Test No. 71-CI-31
Texas buif Sulphur Company
Wet Process Phosphoric Acid Plant
Aurora, North Carolina
November 17-18, 1971
U.S. ENVIRONMENTAL
PROTECTION AGENCY
-------
Test No. 71-CI-31
Texas btilf Sulphur Company
Wet Process Phosphoric Acid Plant
Aurora, North Carolina
November 17-18, 1971
Co-Authors - Jerome 0. Rom
John M. Reynolds
Environmental Engineering
-------
TABLE OF CONTENTS
Page No.
II. Introduction 2
III. Summary of Results . 2
Table 1 - Summary of Results 3
IV. Process Description 4
V. Process Operation 6
VI. Location of Sampling Points 8
Figure 1 - Traverse and Sampling Points 8
VII. Sampling and Analytical Procedures 8
Figure 2 - Fluoride Sampling Train 9
Fluoride Result? Appendix A
Field Data 0
Standard Sampling Procedures E
Laboratory Report F
Project Participants
-------
II. INTRODUCTION
Emission tests were conducted by Environmental Engineering, Inc.
under the direction of EPA at the Texas Gulf Sulphur Company, wet
process phosphoric acid plant. The purpose of the tests conducted
November 17-18, 1971, was to obtain data to be used by both the
Industrial Studies Branch and the Standards Development Implementation
Division.
Measurements were made in the outlet stack for total fluorides while ob-
servations of visible emissions were made by a member of the Industrial
Studies Branch.
Pertinent results of the tests are listed in Table 1. Complete re-
sults are listed in the Appendix of this report.
III. SUMMARY OF RESULTS
Fluoride emissions ranged from 0.0034 - 0.0016 Ibs./ton P^O,- fed.
One test result showed an emission rate of 0.0007 Ibs. fluoride
per ton PpOj- fed which is unrealistically low and should be voided.
Visible emissions were 0%. -.--,-..^-.--
-------
TAtiLE.
OF RESULTS
Fluorides
Run Number
Date
Stack Flow Rate - DSCF.M *
% Water Vapcr - % Vol.
P90r Fed - tons/hr.
£ 0
Fluoride Emissions - Water soluble
gr/DSCF*
gr/CF @ Stack conditions
1 L _/'...
iua./ HI .
Ibs./ton P205 Fed
Fluoride Emissions - Total
gr/DSCF*
gr/CF ©Stack conditions
Ibs./hr.
Ibs./ton P205 Fed
Scrubber Efficiency - %
- 1
11-17-71
17855
1.1
20.83
'
0.0003
0.0003
0.0453
0.0022
0.0003
0.0003
0.0463
0.0022
-
1A
11-17-71
15769
Est. 1.0
20.83
0.0004
0.0004
0.0473
0.0023
0.0004
0.0004
0.0473
0.0023
-
2
11-17-71
19232
1.0
20.83
0.0002
0.0002
0.0329
0.0016
0.0002
0.0002
0.0329
0.0016
-
2A
11-17-71
1 7806
[St. 1.5
20.83
0.0001
0.0001
0.0154
0.0007
0.0001
0.0001
0.0154
0.0007 .
-
3
11-18-71
16746
1.9
20.83
3.0005
0.0005
0.0717
0.0034
0.0005
0.0005
0.0717
0.0034
-
*70°F, 29.92" Hg dry
-------
IV. PROCESS DESCRIPTION
This plant has mu Iti compartment reaction tanks made of reinforced
concrete lined with carbon brick and a protective asphalt material.
The reactor consists of a series of tanks with the slurry alternately
overflowing and underf lowing from one compartment to the next. The
multi -compartment design allows temperature and agitation to vary
throughout the reaction sequence as slurry recirculates through
the tank arrangement. Conditions in the first several tanks are
monitored to insure effective acid attack on the rock, while the
last several compartments are critical to promoting growth of large
filterable crystals of gypsum.
The basic reaction is the acidulation of tricalcium phosphate in
the rock with sulfuric acid and water to produce phosphoric acid
and calcium sulfate di hydrate (gypsum). The reaction is:
Ca3(P04)2
3CaS0
Hydrogen fluoride gas (HF) is produced by a side reaction between
the fluorine in the rock and sulfuric acid. HF subsequently reacts
with the silicates in the digesting slurry to form fluosilicic acid
as follows:
CaF
CaS04-2H20
2 HF
6 HF
H9SiFc
c o
The fluosilicic acid in turn can decompose:
H2SiF6 + Heat and/or Acid Si F4 + 2 HF
Due to the presence of an excess of Si02, practically all of the
fluorine evolved in the reaction and filtration steps comes
of f -as SiF*. However, in the evaporation step, both concentrated
acid and added heat tend to shift the equilibrium to the right
to favor the formation of HF in addition to SiF4.
The acidulation or digestion step is a highly exothermic reaction
requiring considerable apparatus for cooling. A vacuum flash
cooler maintains temperatures in the reactor and degasifies the
recirculated slurry of dissolved air, carbon dioxide, and fluorides
-------
The acidu'lation reaction essentially goes to completion in less
than one hour, but the slurry is retained from five to eight
hours in order to grow large gypsum crystals for efficient
filtration.
Some of the cooled slurry flowing back to the attack tank from the
flash cooler is digested further before being fed to the filter.
The remainder is used to cool the first several attack tanks.
Acid from the last attack compartment is pumped to a feed box
located over the Bird-Prayon rotating-tilting-pan filter. Each
of the pie-slice-shaped cells has a supporting grid beneath a
polypropylene filtering cloth. Acid slurry fed to the cells is
allowed to settle briefly before vacuum is applied, allowing the
larger crystals to precoat the cloth for better filtration. The
rotating pans pass under the feed box and wash boxes, which wash
the filter cake countercurrently with successive additions of
weak acid and water. The filtrates are re-used as washes except
for the first filtrate which is the reactor-filter product.
When the filter cake is vacuum dried, the cell is automatically
inverted to discharge the gypsum. After the gypsum is discharged
by the use of water sprays and compressed air it is repulped and
pumped to a nearby pond.
The reactor-filter product acid is then pumped to a storage vessel
and then to the forced circulation vacuum evaporators where the
acid Cun be C6i~iCciii.rai.eu from 30 to 54i f"oU5'
Basic Data
Design/Construction . Wellman-Lord, Inc. ;
Start-up Year 1966
Feedstock Calcined N.C. Rock fe;
Fluorine in Rock (typical) . 3.5-4% £'
Typical Rock Used (% P205) 29-30% |
Scrubber Type Teller Crossflow |
Packing Used Plastic Tellerettes £
Inlet Ducts 2 '
Scrubbing Medium Gypsum Pond Water :"
Gas Phase P, "H90 6 £
£. ,r<
The Teller crossflow scrubber design has a primary scrubbing section I;
consisting of countercurrent sprays of gypsum pond water. The "'.
gases then undergo a change of direction for better vapor-liquid ;:,
contact by passing through a section of irrigated baffles before ;'.,
flowing through the Tellerette packing. i\
-------
V. PROCESS OPERATION
Run 1 was begun @ 9:10 a.m. on Wednesday, November 17. The
west train phosphoric acid plant was selected for testing.
The east train was down for maintenance and repairs. Although
the west train was running at 10% below normal operating rates,
it was decided to commence with the test since higher rates
were not attainable at the time. The low production rate was
due to limited steam supply from the sulfuric acid plant. The
reactor-filter product (30% acid) tank was at the 93% level,
and due to plant design there was no room for accumulation in
the system. Since the evaporators could not be supplied with
sufficient steam to increase rates thereby decreasing the level
in the 30% acid tank, and since the sulfuric acid plant steam
production was expected to continue at the same rate, it was
impossible to test under higher rates. Even if sufficient
steam had been available, the relatively poor quality of filtra-
tion would have prevented operation at a higher rate. Seven
filter pans were dumping wet, indicating plugged filter cloths.
Higher operating rates would have resulted in even greater pro-
duct losses and higher fluoride emission levels from the filter.
Several process control adjustments were made during Run 1. Sul-
furic acid flow to the reactor was slightly increased at 9:20 a.m.
due to decreasing SO/i content in the slurry going to the filter.
A corresponding adjustment was made to tne dilution water su iiial
the proper ratio was maintained.
At 10:20 a.m. the wet filter pan problem was becoming more severe,
so the filter makeup water flow was reduced. Run 1 was completed
at 5:20 p.m.
The scrubbing system appeared to be operating under normal condi-
tions. Ammeter readings showed that the scrubber booster pump
was operating at 63% of full load while the scrubber fan was run-
ning at 70% of full load. Booster pump discharge pressure reached
70 psig (approximately 22 ft. T.D.H.) after the suction strainer
was removed and cleaned. The east train scrubber booster pump
suction strainer, had been removed and cleaned upon discovery of
the west train plugging problem. However, the east train pump dis-
charge pressure was approximately 84 psig as compared to 70 psig
on the west train. Several reasons for this difference were pro-
posed, but none could be verified. One possibility was that
additional undetected plugs existed in the west train piping system
and could have caused excessive pressure drop. East train booster
pump ammeter readings indicated normal operation at 52% of full
load. The scrubber fan was pulling 70% of full load.
-------
The two overflow streams coming from the packed section of the
east train scrubber appeared lower in magnitude than their
counterparts on the west train scrubber. This was an indication
that the east train packed section strainer or nozzles could
have been partially plugged.
With the west train shut down for maintenance and repairs on the
filter, Run II was started at 3:20 p.m. on the east train. The
east train is identical to the west train (mirror image).
Operating rates were still stymied as before due to the*limited
steam supply from the sulfuric acid plant. Filtration was
excellent for the duration of the. run, with no pans dumping wet .
Only minor adjustments had to be made to the process.
Process conditions remained essentially the same for Runs II and
III.
-------
VI. LOCATION OF SAMPLING POINTS
The sampling location well exceeded the 8 diameters downstream
and the 2 diameters upstream restriction, so sampling was conducted
in 3 equal areas. Six points were sampled on each of 2 perpendicular.
axis (Fig. 1).
Figure 1 - Traverse and Sampling Points
VII. SAMPLING & ANALYTICAL PROCEDURES
A. Moisture Determination
Percent moisture in the stack gas was determined by pulling
a measured volume of stack gas through a heated glass probe
and into 2 preweighed midget impingers containing 15 ml.of."
water and sitting in an ice bucket. The percent moisture was
calculated from the gain in weight of the impingers due to the
water collected, and the volume of gas pulled through the impinger.
B. Velocity Traverse
Velocity pressure and temperature measurements were made at 6
points on each of 2 perpendicular axis (Fig. 1). The velocity
pressure was measured using an S-type pi tot tube and oil mano-
meter, and the temperature determined using a dial thermometer.
C. Fluoride Sampling
The EPA fluoride sampling train (Fig. 2) was used for this testing.
A Whatman #1 filter was used in the train for Runs 1, 2, and 3, and
a glass fiber filter (MSA 1106 BH) for Runs 1A and 2A for comparative
purposes. In all runs the 1st and 2nd impingers contained 100 ml.
8
-------
H90 each, the 3rd impinger was dry and the 4th impinger
contained approximately 175 grams of accurately weighed
silica gel.
1. Stainless steel nozzle . 12.
2. Stainless steel coupling 13.
3. Heated glass probe and sheath 14.
4. Filter holder 15.
5. heated section of sample box . 16.
6. Ice bath section of sample box 17.
7. -Modified Greenburg-Smth inpinger 18.
8. Grecnburg-S-oith inpinger 19.
9. Modified"Grcenburg-Sr.Hh impinger 20.
10. Modified Greer.Lurg-Smith impinger. 21.
11. Thernameter
Check valve
Umbilical cord
Vacuum guage
Course adjust valvet
Leakless Dump
Fine adjust valve
Dry gas meter
Calibrated orifice
Dual mjnor.eter
S-type pilot tube
Figure 2 - Fluoride Sampling Train
-------
The data from the velocity traverse was used to determine
the nozzle size needed to sample isokinetically and at a rate
. of approximately 0.75 cfm. The center of each area (Fig. 1) was
sampled isokinetically for 10 minutes for a total of 120 minutes
per each test run. Isokinetic flow was maintained using the
nomograph described in the test procedures. Complete test
procedures are in the Appendix.
Runs 1 and 2 were above the isokinetic sampling rate due to a
leak in the orifice manometer. Runs 1A, 2A, and 3 were well
within the ± 10% of 100% isokinetic.
Samples of incoming materials, product, and scrubber liquids
in and.out of control devices were also collected during test
runs so that completp fluoride and PpOj- balances can be calculated.
D: Analysis
Water soluble fluorides were done by sulfuric acid distillation
followed by the SPADNS-ZIRCONIUM Lake Method.
Water insoluble fluorides were first fused with N OH followed by
a sulfuric acid distillation then by the SPADNS-ZTRCONIUM Lake
Method. P~0r analvsis were done by plant personnel.
10
-------
APPENDIX A
Fluoride Results
-------
i:.'j"JRT NO.
PAGE
OF
PASES
M,
71-CI-31
No. Runs 5
Name of Firm Texas Gulf Sulphur Company _
ocation of Plant Aurora, N.C.' "
Type of Plant Wet Process Phosphoric Acid
Control Equi pinr-nt. Teller Cross-Flow scrubber
Sfijriplinq Point: Locations Stack Outlet
Pollutants Sarr.pled Fluoride
Time of Particulate Test:
Run No._
Run Mo._
Run i!o._
i\uii nC
Run No."
IA
Date 11-17-71 Begin 0900
Da te 11-17-71 Beg i n 1233
eg in
iy 11
Begin
End 1140
End 1433
Date 11-17-71
n-, J- * T 1 1-7 TT
L/U UC I I I / / I
Date 11-18-71
n ^ ..
ucy i ii
1520
I C.VJVJ
1747
End 1730
End 1415
End 1947
FLUORIDE EMISSION DATA
No.
? barometric pressure, "Hg Absolute
i-1^ orifice pressure drop, "H?0
V n volume of dry gas sampled CJ rr.eter
'' conditions, ft.3
T Average Gcs Meter Temperature, F
V Volume of Dry Gas Sampled & Standard
std. Conditions, ft.*s
V Total H?0 collected, ml., Impingers
w & Silical Gel.
Volume of Hater Vapor Collected
ft. 3 0 S-tendnrd CcuidHion^
L :....-
ri
c
1
30
1.27
20.905 {
69
222.43
54.1
2.46
1A
30
1.50
H.885
94
78.77
Est.
Est.
2
30
1.56
?35.302
72
236.26
53.4
2.42
2A
30
1.74
86.006
92
83.09
Est.
Est.
3
30
1.16
'5.752
63
77.13
33.0
1.50
S
i
'A
r
«
>', .
.*
''&
;:.f
3
«4
'/St
^
*-:"
"'*
* 70°F, 29.92i! He;.dry
-------
FLUORIDE EMISSION DATA (cont'd)
Hun Ho.
%l'i - % Moisture in the stack gas by volume
'
\'\, - Mole fraction of dry gas
% co2
% o2 ..-"-.
% tiy
K V! . - Molecular weight. of dry stack gas
M W - Molecular weight of stack gas
<^Ps - Velocity Head of stack gas, In. HO
Tc - Stack Temperature, F
? /I>~xu^o)
ji - »
1 n CJ.-.^I- l)v.ni-r >i»r> " Hn C.I 1 . . j. .
1 ^ ~s VVIKIX 1 v--/- - i ~ > ..-,. f'-JlylJV, I U l-C
V - Stack Velocity 0 stack conditions, fp:n
A - Stack Area, in.
Q - Stack Gas Volume & *
5 Standard Conditions, SCF.M
T. - Net Time of Test, min.
D - Sampling Nozzle Diameter, in.
%1 - Percent isokinetic
mff - Fluoride-Water soluble, mg.
nf^. - Fluoride - total, mg.
*
CF - Fluoride - Water soluble, gr/SCF
an
i
i Cf . .-- Fluoride - total, gr/SCF*
.30
1
1.1
0.99
29
28.89
75
14.09
30
2081.9
1256
17855
120
.025
264.8
4.397
4.397
D.0003
L0003
1A
Est.
1.0
0.99
29
28.89
80
12.56
30
1855.9
1256
15769
120
0.254
102.9
1.876
2.148
0.0004
0.0004
2
1.0
0.99
29
28.89
73
15.12
30
!234.1
1256
19232
120
0.25
261.1
2.568
2.603
0.0002
i
;0.0002
2A
Est.
1.5
0.99
29
28.89
70
13.92
30
2056.8
1256
17806
120
0.254
96.10
0.415
I
j 0.620
p. oooi
b. oooi
3
1.9
0.98
29
28.. 78
72
13.25.
30
1961.5'
1256
16746 .
120 i.
0.25
97.9
2.485'
2.526
0.0005
0.0005
CF.
Fluoride - Water soluble, gr/cf ^stack
conditions
0.0003 !0.0004 :0.0002 0.0001 J0.0005
-------
FLUORIDE EtilSSIG;: DATA
! I' '!.,
CF - Fluoride, total, gr/cf @ stack cond.
M U
CF - Fluoride - water soluble, lb/ hr
aw
CF - Fluoride - total, lb/hr.
ax
CF - Fluoride - water soluble
ay Ibs./ton P00r :ped -
CF - Fluoride - total, Ibs./ton P0Cv Fed
32 c- 0
i
0.0003
0.0463
0.0463
0.0022
0.0022
1A
0.0004
0.0473
0.0473
0.0023
0.0023
2
0.0002
0.0329
0.0329
0.0016
0.0016
2A
0.0001
0.0154
0.0154
0.0007
0.0007
3
0.0005
0.0717
0.0717
0.0034
0.0034
*70°F. 29.92" Hg. dry
-------
APPENDIX D
FIELD DATA
-------
SOURTE^SAMETOJG FTECD
Plant "J~" C=r -5 Mat'l Processing Rate-"- &OQ ~f~P D
Sampling Location /%,...< A-v-CCv..^-/^^ 0^-t.ii-1'
Date ( f *"~ /7 "" 7 / Rurt No . f
Time Start «? ; / d <& Time End /^ -. V ^ ^
Sampling Time/Point /^?/mWv
DB .5"^ °F, WB,5"/~/"*S
Stack Dimensions: Inside Diameter jO in
_ ._ - Inside Area ft.2
w-~ " ' - Height .. ft
/?"/> trP./?^- F~ \& (Ljt*~> -^jTf-i.^A;
Sketch of Stack
\
t
i
' s
< s.S
^^
Final Gas Meter Reading 3&3. 2 '/2^ ft3
Initial Gas Meter Reading /3 2 - 33 7 ft3
Total Condensate in Impingers = ~1-3~* m^-
Moisture in Silica Gel gm
Silica Gel Container No. .33,5"* Filter No, /
Orsat: C00 3 O \ 6 .&
CO O- -~0-
N7 ??, / 7^-0
Excess ''-''" ,
Air .'J.,-; /I. . ..;.-'.»
Test Conducted By: rq/Qoul
AJ/4 »
Joh /> 5 c n
Remarks :
'' ° ' -. ^ . .
Port and Distance Clock Gas Meter Stack Meter Stack Gas Gas Sample Sample Last ' Vacuui
Traverse from End Time Reading Velocity Orifice Temp, Temp.@ Dry Box Impingpr on
Point No. of Port (ft3) Head Press. Diff. (°F) Gas Meter Temp, Temp, Sampl
Port and
Traverse
Point No.
H
/'"2-
i'?
\-tf
Distance
from End
of Port
(in)
' -Vy'
$ Vt"
>) 3 fa"
Z£ Yf"
Clock
Time
c\'}3
c/.'/T
*
- ' / c5*
/ / '
Stack Gas
Temp,
^ t
5H '
frl '
^$5 !
% ,5" :
£2-- ';
^r z
Gas Sample
Temp . @ Dry
Gas Meter
f°F
In
^0
/<0
^ /
^tJL
£7
-7/
7Z
Out
<^O /
^o >
^C /
£o ''
(2 / ^
A ( '
6 *-
(/ 7
Sample
Box
Temp,
'
'
Last
Impingpr
Temps
3-5^
f2*
^l/
5 z/
.'f
/£. ^
IS
-------
Port and
Traverse
Point No.
Distance
from End
of Port
(in)
Clock
Time
Gas Meter
Reading
(ft3)
jSU3L
Stack
Velocity
Head
C"H20)
Meter-
Orifice
Press. Biff.
...C"H20)
Cal. Actual
I
A
Stack Gas
Temp,
C°F)
Gas Sample
Temp.@ Dry
Gas Meter
. C°F)
In Out
77
22L
Sample
Box
Temp-,
C°F)
Last
Impinger
Temp.-
Vacuum'
on
Sample-
Train
C'Hg)
1 - 6
[6 '
o. 3?
O-32.
. 72.
72-
.5:7
Z-L
ITT
A7?k
ILA5
70
11 10
0/37
-//
II /s
e. 3
]££.
16
//"2-0
CM
77
13
0 - H 3
?
2-3
.'l f
73'.'
/-^f
1*
77
r.3
-------
^bUR^^SAMPHWS FJlbUJ^ DA1A fsHEET
Plai^i < (jf f) Mat'l Processing Rate
Sampling Location f/t^ $c^l&u*$^ ( ^.A^~^
Date / 1 *. t «7 *y ) Run No . "X
Time Start Time End
Sampling Time/Point \ (3
DB °F,
WB °F, VF @ DP "Hg
Moisture %,FDA ,Gas Density Factor
Barometric Press.7c?,"2J'Hg,
Weather £-£r^t,v_. (jJ
Stack PressJe^'Hg
/JLA-~X^
Temp. °F, W/D , W/S
Sample Box
Meter &H@ /
No. Meter Box
No, ^
.^ 7 Pitot Corr. Factor $. £3
Nozzle Dia..-.2 $" in, , Probe Length *-j ft
Probe Heater Setting
..
-
Stack Dimensions: Inside Diameter^ £? in
Inside Area ft 2
Height ft,
Port and
Traverse
Point No.
M
l~~~2-
j-3
t-iy
Distance
from End
of Port
(in)
,
Clock
Time
o * *~
3 XT
.T 30
75 35"
"9 ."/*
J ^
,? "S"^
S 6-^
Sketch of Stack
?, - '
.0 -.
*, v *
' " V . , / '
1 - >-
\
\
*../
Final Gas Meter Reading £T~ ^9, 0 '/// . ft3
Initial Gas Meter Reading ,^f>3. X ^r^- ft3
Total Condensate in Impingers ^ 5 ml
Moisture in Silica Gel
gm
Silica Gel Container No. Filter No. .?.
Or sat: C02
2
CO
N2
Excess
Air
C)^
/f,7
-c-
7^'H
Test Conducted By: f^a. 1 q V u~7~
Remarks :
Gas Meter
Reading
(ft3)
3'53.a^-x-
.f ^ /. a.
"^69. ^*
_ .
J? o» ""7 ^^"^
r P /» -wX
3^< 5^
//(?^/ 9
4 1 %r ^
Stack
Velocity
Head
("H20)
d.2,2
d-2.2-
c-,lr
^
^^"/
6i.'f
&3~J
i 3"'
^4''/
Sample
Box
Tenp ,
;'7D
&
^
r
V
Last
Imp ings r
Temp t
5V
57
f?^,
Sb"
£3
^3
53
Vacuum
on
Sample
Train
C"Hg)
o
o
(3-f
/<£. £
/Jl/^
ff*0
/6.0
/£, ^
-------
Port and
Traverse
Point No.
Distance
from End
of Port
(in)
Clock
Time
Gas Meter
Reading
(ft3)
Stack
Velocity
Head
C"H20).
Meter.
Orifice
Press. Biff.-
Cal.
Actual
Stack Gas
Temp,
Gas Sample
Temp.@ Dry
Gas Meter-
In Out
Sample
Box
Temp;
ra
Last
Impinger.
Temp,-
Vacuum
on
Sample-
Train
C"Hg)
M^
ML
1-7$
903
l-nf
53
±L
/
72-
75
63
477.7
67
77
70
6.
7r
If)
-2-3
soi.l
LZO
11'
5-0
32L
77^
5-65
, 9
. S"/
-7.1
7-L,
ILO
/
6,
A 9
7V
7'
t
J&o_
A
5* '
1
72
-------
FIELD
Plant / CT>
Sampling Locations/7/^ /Trv^^^/^ (fy'tfT)
Date //^/'
f~7f Run No. "^
Time Start Time End
Sampling Time/Point
DB'7;"3 °F,
Moisture^'7
Barometric
Weather
Temp '~2j5~_
Sample Box
Meter A H@ /
WB73 °F, VF @ DP£/£3 "Hg
%,FDffi/!&Gas DensityFactor^^
Presiga- "Hg, Stack Pressing
°F, W/D : , W/S
No. Meter Box
,/^Z.Pitot C
No. "-/
i^j
:orr. Factor O-- #J>
Nozzle Dia< Ky in,, Probe Length ty ft
Probe Heater Setting }.
Stack Dimensions : Inside
Inside
Height
Port and
Traverse
Point No.
%- "i
?~r~c?
T.-6
1--.3
I
Distance
from End
of Port
(in)
.
7 >' r-.'.C c
^"
; Diameter ^Q_ in
; Area Ft 2
ft
Clock
Time
/3L0TO./'
/z «s.r
/2.-/6
/12.5"
/2-'-3 6
/z JJT
i ^/6
yz ^/ut
Remarks :
Gas Meter
Reading
Sg"^O£>/
.5"^^
Jffi&.S-.
5^.3
£63,5"
6/0. 0
fe/3..>0
<£.>
-------
Port and
Traverse
Point No,
Distance
from End
of Port
(in)
Clock
Time
Gas Meter
Reading
(ft?)
Stack
Velocity
Head
Meter-
Orifice
Press. Diff,
...C'H20)
Cal. Actual
Stack Gas
Temp,
Gas Sample
Temp.@ Dry
Gas Meter-
In
Out
Sampte
Box
Temp-,
Last
Impinger
TemD;
Vacuum
on
Sample
Train
("Hg)
"72-
£7
2--
f
£33. /
2.6
6 2,
L2.
6.7
J&L
63
/o
/.
',
f 2-0
2-S"
72-
SS?, 5"
Ml
$jQj_
Ft
£>!
&±£>-
£.0
1.3$
v 0
72-
58
6 ^ 2.
LULL
131
i-r
i
7^
UL
59
3.0
"L
>,? 5"
TL'/o
a
\.
f
-------
APPENDIX E
Standard Sampling Procedures
-------
APPENDIX F
Laboratory Report
-------
ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park, North Carolina 27711
' to
* Date: 1/4/72
Subject: Fluoride Analysis
Texas Gulf Sulphur
-[
Mr. Jerome J. Rom
Emission Testing Branch
THROUGH: Dr. Robert E. Lee, Jr.
Chief, SSFAB
Attached is the Fluoride Data for the Texas Gulf
Sulphur Company. The water soluble fluoride was done
by sulfuric acid distillation followed by the SPADNS-
ZIRCONIUM Lake Method.
The products were first fussed with NaOH followed by
sulfuric acid distillation than by the SPADNS-ZIRCONIUM
Lake Method.
C
Allen E. Rilej
Source Sample and Fuels
Analysis Branch, DAS
Attachment
cc: R. Lampe
J. McGinnity
J. Reynolds-
D. von Lehmden
-------
TBX"S GULF SULPHUR
PHOSPHATE FERTILIZER
i
Sample Number
24 PE
37 PE
38 PE
44 PE
61 PE
56 PE
39 PE
79 PE
80 PE
97 PE
98 PE
113 PE
114 PE
73 PE
74 PE
75 PE
127 PE
128 PE
129 PE
Sample Description
Rock Cake
Rock
Rock.
Rock Cake
Rock Cake
# 1 Filtrate
54 % Phosphoric Acid
54 % Phosphoric Acid
70 % Phosphoric Acid
54 % Phosphoric Acid
70 % Phosphoric Acid
54 % Phosphoric Acid
70 % Phosphoric Acid
Silica Gel
Silica Gel
Silica Gel
Silica Gel
Silica Gel
Silica Gel
F~
11,312 ng/g
45,504 M-g/g
43,130 p-g/g
12,577 ng/g
15,678 p.g/g
F~ M.g/T(
17,472,000
9,948,000
6,280,000
5,483,870
. 6,200,000
5,616,000
5,522.123 -
Gain in.Mass gro
32.1
28.4
15.0
19.3
23.2
21.4
-------
TEXAS GUM' SUf.PHUR
PHOSPHATE FERTILIZER
Sample No.
25 PE
27 PE
29 PE
30 PE
32 PE
34 PE
47 PE
49 PE
50 PE
52 PE
54 PE
62 PE
64 PE
66 PE
67 P3
69 PE
71 PE
PE
86 PE
PE
ll 69 PE
91 PE
93 PE
Sample Description
Probe HO Wash
Filter HO Wash
Filter #1
1st. Impinger* HO
2nd. Impinger HO
3rd. Impinger HO
Probe HO Wash
Filter HO Wash
Filter #2
1st. Impinger HO
2nd. Impinger HO
3rd. Impinger H^O
Probe HO Wash
Filter HO Wash
Filter # 3
1st. Impinger HO
2nd. Impinger HO
3rd. Impinger HO
Probe HO Wash
Filter HO Wash
Filter #4
1st. Impinger H?0
2nd. Impinger H_0
3rd. Impinger HO
Mass qm
0.000
0.000
Fluoride ug/sample
14^8.
1219
1570
140
365
1868
305
30
Total Soluble
Fluoride uq/sample
Total Insolub!
Fluoride ug/
saroplt
4397
2568
0.000
2485
0.000
1209
10243
1660
36
-------
TEXftS GLT.F SUT.PHUR
PHOSPHATE FERTILIZER
Sample No.
Type Sample
Densitv
PH -
Temperature
20 PE
21 PE
22 PE
23 PE
36 PE
40 PE
41 PE
42 PE
43 PE
57 PE
58 PE
59 PB
60 PE
81 PE
82 PE
95 PE
96 PE
111 PE
112 PE
Scrubber HO IN
Scrubber HO OUT
Nash Pump OUT
Hotwell - Condenser HO
Well H O To NASH Pump
Scrubber H 0 IN
2
Scrubber HO OUT
NASH Pump OUT
Hotwell-Condensor HO OUT
Scrubber HO IN
Scrubber HO OUT
NASH Pump HO OUT
Hotwell-Condensor H_O
Scrubber HO OUT
Scrubber HO IN
Scrubber HO IN
Scrubber HO OUT
Scrubber HO IN
Scrubber HO OUT
6.489,000
7,105,250
6,613
116,250
1,170
6,820,000
6,842,000
23,332
282,720
4,552,777
5,422,222
8,056
7,650,000
7,498,667
7,850,000.
'7,026,667
6,936,000'
'8,111,250.
8,137,506;
-------
R
PHOSPHATE FERTILIZER
Sample No.
Sample Description
Total Soluble
Masa crm Fluozide u.q/sample Fluoride jig/sample
Total Insoluble
Fluoifide ucr/samole
99 PE
101 PE
103 PE
104 PE
106 PE
108 PE
Probe H O Wash
Filter HO Wash
Filter #5
1st. Impinger HO
2nd. Impinger H^O
3rd. Impinger H^O
0.000
35910
116 PE
118 PE
120 PE
121 PE
123 PE
125 PE
Probe HO Wash
Filter HO Wash
Filter #6
1st. Impinger H
2nd. Impinger H
3rd. Impinger H
0.000
11781
130 PE. Probe HO Wash
132 PE Filter HO Wash
134 PE ' Filter #7 (012472)
135 PE 1st.- Impinger
137 PE 2nd. Impinger
139 PE 3 rd. Impinger
0.000
1876
141 PE
143 PE
145 PE
146 PE
148 PE
150 PE
Probe HO Wash
Filter HO Wash
Filter #8 (012471)
1st. Impinger
2nd. Impinger
3rd. Impinger
0.000
415
-------
Reply to
Attn of:
Siibirct:
ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park, North Carolina 27711
: 2/15/72
Fluoride Analysis, Texrs Gulf Sulphur
To:
JYir. Jerome J. Rom
Emission Testing Branch
THROUGH: Mr. Howard Crist
Source SBtple Analysis Section
Attached ir the fluoride data for Texas Gulf Sulfur.
The water insoluble were first fussed v:ith N?OH followed
by sulfuric acid distillation then by the SPADNS-ZIRCONIUM
Lake Method.
'£>*. C
Attachment
cc: R. Iverson
f R. Lampe
J. JMcGinnity
D. von Lehmden
R. Lee, Jr.
H. Crist
Allen E". Rile"y
Source, Sample Analysis
Section, SSFAB, DAS
-------
Texas Gulf Sulphur
f '
Srrrolo Number . {J.a/S:-r.nl
0
35
3 ?? 40 . .
4 g>£/^ 17
5 A3/^. .., 0
100
7 272
8 14£?6- 205
On the water soluble portion there was one mistake. .
lumber 43 PS - It is a factor of 10 lev:. It should
read 2,827,200 p.g or 2.8 g/L.
-------
iVIC.1^ I ML. f r\^J
Research Triangle Park, North Carolina 27711
^ ;/: Dau: 2/29/72
''Jfct:- Density 'and PH
Texas Gulf Sulphur
To:
Mr. Jerome J. Rom
Emission Testing Branch .
THROUGH: Mr. Howard Cri?t
SSAS, SSFAB, DAS
Attached is the Density and pH of the scrubber water
ssrr.ples from the Texas Gulf Sulphur Company, which completes
the analysis of all samples.
Allen E. Riley
Source Sample and Analysis
Section, SSFAB, DAS
Attachment
cc: Mr. R. Lampe
Mr. J. McGinnity
Mr. J. Reynolds
Mr. D. von Lehmden
Mr. F. York
Mr. J. Kelly
Mr. D. Slaughter
Mr. H. Crist
-------
TEXAS GUr.F SUT.7HUR
ample No.
20 PE
21 PE
22 PE
23 PE
36 PE
40 PE
41 PE .
42 PE
43 PE '
57 PE
58 PE
59 PE
60 PE
81 PE
82 PE
95 PE
96 PE
111 PE
112 PE
Type Sample
Scrubber HO IN
Scrubber HO OUT
Nash Pump OUT
Hotwell - Condenser HO
Well H O To NASH Pump
Scrubber HO IN
Scrubber HO OUT
NASH Pump OUT
Hotwell-Condensor HO OUT
Scrubber HO IN
Scrubber HO OUT
NASH Pump HO OUT
Hotwell-Condensor HO
Scrubber HO OUT
Scrubber HO IN
Scrubber HO IN
Scrubber HO OUT
Scrubber
IN
Scrubber HO OUT
'HOSPHATE FERTI
Density
1.021
1.020
0.998
1.001
1.003
1.020:
1.016
1.003
1.011
1.024
1.023T
1.002
1.022
1.018
1.025-
1.021
1.016
1.023
1.027
r.TZEl
i
PH
1.5
3.2
9.5
3.9
7.0
2.5
2.9
9.5
2.6
1.5
2.2
8.9
2.4
2.3
2.4
2.4
2.4
1.5
1.3
'Bmperature
O
76 F
6.489.000
7,105,250
6,613
116,250
1,170
6.820,000
6.842.000
23,332
282,720
4,552,777
5,422,222
8,056
7,650,000
7,498,667.;
7.850.0QO. ..
'7,026,667 .:.
6.936,006":
"8,111,250...
8.137,500"
-------
APPENDIX I
Project Participants
-------
PROJECT PARTICIPANTS
Name ' Title
John B. Koogler, Ph.D., P.E. Project Director
Dennis A. Falgout, E.I.T., M.S. . Project Manager
George F. Allen, Sr. Tech. Environmental Specialist
Eric H. Johnson, Tech. Environmental Specialist
------- |