ i _1532^5_ J_ 40 . 34 _]_ 40.34 J_ 40 . 34 J_ 4~0 .34 J. 95245 1 _13.614_7_ J_ 12G J_ 120 J_0.25 ^"D."2b _[59.5 J_ 78.9 \-rmn~-5 — -]-2T^— — j^ti ."4 b 0 4 . j^ "O.^IJ^ |1T."I|-T)"015 j_ u.^Tl'S1? i "0 ."5 u~B~3 i "0 . "2'5"2"TT _[375.8 _[ 330.7 J_376.1 J_ 330. a 1 1 _[23.5 Ji 20.0 J[23.5 J[ 20.0 - **$S .P.*~>-DRY, 70 DEGREES F, 29.92 INCHES MERCURY*** Saturated gas; % moisture figured from psychrometric chart, not from volume of water collected.


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                           IQURCE  TEST VATA
    TEST  no  -
    PLANT -  ROYSTER POP
    SOURCE - MIXING CONE
    TYPE  OF  PLANT -
    COUTROL  EQUIPMENT -
    POLLUTANTS SAMPLED -
               NO ' OF
   BARTOW,  FLA.
PICKUP
RUNS -
1)RUN NUMBER
2) DATE
3) TIME BEGAN
UPTIME- END
^BAROMETRIC PRESSURE, IN HG
S)METER ORIFICE PRESSURE DROP, IK H20
1)VOL DRY GAS, METER COND, CUBIC FEET
8) AVER AGE GAS METER TEMPERATURE, DEG F
9) VOL DRY GAS, S.T.P. , CUBIC FEET
- 10) TOTAL 1110 COLLECTED, ML
11)VOL U20 VAPOR COLLECTED, S.T.P. , CU FL
12)STACK GAS MOISTURE, PERCENT VOLUME
13)ASSUMED STACK GAS MOISTURE, PCT VOL
1H)PERCENT C02 .
1S)PERCENT 02
16) PERCENT CO
17) PER CENT N2 '
1B)PERCENT EXCESS AIR
13)MOLECULAR WEIGHT OF STACK GAS, DRY
2Q)MOLECULAR WEIGHT OF STACK GAS, STK CON!
2DSTACK GAS SPECIFIC GRAVITY •
22)AVG SQUARE ROOT (VEL HEAD), IN U20
23)AVERAGE STACK GAS TEMPERATURE , DEG F -
2H)AVG SQUARE ROOT (STK TEMP*VEL HEAD)
2 5) PI TOT CORRECTION FACTOR
2b)STACK PRESSURE, IN HG, ABSOLUTE
27)5 TA CK GAS VEL , STA CK COND, F.P.M.
28)STACK AREA, SQ FEET
23)EFFECTIVE STACK AREA, SQUARE FEET
30)STA CK GAS FLOW RA TE , S.T.P. , S CFMD
31) NET TIME OF TEST, MINUTES
32)SA!-!PLING NOZZLE DIAMETER, INCHES
33) PERCENT ISOKINETIC
3H)FLUORIDE - WATER SOLUBLE, MG
3S)FLUORIDE - TOTAL, . MG
3&) FLUOR IDE - WATER SOLUBLE, GR/SCF
37)FLUORIDE - TOTAL, GR/SCF
3B)FLUORIDE - WATER SOL., GR/CF, STK CUD.
3<3)FLUORIDE - TOTAL, CR/CF, STK CND.
HO)FLUORIDE - WATER SOLUBLE, .LB/UOUR
HDFLUORIDE - TOTAL, LB/UOUR

H3)FLUORIDE - WATER SOL., LB /TON P20l> FED
HH)FLUORIDE - TOTAL, LB/TON P20b FED
i _ i .
L-ZLZZLl
I 15i.l2.
i 30
J_ 0^5
J. 52 177
i 82^6
J_ 5 1 ,JL 6 9
1 0. 6
M 0.03
1 O*-1
i 2
i
1
i 	
i

| 28.85
; 1 28.84
J_ 0. 99
J_ 0. 4
1 90
]_ 9. 373
_! 0.83.
J_ 30
1 1355.3
J_ 0. 19
(0.19
1 246
1 12°
J_ 0.~25
I ~9~5~. G
["^TT.I]
|Troir."^
jl"D~."DlTiT
iTT.T2^"l
'\ tf~. W ^
|"U~.T1TB"
i TT."D"2T; /
i T) ,T5 yTi
i ^1T1.

it) .THIS ^
1 _a 	
•2— J-J/-2.9-A7.3.-
1 -> 8- • U-0-
1 ^a
i a U.K
_L !l° f'1 3.
1 a.6._6 	
1 U.8. US.2.
1 1 5. 5.
1 Q. T-^
1 1 5.
1 2. —
__ 1 _- _ _
_[
1 _
J
1 o_ 	
i ™28r_.Ji.Ii-
1 _2.8_ QJL
1 0_^_9_
1 Q.J2J' "•
J. 9_Q_
1 9 1 1 'i
1 0 «JL3
1 _3_0__ _ _
J. 1 3 2 1 U
1 0.19
1 Q_,- 1 9
J_ 239
1 12°
J_ 0.25
1 94.2
1 61
1 ^ ° 8
J_ 0.01 94
_[ 0 . 1 2 9 G
J_ 0. 018.4
J_ 0.1233
J_ 0 . 0397
J_ 0 . 2G.54
_[
J_ 0.0025
J_ 0 . 0 1 6 G
1 ^ 	 .

L Ul • OJL
1 _an. 	

i 6,1 it°u
1 71^,7
1 61 iiRj
1 2 9 u
1 -L.J59
I 2 °
1 -2 _

1 _
1 _ _
1
1 _c _
1 2 8_, 8 5
_[ 23_, 51
1 0_, 9 n
1 0_,U73
J. 80
J_ 1 1^ 0 0 3
1 °_i 83
1 30
J_ 1597. I.L
1 o.1^
J_ 0.19
_[ 292
1 12°
J_ 0 . 2 5
1 "7 • 7
_[ 11.1
J_ 7 7 8 . 1
J_ 0.0028
_[ 0.1 0 5
J 0.002 7
1 . -L <• -' -^
j_ 0 . 0 0 7
j_ o./ion
j_
i 0.000';.
J_ 0" . 0 2 D R

-









































***S.r.P.4~*Dliy,  70 DEGREES F,  29.92  INCHES MERCURY***

-------
                              SOURCE TEST DATA
      TEST NO -                               HO OF  RUUS  -
      PLANT - ROYSTER ROP    ' BART Oil,  FLA,
      SOURCE - OUTLET NORTH
      TYPE OF PLM1T -                         .
      C011TROL EQUIPMENT  -
      POLLUTANTS  SAMPLED -
  DltUil  NUMBER        .                          1	.1	L	.2	1	1	1
  2) DATE                      . •'                 l__2/2a/2.2.-.l	2/,2.2./.7_Z_l	iZ.LZ.L2.	1
  3)TIME BEGAi;            '             '         i	12-^U.Q.	L	lli-Hil.	1	Q-L-Q-Q	1
  H)TIME El-ID           .                          1	I£i2a_	L	laiO-ii.-	L_1.1.LL2_	[
  ^BAROMETRIC PRESSURE,  III HG                i	2Q	1	ad	1	3.0.	J.
  &)METER ORIFICE PRESSURE DROP,  III H2°      1	2.^0.2.	1	2,^.0.2.	i	Li_lQ	1
  1)VOL  DRY CAS, METER COI1D, CUBIC FEET     J.	2.2. ,1.2.3.	1	^2.^15.0.	L	i.!i_51JL	1
  K) AVERAGE GAS METER TEMPERATURE, DEC F    J.	a5...5.	i__9Q.^9	1__?JLJL	1
  <3)VOL  DRY GAS, S.T.P.  ,  CUBIC FEET         J.	a5.^au.a	1	2.6.JL2JL	i	!1-JL.8JL	1
 10)TOTAL U20  COLLECTED,  l',L                   J.	Q.ZU-.	I	5.8...S.	J.__'L-JL_	1
 11) VOL  H20 VAPOR COLLECTED, S.T.P.  ,  CU FTJ.	2__ai_	1	2.JLL	J.	°--J^L	1
'•12)STACK GAS  MOISTURE,  PERCENT VOLUME      J.__a	J.	2_,_Q.__	J.	O.J|	J.
 13)ASSUf!SD STACK GAS MOISTURE,  PCT  VOL     J.	£._fl	1	2.JJ.	i__2_._5	i
 !H)PERCEiJT C02                                 1	1	.	1	.	1
 1S)PVRCEI}T 02                                  1	L	1	1
 lb)PERCE!JT CO                                  1	1	1	1
 IDPEHCEUT N2                                  1	_.	1	1             '
 1Q)PERCEHT EXCESS  AIR                         i	0.	1	Q.	1
 1S)MOLEC'ULAR  HEIGHT OF  STACK GAS, DRY      1	2_8._8JL	J.__?JL_QJL-	1__2_8_-JLL	i
 2Q)MOLECULAR  WEIGHT OF  STACK GAS, STK COI!L\[	2_8._5.3.	J.__2_8AJ5JL	l__2JL--°J-_	i
 2DSTACK GAS  SPECIFIC GRAVITY                1	Q.^.98.	1	Q_JH3_	1__°_'_9JL_.	1
 22)AVG  SQUARE ROOT (VEL HEAD),  III H20      1	Q.^.TJLS.	1	Q--_7J_8_	i__°_-_C_°_9_	J
 23)AVb'KAGE STACK GAS TEMPERATURE,  DEG F    1__8_8_	JLJL8_-_7_	l_JLG_-_2	__.i
 2H)AVG  SQUARE ROOT (STK TEMP*VEL HEAD)     l^JLSLJJL	l.-AJLJl2..	l_J_LrJHL__J
 2S)PITO? CORRECTION FACTOR                   JL.JLJL3.	J._JL-JL3-.	1__0_-JSJ	J
 2&)STACK PRESSURE,  III HG , ABSOLUTE          1__3P	1__3_°	1__3_°__:	
 27)STAOK GAS  VEL,  STACK COI.'D,  F.P.lf.        1 JLl3-4	1 JJLHJL'J	l__2_3_2^_-_2	
 28)STACZ AREA, SQ  FEET        .  '    .          1__2JL-_2J_	l__2JL-_2_7_	1_^2_8JJ;J	
 2V)EPFECTIVE  STACK AREA,  SQUARE FEET       1__2JL-JL7_	1__2JL'_2_7_	1
 3Q)STACK GAS  FLOW  RATE,  S.T.P.  , SCFMD     L___5_!t7JL1	1__GA.0_G_°_	1
 31)NET  TIME OF TEST, MIIU1TES        .        l_J-_2_°	1_J_2_0	•^—rr-^r	
 32)SAt-:PLi;iG KOZZLE DIAMETER, III CUES         l__°_-_2_5__	!__?•"_	-i--?-A-^-	
 33)PERCENT ISOKIUETIC                         l-J-JL1---8	J-^-r-J	__!_.;„-:-	
_!,
   )FLUORIDE  -  WATER SOLUBLE,  MG             1__3J_'JL	__i_ ^HJ b	I."0"
 35) FLUORIDE  - TOTAL,           MG   .          l_jll:_.L	1_4-*TT	J—TV-TTI	
 36)FLUORIDil. - WATER'SOLUBLEt  GR/SCF        i.JL'-0-0-5.0-	l_ij^.?_	l_^_l^i«___.
 3'DFLUOiUDE  - TOTAL,           GR/SCF        i_£
 3i\)FLUORIDE  - WATER SOL.,  GR/CF, STK CUD.  i__°.
 3Q)FLUORIDE  - TOTAL,       GR/CF, STK CUD.  1_ °.
 ilO)FLUOHIDZ  - WATER SOLUBLE,  LB/UOUR       i.^J^^	1_.
 H1)FLUORIDE  - TOTAL,        .   LB/UOUR       1_"3.
 H3)FLUORIDE  -  WATER SOL.,  LB/TOil P20l>
 '4 M ) FL UORI i)E  -  TOTA L ,        LB / TO// P2 0 5
     '.T.P.++DRY,  70  DEGREES F,  29.92  IVCUES MERCURY***

-------
                          SOURCE TEXT
     TEST 110  -
     PLANT -  ROYSTER ROP
     SOURCE - OUTLET SOUTH
     TYPE OF  PLANT  -
     CONTROL  EQUIPMENT -
     POLLUTANTS SAMPLED -
            no OF nutfo
x -
BARTOWt FLA.
DRUil NUMBER
2) DATE
3) TIME BEGAN
UPTIME END , . -
^BAROMETRIC PRESSURE, 177 HG
§)METER ORIFICE PRESSURE DROP, IN H20
7) VOL DRY CAS, METER COUD, CUBIC FEET
B) AVER AGE GAS METER TEMPERATURE, DEC F
• 9) VOL DRY GAS, S.T.P. , CUBIC FEET
lO) TOTAL 1110 COLLECTED, ML
1D1/OL L'20 VAPOR COLLECTED, S.T.P. , CU
12)STACK GAS MOISTURE, PERCENT VOLUME
13) ASS mi ED STACK GAS MOISTURE, PCT VOL
mn-ERCENT CO 2
- \5) PERCENT 02 . .
1C )PERCENT CO
1 7 )PER CE'l T 111
1B)PL'XCEUT EXCESS AIR
\$)MOLECULAR WEIGHT OF STACK GAS, DRY
2Q)MOLECULAR WEIGHT OF STACK GAS, STK CO
21) STACK GAS SPECIFIC GRAVITY
22)AVG SQUARE ROOT (VEL HEAD), III H20
23) AVER AGE STACK GAS TEMPERATURE, DEG F
•2^)AVG SQUARE ROOT (STK TE'dpy-VEL HEAD)
2 b) PI TOT CORRECTION FACTOR ,
2^) STACK PRESSURE, IN JIG, ABSOLUTE
2DSTACK GAS VEL, STACK COUD, F.P.M.
.28)STACK AREA, SQ FEET .
23)EFFECTIVE STACK AREA, SQUARE FEET
30) STAC K GAS FLOW RATE,, S.T.P. , SCFMD
3l)i1ET TIME OF TEST, MINUTES
32)SAi-:PLIl]G NOZZLE DIAMETER, INCHES •
33) PER C EH T ISOKIUETIC
3 4 ) FL UORIDE - WA TER SOLUBLE , I-1G
3 5 ) FL UORI D E - TO TAL, MG
3&)FLUORIDE - WATER SOLUBLE, GR/SGF
3rJ)FLUORIDE - TOTAL, . GR/SCF
3Q)FLUORIDE - WATER SOL., GR/CF, STK CUD
31)FLUORIDE - TOTAL, GR/CF, STK CUD
HO)FLUOHIDE - WATER SOLUBLE, LB/HOUR
m)FLUORIDE - TOTAL, LB/HOUR

H3)FLUORIDE -WATER SOL., LB/TON P2(7I> FE
H^)FLUORIDE - TOTAL, LB/TON P205 FE
i !„ 1 _2 	 1_ 3. „_ i

1 !9'iiH 1 1£ • r£ i ° • Q.Q. 1
i 1i'2fi. 1 1^'J2JQ • 1 •LL--L2. •
i 30 - J. 30 1 3JL !
1 Q.,.9 1 1 u^^^ 1 a a.0. 1
1 7 3^4 Q.9 1 69^.122. 1 G.8. 5.GJL 1
|863 ip9L|- • 1 "Lu 3_ ' '
171375 J.66£° lrs_ 014 '
i '^5*.5 1 45 1 2. 3. '
FT\ 216 J. 2*.12. 1 G-^JLL J.
log J. .3. -1 1 d^P i
12,_9 129 1 ° 2. !
1 _ 1 _ 1 _ 1
1 1 ___ __ 1 _ _ 1
1 1 _ _ 1 _ !
1 „ J. 	 _1 :
lo lo 1 o_ i
1 28,_85 _ 1 28 ^85, 1 28 ^ J
77ZJ1 28.53 1 28.51 J.28 OJL J
10.98 10.98 1 Q_^_9_9
J_ 0 . 4 6 8 1 0 . H 5 4 1 O^J-h o_5
j_ 8-8 . 7 J_ 89 ^5 1 80 5
J_10.9G8 1 10. 6H5 110,879
10.83 10.83 1 0_, 8 3
J_29.91 1 2 9 ^9 1 1 2 9_, 9 1
I-ICQP. O l"1s^n Q 1 *1 C *7 1 • "7
| JL O r? O ^ J 1 .u O O v* « O i J_ D / H- . /
J_ 28. 27 _[ 28.27 128.27
J_ 2 8 . 2 7 J[28.27 128.27
142317 140952 143090
1 120 J_ 120 1120
|0.25 . J_0.25 10.25
j_116.G _[112.9 1109.2
1 24 . 5 j_ 1 7 . 8 1 0 .~52
j^ 24. 59 j_ 17 . 8 _[ 0. 52
j^l) ,~0~b~5 3 J_ 0 . 0 0 4 1 10.0001
i"D.0053 J| 0.0041 _[0."0001
J[~0.005 . J_ 0.0.0 3 Pi _[ 0.0 001
j^T).T)l)5 J_ 0.00 30 _[0."0001


1 1 1 -
p i "D .l"2^Ti i 0.. 0 8 9 9 J_ 0 . 0 0 2 G
D l"0."^"2"5^ jTT.trBgg _[0.002G
***S.'f.P.*~+DXy,  70 DEGREES  F,  29.92 INCHES  VERCUR Y* +

-------
                            SCRUBBER EFFICIENCY
\

-------
                                                                                           107058
                                                                                           4.99
                  Scrubber
                    Inlet
Flow: 105575(DSCFM)
Fluorides: 340«9 (#/hr)
                                     From  Pond
Scrubber
                                     Efficiency:98.5%
                                                     y

                                                  To Pond
                                                                            64741
                                                                            3.09
                                                                                             To

                                                                                        Atmosphere
                                                                                  North
                                                                                  Stack
                                                                42317
                                                                1.9
                                                           South
                                                           Stack
                                                            Royster Company
                                                        Triple Super Phosphate
                                                                Run 1

-------
                  Scrubber
                    Inlet
Flow: 95245 (DSCFM)
Fluoride: 376.1 (#/hr)
                                         From Pond
                                           V
Scrubber
                                       Efficiency:99.0%
                                                   To Pond
                                                                           65060
                                                                           2.21
                                                                                              106012
                                                                                              3.61
                                                   To

                                              Atmosphere
A
                                                                                   North
                                                                                   Stack
40952
1.4
                                                          South
                                                          Stack
                                                         Royster Company

                                                     Triple Super Phosphate
                                                              Run 2

-------
                  Scrubber
                    Inlet
Flow:136147(DSCFM)
Fluorides:330.8 (#/hr)
106681
0.57


From


N


Pond
/

I
63591
0.53

• Scrubber
Efficiency: 99. 8%

\
To P
/
ond




To

^ Atmosphere }

North
Stack

J


*








s

South
Stack

/


v •
43090
0,04

                                                          Royster Company
                                                      Triple Super Phosphate
                                                              Run 3

-------
APPENDIX  B
Field Data

-------
PRELIMINARY MOISTURE DETERMINATION

-------
                                    PRELIMIMARY CHECK FOR STACK GAS
                                MOISTURE CONTENT AND SPECIFIC GRAVITY
V
' Plant fxOW-'S** r i I © Pt %s ; S1W&%@ Stack ^*,/$f&f
*ai
Date ^/Sf /*?^ Sample Time / O 2_^f Barometric Pressure
T ~\
? •'• •' "Hi
Moisture Content -- Method 1 .->
0^
 , & O &
Initial Dry Test Meter Reading ^ ' '3 1 ,, "7 ^ f~~'
/~>7' (7 r**"
{#J & -3
Average Meter Temperature / ^
Average Meter Vacuum ^&^f~r^~^~m
Average Meter. Orifice AK £-\ ~c,<^>
Sampling Rate ' ™~
Barometric Pressure ® Meter Orifice 7 *- '\ "' ""•'
Dry Gas Volume Sampled § 70 °F, 29.92 "Kg
Condensate Volume
Water Vapor Volume 3 70°?; 29,92 "Hg
Moisture Fraction, HoO &'02r~i ^ Fraction Of Dry 'Air. FDA
Ft3
Ft3
Ft3
OF
«W«r
"H-,0
LPM
„„.,
Ft 3^
ml
Ft3

             • Moisture.. Content — Xqthcd 2                            .
                  Dry Bulb Te.np. _ IF  Wet Eulb Temp.      °F  Dew Point Temp.
                 Vapor  Pressure Of .K20 5 DP          •  "Hg   Stack Pressure?6"  ^.^ "Hg

                 Moisture  Fraction,  HgO .  _ ___   Fraction Of Dry Air, FDA
               Specific Gravity
          \
Dry Molecular Weight, Md = J0.^4(^C02;] +J0.32(^02i[ -*-.[o.28(;6
                                                                            N2 +
                  Molecular Weight 3 Stack Conditions, Ms = [CMd-)x(FDA)] +  ^i8)x(K2Co] =
                  Specific Gravity (Referred to air), Gs = (Ms) -7- (28.99)  = _

-------
AA/      Fraction Of Dry Air,  FDA  ^
              Sr-ecj.f ic ..firavity

                 Dry Molecular 'height, Md = ^.^(^002^] +E.32(^02)j +-|0.28(;Si-I2 + CO)] =

                 Molecular Weight 3 Stack Conditions, Ms = [(Md)x(FDA)]  + [?lS)x(H2ol] =

                 Specific Gravity (Referred to air), Gs =  (Ms)  -f- (28.99)  = 	

-------
                     PRELIMINARY CHECK FOR STACK GAS

                 MOISTURE COOTENT AND SPECIFIC GRAVITY
Plant ReJ^'O- 1^%.  Mg-a «,           Stack
Date  .iS/ISf /?"&>     Sample Time	  Barometric Pressure   '     '   "He
Moisture Content — Method  1
                                         f
   Final Dry Test Meter Reading         -•' '    ''
   Initial Dry Test Meter Reading   ^ .&&.  & 'O
                                          ^-")
   Dry Test Meter Volume Sampled__	 & '  O

   Average Meter Temperature	/ -^	'

   Average Meter Vacuum	~r          	
   Averae Meter Orifice A K      &&£>&
   Sampling Rate	|	LFM

   Barometric Pressure '3 Meter  Orifice	>!•?0	   "Hg

   Dry Gas Volume Sampled 3 ?0 °F,  29.92 "Kg	^, 9 "7   	__Ft3

   Condensate Volume	  ^  ' O, c;  y>J •	pi

   V/ater Vapor Volume '§ ?0 °F, 29,92  "Hg             	       ?t3

   Moisture Fraction, H20	Fraction "Of Dry Air, FDA	


Moisture Content. — "nthcd 2

   Dry Bulb Temp. ^£>   "F  Wet  Bulb  Temp.	^.F  Dew Point Temp.	°_?

   Vapor Pressure Of II20 ^ DP   	"Hg   Stack Pressure	"Hg
   Moisture Fraction.  KpO  &' ® &       Fraction Of "Dry Air, FDA  0 ^ •i


Specific Gravity

   Dry Molecular V/eight,  M^ = J0.^4(^C02)| + [0.32(^Og)] +-}o.28(>oM2 + C0)| =

   Molecular V/eight @ Stack Conditions, Ms = [(Md)x(FDA)] -4-  ^1S)x(H202]

   Specific Gravity (Referred to air), Gs = (Ms) -f- (28.99)  = _________

-------


                      PRELIMINARY CHECK FOR STACK GAS

                  MOISTURE CONTENT AND SPECIFIC GRAVITY
 Plant  Pu«j-Q- ^fe    Wq  .'S7M»re.   stack   j>ure.f,r"
 Date £80y»-       Sample Time ffatf j*  IriSl*  Barometric Pressure  2^, ?Z-   "Hg
     (|«II»IH^^^«^""™"""»^"«™™^^»^™^             ™ «*^B»««W » J 1 "I II I «l^ MtJIJ «JIIIJ



 Moisture Content -- Method 1

    Final Dry Test Meter Reading^ _           3 4-4-,C> 0 /     Ft3

    Initial Dry Test Meter Reading _ ; _        342 . ^tf?     Ft3

    Dry Test Meter Volume Sampled__ _ ; _  /•  6 ^ ^   _ Ft3

    Average Keter Teiaperature            '   . _

    Average Meter Vacuum _ •_    _           •

    Average Meter. Orifice AH                 _ .,, £)

    Sampling Rate   _ . _

    Barometric Pressure @ Meter Orifice
    Dry Gas Volume Sampled § ?0 °F, 29.92 "Hg _     . _         Ft
                                            •
    Condensate Volume _ .                 _ ; _   • _  pj.

    V7ater Vapor Volume % ?0 °F, 29,92 "Hg               _ _ Ft
    Moisture Fraction, H20      _   Fraction Of Dry Air, FDA
. Moisture,,Content _-- Method 2        .          .                     .

    Dry Bulb Temp. .     °F  Wet Bulb Temp,	_^F  Dew Point Temp.   ;._ °F

    Vapor Pressure Of H20 3 DP	    "Hg   Stack Pressure  7^- 9   "u~

    Moisture Fraction, H20	   Fraction Of Dry Air, FDA_


 Specific Gravity
    Dry Molecular Weight, Md = ^.^(^C023j +^.32(^022J +'^.28C^N2 + Co]] = _

    Molecular Weight' 3 Stack Conditions, Ms = [(Md jx(FDA)] + -[TlB)x(H2Cl)] =

    Specific Gravity (Referred to air), Gs = (Ms) -f (28.99).  = 	

-------
                            FLUORIDE EMISSIONS
\

-------
                                                  Gainesville,  Florida

                                            SOURCE SAMPLING FIELD DATA SHEET
   Plant
Sampling Location

Date
                      Run No,
                 s
Time Start	j 2.*? I    Time End_

Sampling Time/Point  '/ >y>Gas Density F act or_
   Barometric Press29.9il'Hg, Stack
   Weather
               , W/D'
                          ,w/s
       Le Box No.  ^f    Meter Box No._
   Meter AH@      Pitot Corr. Factor  •
   Nozzle Dia. .25*in.,  Probe Length
   Probe Heater Setting
                           £t
   Stack Dimensions: Inside  Diameter
                    Inside  Area  O /.  $~
                                                                         itial Gas Meter Reading
                                                                             '
                                                                           .   T  .
                                                           lotal Condensate in Impingers

                                                           Moisture in Silica Gel

                                                           Silica Gel Container No

                                                           Orsat:  C02

                                                                  02 _____
                                                                  CO

                                                                  N2
                                                               Excess
                                                                 Air             .
                                                                                                        Filter No.78fl«ft,?j
                                                           Test Conducted by:
                                                                                                A« L*
                                                 -- 7./7
                                                                        Remarks:
#
    Port and
    Traverse
    Point No.
 Distance
^from End
'of Port
  (irrr)"
                 .35"
                         Clock
                         Time
                                  Gas Meter
                                   Reading .
                                    (ft3)
                    933.,
                        •  Stack
                        Velocity
                          Head
                          C"H2OJ
                           Meter
                           Orifice
                          Press. Diff.
                            ("H20)
                                                            Calc.   Actual
                       Stack Gas
                         Temp.
Gas Sample
Temp.t? Dry
Gas Meter
  C°F)
Sample
 Box
 Temp.
                                                                                      In
                                                                            Out
 Last
Impiiger
 Test '
Vacuuriij
  on
Sampl
Train
("Hg)
                                                            Qjo.
                                                   O,l o
                                                                                        3^,
                    ^40,
                                                         L3£
                                                                            7?
                                                                                        22L
                                                                                II
                                                   0*10
                                                                         2L
                                                                                                  5"
       5
    ~£
 I- 40
)3_/_4
957,. /
<9-^
                                                         0.64
                                                                          7?
                                                    0.60
                                                                           93
       7
  1.0*
                                                                                                               6

-------
Port and
Traverse
Point No.
          Distance
          from End
          of, Port
              ft
Clock
Time
Gas Meter
Reading
 (ft3)
Stack
Velocity
Head
C'H20)
Meter
Orifice
Press, Diff,
  C"H20)
                                                   Calc.
                                     Actual
Stack Gas
  Temp,
Gas  Sample
Temp .@ Dry
Gas  Meter
  ra-
                                                                              Out
Sample
 Box
 Temp.
Last
Impinger
Temp.
 ra
Vacuum
  on
Sample
Train
                      133-7
                                         o,
                              a 79
                                                    a
L
    II
           S.io
                      LSJZL
              7,20
                     0,10
                                            0,1
                                                     /'
                                                     /,
                                               2/
                                             . -ft.
                                                                         loo
                                                                 _ZZ
                                                                 77
                                                                           loo
                                            2JL
                                                                         }QQ
                                                                        loj_
                                                                                                      7
                                                                          «Kn  I
                                                                          3  1
                                                                          «^
                                                                                                 "h^
                                                                                                  I  c#


-------
                                             Gainesville, Florida

                                        SOURCE SAMPLING FIELD DATA SHEET
Plant
Sampling Location

Date  ^
                  Run No,
Time Start
                     Time End
Sampling Time/Point

       °F, WB 	
DB
    F, VF @ DP
               'Hg
Mcisture^^TJ, FDA

Barometric.

Weather
                    ,Gas Density Fact or

                    g,  Stack
 ample Box No,__Tl___Meter Box No.	£
         / ^JO ff  •                ,*— jrf»*
Meter

Nozzle
                   Corr.  Factor
               in. , Probe Length
          «_ft
Probe Heater Setting
Stack Dimensions: Inside Diameter
                Inside Area_ --j^i
                Height    ~~
               in
              Tt2
               ft
                                             /
                                           ,-,/'
                                                        2±
                                                             H
                                                     &$.
JLL
                                 13.7
                                              0,30
                                                7S-
                                                                           33L
                                                            QJtL
                                                                       75-
                70
                                2.0,5
                                                75-
                                                                          JLSL
    7
                                                      0,75
                                     0.7S
                                                         75"

-------
Port and
Traverse
Point No,
          Distance
          from End
          of Port
            (in)
   £
Clock
Time
Gas Meter
Reading
 (ft3)
JL
17.
 /V#i
            6,9?
       JtZ*.
Stack
Velocity
Head
C"H20)
Meter
Orifice
Press, Diff.
  ("H20)
                                                  Calc, | Actual
                                                   'M^g&jL
                                         0.70
                                         o.iz

Stack Gas
  Temp.
                                  £>.^7
                                                                75"
                                                                7C
Gas Sample
Temp.@Diy
Gas Meter
  C°F)
                                                                        In
                                                                •7S-
                                                                           Out
Sample
 Box
 Temp,
 TO'
                                                                          2*
                                                                         -H
                                                                                          6$
                                                                                                6
                                                                           ./^}
                                                                            Z'5J
                                                                                                    —1

-------
      Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
Plant
                               Mat'l Processing Rate
Sampling Location jjjLH'T
Date "3 -t- 72 Run No, ?
Time Start Q "%?> ^ Time End 1 ( O ~Z_
Sampling Time/Point 7w~U, /£•/• ( \2& u-CvO
DB °F.
WB °F, VF /DP , £7S~£> "Hg
Moisture2/?Z%,FDA.?7 ,Gas Density Factor
Barometric Press2?,VHg,
Weather CC^^> te.
Stack Prc
sss2fc*£'Hg

Temp. 75- °F, W/D ,W/S
Sample Box No, ^ Meter Box No. f
Meter MI@f,7«? Pitot Cor
Nozzle Dia.
r. Factor
, %3
, ? Tin. , Probe Length $T ft
Probe Heater Setting • ^%&
Stack Dimensions: Inside
Inside
Height

Port and
Traverse
Point No.
1
2L
^f^
£f
£~
6
7

Distance
from End
of Port
(in.)







Diameter 1i>?/#
0^17
ofoy-
€>^3/
p$$$
OW?

OM.,.,7^
Gas Meter
Reading
(ft3)
7O. *&
•757*7
$ /• S~
$23
^J3 tf
*$&¥
/o&l
• Stack
Velocity
Head
("H20)
0.70
O*6O
Oi&O
Q.bt>
&>kJ
o.fee*
0&$
Final Gas Meter Reading / '?'¥ ,,%••& £> ft3

Meter
Orifice
Press. Diff.
("H20)
Calc.
2,9
2.%
2/36
2,3&
2.7&
_2jfc
2.?^
Actual
2-S'
£ * J* O
"i? ? /-»
2,36
2,70
2.3fe>
1>7t>
Lsiitial Gas
T3€'"'itd * *
Total Condei
Moisture in
Silica Gel
Orsat: C02
r °2-
co
N2
Excess
Air
Test Conduc
Remarks : T
c&imv
Meter Reading £J. S SO ft3
is ate in Impingers tL 3 *5 ml
Silica Gel
Container No




/2-*2- gm
&(<% Filter No ."22O$






ted by: /$ .^ , LO t L So<«J
UA)^



Stack Gas
Temp .
7*
7«<
7?
?y

itj

(< , >^t A-^cjift.*—


4 &]£[&£. QftP F/irtO
fitrZ/UG 33s£ift&


Gas Sample
Temp . @ Dry
Gas Meter
In
•70
7?
7&
7&
76
7f

Out
6&
&*7
4^9
7^
-71
7^.
73
Sample
Box
Temp.
(°FJ
	
^-—
—
—
— -
~-
-
Last
Impirger
Test
9^
7f

7^
7^
7
-------
'Port and
jTraverse
Point No,
Distance
from End
of Port
  (in)
Clock
Time
Gas Meter
Reading
 (ft3)
Stack
Velocity
Head
C'H20)
Meter
Orifice
Press, Diff.
   ("H20)
Stack Gas
  Temp,
  •TO
Gas Sample
Temp. @ Dry
Gas Meter
Sample
 Box •
 Temp,
Last
Iinpinger
Temp.
Vacuum
  on
Sample
Train

-------
Plant
Sampling Location/^^(j^  CM.Z. 6

Date  2.**- 2^\~"? £-»Run No.  	/
                              -fV'IF	T-NT/" TIG I   1INC.  T«V
                                   Gainesville, Florida
                             SOURCE SAMPLING FIELD DATA SHEET
                                                            Mat'l Processing Rate
Time Start   /£ ,'^£>T.ime End^

Sampling Time/Point
DBJ?|T_0F, WB
Moisture!?! Q%, FDA

Barometric Press^/^"Hg,  Stack Press^Q "Hg

V»:eatiier    /A3£tl>t£   $ L.l>&t	
Te;np.   ^-~CF, W/D   —   ,W/S  —*•	

Sample Box No.   ^»»  Meter Box No.   ^f
Meter AH3  J,£zPitot Corr. Factor_       ^

Nozzle Dia. /y in., Probe Length

Probe Heater Setting	**~>&?
Stack Dimensions: Inside Diameter
                  Inside Area
                                                            Final Gas Meter Reading
                                                                                                                      ft5
                                                             Initial Gas Meter Reading
                                                             Total Condensate in  Impingers_

                                                             Moisture  in Silica G
                                                                                                                 *?&>
                                                                                                                      gm
                                                            Silica Gel Container No.

                                                            Orsat:  C02

                                                                    02
                                                                    CO
                                                                                                         Filter Ko.
                                                                                  N2._
                                                                               Excess
                                                                          Test  Conducted by:
 Port and
 Traverse
 Point No.
Distance
from End
of Port
 (in.)
               W*
               -if--— <
                          Clock
                          Time
Gas Meter
 Reading
  Stack
Velocity
  Mead
 •("H20)
  Meter
 Orifice
Press. Diff.
  C'H20)
                                                            Calc.
                                                     Actual
Temp .
Temp.@ Dry
Gas Meter
  C°F)
                                                                                       In
                                                                               Out
                                                                                                   Temp.
                                                                        Test
                                     Sample
                                     Train
                                     ("Hg)
                                                                              3o.
                                                                        29-
                                                                                             M
                                              SfSt
                                                                   6,
         3
                                                                   0
                                                                                             gt)
                            1 Cfo
                                                                                      3$
                                                                                      S3
                                                                                                             'O
                                                                                                                    :?:

-------
Port and
Traverse
Point No. .
tyi&^lS

k





















Distance
from End
of Port
(in)
&l
*_/
/
J4f*
f " " -"-











,








Clock
Time
•*9 » £'•*/?
^_-£*>.b /,
3* / 2*
.. f &\
eaasf





















Gas Meter
Reading
(ft3)
J6$?>i
' loy$.e&
f • • * *
ma*-





















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Velocity
Head
("H20)
O*% *5
*> &>£»*•.
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Va*''/ i&^*^












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Orifice
Press. Diff.
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o>7f
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"""ii
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Stack Gas
Temp .
(°F)
§0
a-
. I^w^o^H^





















Gas Sample
Temp .8 Dry
Gas Meter
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In
?d»
87






















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w
%4






















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Box
Temp.
(opy
33E?y.*M«»
(MHijijjin*
^«»,





















Last
Impinger
Temp.
(°F)
yd
^r ^5
_JTS_


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on ''
Sample
Train
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j*^«* JT:*%J
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i
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,


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i











-------
Plant
                                             jbiMViKUNMluYIAL ENGINEERING,  INC,
                                           I       Gainesville,  Florida

                                            SOURCE SAMPLING FIELD DAtA SHEET
Sampling Location_

Date   2^-2^-7'2, Run No,
                       Time End
Time Start

Sampling Time/Point

DB *W]) °F, WB   ^r^F; VF @ DP
                                          Hg
Moistur
              FDA
                      .Gas Density Fact or
Barometric Pres

Weather

Temp.
                       ,  Stack PressJ|'.$ "Hg
             > W/D
                           ,W/S
Sample Box No.
Meter AH@

    ie Dia.
                      Meter Box No.
                                          ft
Probe Heater Setting	_L
                                   ******$ -r*»
Stack Dimensions: Inside Diameter Q^|f in
                  Inside Area   £*?,,  j^jj^Ex.2
                  Height	ft
                                      Mat'l  Processing  Rate	

                                      Final  Gas Meter Reading	

                                      Initial  Gas Meter Reading	

                                      Total  Condensate  in Impingers

                                      Moisture in Silica
                                                                                                                      .ft->

                                                                                                                      ~ft3'
                                                                                                                       ml
                                       Silica Gel  Container No._

                                       Orsat:   C02	

                                               02	

                                              . CO
                                                                                                                 No ."  
-------
Port and
Traverse
Point No,
Distance
from End
o£ Port
(in)
il&M <£"
|^ -
.4























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•








Clock
Time
£'35T























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Reading
-(ft3)
^-"7 S
o /*l®
*$£*• l/tyO
.-—





















Stack
Velocity
Head
C"H20)
"&i &2~
rf^>rf *7^
vi^r Q
^£^
Vacuum
i
on
Sample
Train
J^oj
.^s*,
(Ci jf®
O«- f J
VWI«.LIL:!"'. j cwrST*«i.«r*^
j





















!
"
.







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-------
Plant
Samp ling Loation
                                            E'
                                                Gainesville, Florida

                                           SOURCE SAMPLING FIELD DATA SHEET
                                                                         Mat'l Processing  Rate
Time Start

SampjjjTg Time/Point

DB
  	'°P,  WB ^°F. VF @ DP	
Mo i s ture^.-fll, FDA *7 jy. l/Gas Density F act or_
                           .W/S
Barometric Press.l^V'Hg, Stack

V/oatlier	|

Temp.	°F,  W/D	    	

Sample Box No.   ""2-- Meter Box No.

Meter &H@ /,6>"%>itot Corr. Factor^

Nozzle Dia.  l/jAn., Probe Length

Probe Heater Setting
                                         ft
Stack Dimensions:  Inside Diameter
                  Inside Area_j*
                  Height	~
'^p
IT

d/9*M"
. N\ ^^^iSssta^
- NX **^ 	 J

A •/ /
-//
6-





Final Gas Meter Reading ASia"* *7<3o ft-
Initial Gas Meter Reading yO. -^ v^ ft-
Total Condensate in Impiijgqrs /j*? ml
*-^*wl«< — - - » ^*^ •
Moisture in Silica Gel29%9-ZJ$~Srs /$£ gm
Silica Gel Container No. ^'Z^ Filter No^£i?j1
* *
Orsat: C07
02
CO
N?
Excess
Air
Test Conducted by: ^t 'j^'UJi&^g **^s
0
•

                                                                         Ren1
                                         ft
                                                                                                                      ']
 Port and
 Traverse
 Point No.
              Distance
              from End
              of Port
               (in.)
Clock
Time
Gas Meter
 Reading
  Stack
Velocity
  Head
 C"H20)
  Meter
 Orifice
Press.  Diff.
  ("H20)
                                                           Calc.  Actual
Stack Gas
  Temp ,
Gas Sample
Temp . S Dry
Gas Meter
Sample
 Box
 Temp.
                                                                                     In    Out
 Last
Impir^er
 Test

                                                                                         on
                                                                                       Sample
                                                                                       Train
                                                                                       ("Hg)
                                   IQI, s
                                                                              So.
                                                                                     la
                                                                                  & 9
        3
                                                                              583
                                                           .72
                          /O ; O
                         ions
                                                                                     72
                                                                 21-
                                                    Zff
                                                                                     77
                                                                                 •HW*-*V «\
                                                                                  sQ

-------
Port and
Traverse
Point No,
(W*l
A? 1^5
f
fo





















Distance
from End
of Port
(in)
- gn
J
^5^n
f &




















Clock
Time
/&<&
//tOf
QSMfStSZO





















Gas Meter
Reading
(ft3)
!^%r

<**>**»





















Stack
Velocity
Head
C'H20)
O*Zf
0. 2^






















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Orifice
Press, Diff.
("H20)
Calc,, ! Actual
®k£/
^,f/






















o.8f
o,n






















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Temp.
(°F)
9A
||CJ
f^^A
#<$
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Gas Sample
Temp. @ Dry
Gas Meter
(°F)
In
?F
7?
«r«t#!





















Out
^3
( *a&
*~$fi
/T
f /





















Sample
Box
Temp.
TO'
«JWUU1U^*
^^aj It^f-
5=»ra»





















Last
Impinger
Temp.
(°F)
73
75
Vacuum
on
Sample
Train
$?»O
S (^
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'


!
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. ! .





.
. . . • . .
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-------
                                            LNV JlONMcmKL ciNtjJNEEKilNG*,  INC.'
                                                  Gainesville, Florida

                                            SOURCE SAMPLING FIELD  DATA SHEET
Plant
                               j
Sampling Location
Date  2fe3f?3*
                    Run No.
                               /
Time Start  J£\  I/O    Time hnd
Sampling Time/Point	4-Q 3o ~
                                           f^'-'
                          @  DP
                                         Hg
MoisturGAJj,FDA_
                    __,Gas Density Factor__

Barometric Press«3.O"Hg,  Stack Press^C_
iveather
                                         Hg
            F, iV/D
                           ,!V/S
                      Meter Box No.
Sample Box No.__X,_
Meter AH@  !•"? Pitot Corr.  Factor  , & J
Nozzle Dia-j.J?J?_in.,  Probe Length
Probe Heater Setting      £>/U
                                          ft
Stack Dimensions:  Inside Diameter
                  Inside Area	"
                  Height	
      in
    Tt2
    " ft
                                       Mat'l Processing Rate
                                       Final Gas Meter Reading
                                       Initial Gas Meter Reading
                                       Total Condensate in Impingers

                                       Moisture in Silica Gel
                                       Silica Gel Container N

                                       Orsat:  C02

                                               02
                                               CO
                                               N2
                                                                                                           J , £> "7*7
                                                                                                                  CfO
                                                                                                                       ml ,

                                                                                                                      . & '
                                                                                                          Filter
                                                                                Excess
                                                                                  Air
                                                                           Test Conducted by:
                                                                           Remarks \
                                                                              p-f-.Z
                                                                                              2-
 Port and
 Traverse
 Point No.
              Distance
              from End
             'of Port
               (in.)
                          Clock
                          Time
Gas Meter
 Reading
                                                  •  Stack
                                                  Velocity
                                                    Head
                                                   (MH20)
  Meter
 Orifice
Press. Diff.
  ("H20)
                                                            Calc.
                                                                   Actual
Stack Gas
  Temp .
Gas Sample
Temp.g Dry
Gas Meter
  C°F)
                                                                                       In
                                                                                             Out
Sample
 Box/
 Te
 Last
Impirger
 Test
  C°F)
\:acuuir,
  on
Sample
Train
                                                                                                                   ("Hg)
I-  /
                                          '  7
                                                            LO.
                                                       o
               3L
                                                                    A"/

                                                      is:
                                                                   LL
     (p
                                            2-
                                                                   ^ * o
                                                                                                                    /
                                                    5 *
                                                                    - )
                                                                   .'-A

-------
Port and
Traverse
Point No,
Distance
from End
of Port
  (in)
                Clock
                Time
Gas Meter
Reading
 (ft3)
Stack .
Velocity
Head
C"H20)
Meter
Orifice
Press, Diff,
  C'H20)
                                                      Calc. i  Actual
Stack Gas
  Temp.
Gas  Sample
Temp. @ Dry
Gas - Meter
                                                                             In
                                                                      Out
Sanple
 Box
 Temp,
 C°F)'
Last
Impinger
Temp,
Vacuum
  on
Sample
Train
        f
^
             5V
        II
                                                                 7!?
                                                                          g/f
          /3
                                     .  6
                      73'jb
                                                                 ft
                                                                 tf
                                                                          ft)
                                                3,35
                                                                       /3
                       13:
                    5-77
                                               1*0
                                              it
       6
       7
                                                                              w
                                               to
                                                                             Jdo
                                                                 lot
                                             n
                    S9 7,7
                                       55"
                                                                     101
                                              'bo
                                                        5?
                                                            .£•'55
                                                                                                            .._,
                                               lob
                                              70
                                            75
                                                                             M
      /3
                                 • 70
                                             -lo
                                                                 ttf
                      \S\l
                                 •  10
   f-
                                                                                                ^**i . i i* .^

-------
                          / INC.
      Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
Plant RuA/"0-P|l£ AHafStata^ Mat '1 Processing Rate
Sampling Location () (jfL £T /1/OfTh.
Date <2- 13^/7 3- Run No, ?— '
Time Start /"7 » O4- Time End
Sampling Time/Point ^fl)/n @ 30f>k- &O f° '
DB $^ °F, IVB °F, VF @ DP "Hg
Moisture^?' / % , FDA »9?&, Gas Density Factor
Barometric Fress3o"Hg, Stack Press S° "Hg
We a the r C / £ ^ ^
Termo.^^ °F, 1V/D - ,W/S C^ir^
Sample Box No, / Meter Box No. •""
Meter AH@/-7^Pitot Corr. Factor . ^3
Nozzle Dia. .^5 in. , Probe Length <£> ft
Probe Heater Setting 'O^yU^
Stack Dimensions: Inside Diameter/7^' in
Inside Area ft^
Height ft

•

Final Gas Meter Reading

x~7 'Q tf O f~>c~~7 -F*3
/ a^ n '^A-C^7 / Ii-
Initial Gas Meter Reading £>&% '-aCf? ft3
Total Condensate in Impingers T (o mlA
Moisture in Silica Gel
^6*233.^sgr
Silica Gel Container No. fo/*} Filter No.72^^
Orsat: C09
02


CO
N?
Excess
Air
Test Conducted by: /•

. A fcfco yo
*


Remarks :




                                                                                C"
Port and
Traverse
Point No.
i
^
3
M
£
L,
n
Distance
from End
of Port
(in.)

, 	





Clock
Time
I1:Vl>-V
(^o-o
• Stack
Velocity
Head
("H20)
.25-
'35-
.35-
'4-5-
,,50
• 55"
• ^
Meter
Orifice
Press. Diff.
C"H20)
Calc.
/,o
I'V
/'^
/•^
^'D
a.2-
2. 35
Actual
AO
I'l
/-1/
/^
^L'O
5.^
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Stack Gas
Temp.
(°F)
^?
?9
f?
«"7
??
S"?
??
Gas Sample
Temp.g Dry
Gas Meter
(°F)
In
9?
^
?^
?^
100
loo
IOD
Out
1*
^
?5
?V
9^
fV
?f
Sample
Box
Temp.
C°F)







Last
Impirger
Test
(°F)
s-r
%Q
%a
%o
to
go
fro
Vacuum
on
' Sample
Train
("Hg)
s
&>.&
1
1$
/2
/3-r
ZV i

-------
Port and
Traverse
Point No,
      Distance
      from End
      of Port
        (in)
Clock
Time
Gas Meter
Reading
Stack
Velocity
Head
C"H20)
Meter
Orifice
Press. Diff,
  C"H20)
                                                       Gale,
                                                       Actual
Stack Gas
  Temp.
  TO
Gas Sample
Temp, @ Dry
Gas Meter
  TO
                                                                              In
                                                                             Out
S'ample
 Box
 Temp,
 TO~
Last
Impinger
Temp,
Vacuum
  on
Sample
Train
                                                                                                          n
                                                                                                             —i
        II
 Q
isL
       /s
         -A-
                                                                       I*
                                     \3--3Z  
-------
   it  $uA)-£>^pile
     ri-~<-j />«
Sampling Location	
Date r?/ / A-Z-      Run No,
                                                          EiNUj.illEEK.uNj,
                                                 Gainesville, Florida
                                           SOURCE SAMPLING FIELD DATA SHEET
Time Start/ Q"\Q%    Time End
Sampling Time/Point  «f ^^ 6?
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-------
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-------
      Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
k
Sampling Location Atxrtfir JSbttvvi
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-------
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-------
                                            L.V
                                                                         1
                                                                      JUNO.
                                                 Gainesville, Florida

                                           SOURCE SAMPLING FIELD DATA SHEET
Plant

Sampling Location   @^

Date 2.-2.9 — 77/   Run No,
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                                    fC Final Gas Meter Reading	
                                     Initial Gas Meter Reading_
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                                     Moisture in Silica Gel
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                                                                         Silica Gel Container No.

                                                                         Orsat:  C02

                                                                                 02
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-------
 ort and
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-------
Plant
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                                              Gainesville,  Florida

                                         SOURCE SAMPLING FIELD DATA SHEET
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                                              Final Gas Meter Reading
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                                                                                 70
                                                              
-------
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-------
GRAB SAMPLE COLLECTION

-------
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-------
                                 1
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          Pot At
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                                        \ . \ o
                                  I    I    I    I
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-------
EPA S
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                                  «

-------
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-------
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-------
          APPENDIX  C
Standard Analytical Procedures

-------
                         ENVIRONMENTAL PROTECTION AGENCY
        ' '.     '    '   Research Triangle Park,  North Carolina   27711

Reply to        '.''**''•'      ''  •'                                            ;
 Ann of:                                           ,                   .n t
                                    *•••'•                        Date: 12-21-72
 Subject:  Summary  of Fluoride Analysis •       • c    •


   *7~ •        ;                           •
    °'   R."  Neuiicht,  EMB, IRL                                              •    . i
             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 important 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 ot a slurry or UAU, anu tiitm Iu&«J «1 LI * "1^311.  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.
                                             tioward L.  Crist
                                 Chief,  Source Sample Analysis Section
                                              SSFAB, QAEML
        cc:  . R.  E.  Lee

-------
                Phosphorous Pentoxide Determination

                                                     o
            Colorimetric Molybdovanadophosphate Method
     An aliquot of sample is hydrolyzed in the presence of HC1 and

HNO  acids by boiling almost to dryness..
           f                              ,
     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 min

utes at 400 nm.  The concentration of phosphorous pentoxide is de-

termined from a calibration curve prepared with standard solutions.
                       • -            •  •                     f       '

-------
     APPENDIX  D
Project Participants

-------
                        PROJECT PARTICIPANTS
 John  Dollar
 Tony  Arroyo
 Bill  Demery
 Bob Durgan
 Eric  Johnson
 Bob Maxwell
 A. L.  Wilson
tJnrrDTscherf i nger
 Jerome Rom
 Leslie Evans
 Roy Neulicht
Project Manager
Environmental Specialist
Environmental Specialist
Environmental Speciali:st
Environmental Specialist
Environmental Specialist
Environmental Specialist
Environmental Specialist
EPA-
EPA
EPA

-------