TEST NO. 71 - CI - 32
TEXAS GULF, INC.
SUPER PHOSPHORIC ACID
AURORA, NORTH CAROLINA
NOVEMBER 19, 1971
<>tirirnl
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TEST NO. 71 - CI - 32
TEXAS GULF, INC.
SUPER PHOSPHORIC ACID
AURORA, NORTH CAROLINA
NOVEMBER 19, 1971
Test Conducted By:
Environmental Engineering, Inc.
Contract No. CPA 70 - 82
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TABLE OF CONTENTS
Page
Introduction 1
Summary of Results 3
Process Description 5
Process Operation 5
Location of Sampling Points 6
Sampling and Analytical Procedures 8
Appendices
Appendix A: Emission Calculations and Results
Appendix B: Field Data
Appendix C: Standard Analytical Procedures
Appendix D: Project Participants
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I. INTRODUCTION
Under the direction of the Environmental Protection Agency,
Environmental Engineering, Inc. conducted emission tests at the
Texas Gulf, Inc. phosphate complex in Aurora, North Carolina. On
November 19, 1971, three two-hour test runs were conducted on TGI's
super phosphoric acid production facilities. 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 EPA.
The outlet stack of the off-gas scrubber was measured for
soluble and insoluble fluorides. Grab samples of the scrubbing
liquid, the process reactant, and the process product were also
analyzed for fluoride content. A schematic flow diagram indicating
the sampling location is given in Figure 1.
Complete test restuls are listed in Appendix A.
-------
54%
Acid
L
<$- Steam
Barometric
Condenser
Emissions
Scrubber
Product
Cooler
-{> To Storage
Test
Location
Separator
Box
Gypsum Pond
Figure 1
VACUUM EVAPORATION SUPER PHOSPHORIC ACID
-------
II. SUMMARY OF RESULTS
The plant was operating under normal process conditions
during all of the test runs.
One deviation from standard testing procedure was necessary.
The velocity of the exit gas was too low to be measured by Method
2 of the Federal Register even when using a micromanometer. At the
time of the tests, no other method was available. The EPA project
officer decided to conduct the tests, sampling at a constant rate
determined by the AH@ of the meter box. Jerome Rom (EPA) returned
to the test site at a later date to measure the stack gas velocity.
At this time, he measured the gas velocity by igniting a colored
smoke bomb in the stack and measuring the time required for the
smoke to appear at the stack .outlet. The length of the stack from
the sample port to the exit was known; consequently, the stack gas
velocity could be calculated. Several such tests were made, and
the times .from all the tests were averaged; this average time was
^
. used to calculate the gas velocity. Needless to say, this method
will not give the exact velocity. However, because the process
operation does not vary a great deal, this method should give; an
approximate value for the gas velocity during the actual fluoride
tests.
A complete summary of stack gas conditions and emission
levels is given in Table 1.
-------
TABLE 1
SUMMARY OF RESULTS
FLUORIDES
TEXAS GULF, INC.
SUPER PHOSPHORIC ACID OUTLET
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
*
Volume of gas sampled @ S.T.P.
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
1
11/19/71
30
30
1.9
72
420
90.315
13.148
13.148
0.002
0.002
0.002
0.002
0.008
0.008
2
11/19/71
30
30
1.9
72
420
88.809
35,910
35.910
0.006
0.006
0.006
0.006
0.022
0.022
3
11/19/71
30
30
1.8
71
420
90.157
11.781
11.781
0.002
0.002
0.002
0.002
0.007
0.007
Dry, 70°F., 29.92 inches Hg.
-------
III. PROCESS DESCRIPTION
Texas Gulf, Inc. operates two super phosphoric acid (SPA)
production trains at their Lee Creek, North Carolina operations.
Emissions were sampled from the south production train only.
Texas Gulf, Inc. produces SPA by concentrating 54 percent P^Cv
phosphoric acid to 68-72 percent PO^C-
In concentrating the acid, 54 percent P20g phosphoric acid
is continuously fed to the vacuum evaporator (Figure 1). The
overheads, containing fluorides and water vapor, are condensed in
a barometric condenser. The barometric condenser water flows to
the barometric condenser hotwell after which it is sewered to the
gypsum pond. The product acid (68-72 percent Pp^c) is continuously
tapped from the evaporator and pumped to the product acid cooling
tank where it is cooled before being pumped to storage.
Fluoride emissions from the barometric condenser hotwell
and the product acid cooling tank are controlled by a scrubber.
?
IV. PROCESS OPERATION
All three test runs were conducted on November 19, 1971.
The process operated normally throughout the collection of all
samples.
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V. LOCATION OF SAMPLING POINTS
The sampling sites and number of traverse points were
selected as per "Method I - Sample and Velocity Traverses for
Stationary Sources, Part 60, Subchapter C, Chapter 1, Title 40,"
Federal Register, No. 247-Pt. II-l.
Figure 2 is a schematic diagram of the stack configuration
near the sampling location, and the sampling points traversed
during the emission tests.
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-2O. 5 I.D,
SAMPLE
"POINT
1, 5
2, 6
3, 7
4, 6
""DISTANCE
FROM INSIDE
WALL (INCH)
1.25
5.OO
15.00
__.16.7S
A
t
o-
20.5
A8.s'
Figure 2
SAMPLE PORT LOCATION
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VI. SAMPLING AND ANALYTICAL PROCEDURES
A. Preliminary Moisture Determination
The preliminary moisture content of the stack gas was found
by using the wet bulb-dry bulb method as referred to in the Federal
Register (Vol. 36, No. 247, Part II, December 23, 1971).
B. Preliminary Velocity Determination
Because of such a low flow rate, the velocity could not be
measured as per Method 2 of the above referenced Federal Register.
A micromanometer was used with an S-type pi tot tube in an attempt
to measure the flow; however, the flow rate was so low that this
method did not work. The EPA project officer decided to perform
the tests, sampling at a constant rate determined by running the
sample train at the AH@ of the meter box. The stack velocity was
determined by Jerome Rom (EPA) at a later date. The.method used
consisted of igniting a smoke flare in the'stack at the sample port
and measuring the time required for the smoke to travel the known -?
distance to the stack outlet. Several such tests were made, and
the average time of the tests was used to calculate the velocity
of the stack gas.
C. Sampling for Fluoride Emissions
The sampling procedure used for determining fluoride emissions
was similar to Method 5 of the Federal Register. Other than the
velocity measurement, the major difference between the two methods
-------
was the configuration of the sampling train. The sampling train des-
cribed 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 3 is a
schematic diagram of the sampling train used.
After the selection of the sampling site and the minimum num-
ber of sampling points per Method 2 of the above referenced 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. As already mentioned, because of the low flow
rate, it was decided to sample at the AH@ of the meter box (1.62
inches H?0). The traverse points were selected to maintain at least
one inch frpm 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
impinger liquid, the filter, plus the water washings of the probe and
other sampling train components up to the silica gel were placed into
polyethylene containers. During some runs the different sample frac-
tions were placed in separate containers, while during others all
the recovered sample was placed into one container. Field data sheets
are included in Appendix B.
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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.
E. Laboratory Analysis Procedures
Water soluble fluorides were done by a sulfuric acid dis-
tillation followed by the SPADNS-ZIRCONIUM LAKE METHOD. Water
insoluble fluorides were first fused with NaOH followed by a sul-
furic acid distillation then by the SPADNS-ZIRCONIUM LAKE METHOD.
For more details of exact method used, see Appendix C.
10
-------
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9.
0.
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17.
13.
19.
19
Stainless Steel Nozzle
Heated Glass Probe
Glass Connector ' .
Ice Bath ;
Impinger with 100 ml I-LO (Modified Tip)
Impinger with 100 ml H«0 (Standard Tip)
Inpinger, Dry (Modified Tip)
Impinger with 180 grams Silica Gel (Modified Tip)
Filtsr Holder with No. 1 Whatman Filter
Thermometer ' " ;.
Flexible Sample Line . -
Vacuum Gauge
Main Control Valve
By-Pass Control Valve
Air Tight Vacuum Pump
Dry Test Meter -jy
Calibrated Orifice
Inclined Manometer
S-Type Pitot Tube
Figure 3
FLUORIDE SAMPLING TRAIN
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APPENDICES
-------
APPENDIX A
Emission Calculations and 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. . .
AS1- Effective area' of positive stack gas flow, sq. ft.
NPTS - Number of traverse points where the pitot velocity head was greater than ze
TS - Stack temperature, °R
TM - Meter temperature, °R .
H. -.Average, square root of velocity head,
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 impringers, milliliters
Po - Pressure at the dry test meter orifice, fPB +A. H~[ inches Hg
L 13. 6J
STP - Standard conditions, dry, 70°F, 29.92 inches Hg
Conversion of condensate in railliliters 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 f
Dry gas fraction
Molecular weight of stack gas, lbs/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
-------
EQUATIONS FOR CALCULATING FLUORIDE EMISSIONS
VWV - (0.0474) x (VC)
c
'VSTPD = (17.71 x (VM) x (PB + B_ ) 4. TM . . '
c 13^6
VT = (VWV) + (VSTPD) ' "
c ' -,
.'. W = .(VWV)-HVT) ' - ' ' ' '
r. ' . o
FDA = (1.0) - (W) . ' °
FMOIST = Assumed moisture fraction '
MD = (0.44 x % C6£) + (0.32 x % 02) + (0.28 x % N2) + (0.28 x % CO)
MS = (MD x FDA) + (18 x W)
. GS = (MS)-5- (28.99) . ' . .' ...
EA = [(100) x (% 02 - -^O] -7- Qo.266 x % Np - '(% 02 - ^
U = (174) x (CP) x (H) x V(TS x 29,92)-r-(GS x PS) . ;
QS = (U) x (AS) ^ .
QD = (QS) x (FDA) . . '
QSTPD = (530) x (QD)-f-(TS).x (PS) * (29.92) '
PISO = Qo.oo267 x VC x TS) -)- (PQ x TS x VM -r TM)] ~ [^(Time x U x PS x AN)]
a
Fluoride Emissions: . ' '
KG = Milligrams of fluoride from lab analysis - '
Graips/SCF = (0.01543) x (MG) ~ VSTPD
Grains/CF, Stack Cond. = (17.71) x (PS), x (FDA) x '(Grains/SCF) ~ (TS)
«
Lbs/hour = (Grains/SCF) x (O.OOS57) x (QSTPD)
P20$ Fed = Tons/hour, determined from plant data
v
Lbs/ton P20 Fed = (Ibs/hour)-~ (Tons/hour P205 Fed)
-------
S.QUQCE TSS.T DAT&
TEST NO. -
PLANT - TEXAS GULF SULFUR, AURORA, NORTH CAROLINA
SOURCE - SUPERPHOSPHORIC ACID (S. Stack)
TYPE OF PLANT - SUPER PHOSPHORIC ACID .
CONTROL EQUIPMENT -
POLLUTANTS SAMPLED - FLUORIDES
DRUil IWliBER
2 ) DA TE
3) TIME BEG All
^BAROMETRIC PRESSURE, 1/7 EG
&)METER ORIFICE PRESSURE DROP, IN H20
7) VOL DRY CAS, METER COI1D , CUBIC FEET
B) AVER AGE GAS METER TEMPERATURE, DEC F
9)VOL DRY GAS, S.T.P. , CUBIC FEET
10) TOTAL 1120 COLLECTED, ML
11)VOL 1120 VAPOR COLLECTED, S.T.P. , CU F:
12)STACK GAS MOISTURE, PERCENT VOLUME
1H)PERCEIJT C02
I'j) PERCENT 02
lb)PERCL'HT CO
1DPERCEUT 112
19)MOLECULAR HEIGHT OF STACK GAS, DRY
20)MOLECULAR WEIGHT OF STACK GAS, STK COU>
2DSTACK GAS SPECIFIC GRAVITY
23)AVVRAGE STACK GAS TEMPERATURE, DEC F
. .
2b)STACK PRESSURE, III HG, ABSOLUTE
2DSTACK GAS VEL, STACK COUD, F.P.tl.
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)SAi-;PLi;/G NOZZLE DIAMETER, IllCUES
3^)FLUORIDE - HATER SOLUBLE, MG
3S)FLUORIDE - TOTAL, MG
3G)FLUORIDE - HATER SOLUBLE, GR/SCF
3'DFLUORIDE - TOTAL, GR/SCF
3Q)FLUORIDE - HATER SOL., GR/CF, STK CUD.
39) FLUORIDE - TOTAL, GR/CF, STK CUD.
HQ)FLUORIDE - HATER SOLUBLE, LB/HOUR
HDFLUOR'IDE - TOTAL, LB/HOUR
1
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90.243
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90.315
37.3
1.77
1.9
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28.77
28.54
0.98
72
30
197
2.18
2.18
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120
0.25
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13 . 148
0.002246
0.002246
0.002194
0.002194
0.00808
0.00808
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2.18 J_ 2.18
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35.910 J. ll.TJJ^.
0.006239 1 0.002016
0.006239 J_ O.OQ2016
0.00606 J_ O.OQ.1965.
0.00606 J_ 0.001965
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***S.T.P.+"-DRY, 70 DEGREES F, 29.92 Il.'CIfES MERCURY***
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APPENDIX B
Field Data
-------
SAILING FIELD J3flTB. SHEET"
Plant / fr$
Sampling Location
Run No.
Time Start
Time End
Sarpling Time/Point
DB72. °F, WB
F, VF @ DP
tig
1-fo i s tu r e _ I , FDA , Gas Dens ity Fac tor
Barometric Press^jV'Hg, Stack Press^VHg
Sketch of Stack
Meter Box No, ''
Sarrole Box No.
:--ieter£li@ /-£z Pitot Corr.
Nozzle Dia.Jl./ in =, Probe Length_^/ ft
Probe Heater Setting \j ro '" r
Stack Dimensions: Inside Diameter_2._6 in
Inside Area It 2
ft
Mat'l Processing Rate
Final Gas Meter Reading "7 ~.*f , p. (3
67f ^^/
77? 6^
b*&yy .<
b*i- h
Stack
Velocity
Head
C'K20)
'
Meter
Orifi
Press
C"H
- ^ 2
Calc/
/, ^^'l
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1
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Of?f/ 6^? 1 |f, £3- 1
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Temp ,
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Temp. 8 Dry
Gas Meter
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Box
Temp,
£(sQ^
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Last
Impingsr
Te;:p ,
79-
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fe'L
b~L_
67
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Vacuum
on
Sample
Train
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3.0
B~3-
^~3,?T
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3 'ft
Lj,Q
tf.n
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&(₯ \ 4.3
-------
Port and
Traverse
Point No.
/- *J
^r -t! /?
r "
Distance
from End
of Port
(in)
\ F#/
Clock
Time
A3*
)/35
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Gas Meter
Reading
(ft3)
6$ 8, 'if
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Meter
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Press. Diff
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Gas Sample
Temp.@ Dry-
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C°F)
In
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23
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73
Sample
Eox^
Temp-.
ly^i^
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-------
Plant T" <£ 5
Sampling Location
Date
Run No,
Time Start /?.Jo Time End_
Sampling Time/Point
D3 -
3F, IVB
>F, VF @ DP
I'bistur e I, FDA _ , Gas Density Factor
Barometric Press^_e "Hg, Stack Press_.^j_Hg
r t
V'eatlier . ". '.>> -*
, W/S
Sair.ole Box Xo.
Meter Box No, j>;
Meter /iH1
Pitot Coir. ractGT&.
Nozzle Pi a, yj-f in-., Probe Length' ^/ ft
Probe Heater Setting
Stack Dimensions: Inside Diameter_2_j2in
Inside Area ft2
Heisht } o~? ' ft
Sketch of Stack
SHHBT
Mat'l Processing Rate
Final Gas Meter Reading g *j£j. 3* $
Initial Gas Meter Reading
, i'
Clock
Time
to°
//5S
(^ ! /'-VO
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K
r.s?
?:.Q&
3'- c) $
/
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Temp,
(°F)"
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5
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f^:.% *r,;...
Gas Sample
Temp. 8 Dry
Gas Meter
f°Fl
In
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9-5' 5"
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76
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16
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Out
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Temo =
C°F)
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Last
Impinger
Temp,
^13-
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tJS"
'7'^-
7^4/
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03
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14
Vacuum
on
Sample
Train
("Kg)
3, 5*
31. 31
3.3
33
3.2-
3,3,-
B<3~
3.3
-------
Port and
Traverse
Point No.
/- £/
Distance
from End
of Port .
(in)
Clock -
Time
T/ c
_ _p
-
,
r&30
: flj.^s-
J3'.a?t
3'3D
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Gas Meter
Reading
(ft3) -
. .,/ $(** i ^ . ,
r f.A m /P b
7951% '
\
3.'3<3
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-------
APPENDIX C
Standard Analytical Procedures
-------
ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park, North Carolina 27711
Reply to ' '
Aim of: . r. .
J Date: 12-21-72
Subject: Summary of Fluoride Analysis
*7~"
°'' R." Neulicht, EMB, IRL .
This memorandum is in response to your request for a brief
summary of our SPADNS-Zirconiurn 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.
The water insoluble fraction of the sample is evaporated to dry-
ness in the presence of a slurry or (JAU, and than lustJ wlLIi i^ACII. TliC,
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. ->
.-V^X>A
Howard L. Crist
Chief, Source Sample Analysis Section
.SSFAB, QAEML
cc: R. E. Lee
-------
APPENDIX D
Project Participants
-------
PROJECT PARTICIPANTS
Environmental Engineering, Inc.
Name Title
John Koogler, Ph.D., P.E. Project Director
Dennis Falgout Project Manager
George Allen Environmental Specialist
Eric Johnson Environmental Specialist
Environmental Protection Agency
John Reynolds
Jerome Rom
Roy Neulicht
------- |