TEST NUMBER 72-CI-17
FARMLAND INDUSTRIES INC.
WET PROCESS PHOSPHORIC ACID
PIERCE, FLORIDA
PEDCo ENVIRONMENTAL
-------
PEDCo-ENVIRONMENTAL
SUITE 8 ATKINSON SQUARE
CINCINNATI. OHIO 45246
51 3 I"?-? 1-4330
TEST NUMBER 72-CI-17
FARMLAND INDUSTRIES INC.
WET PROCESS PHOSPHORIC ACID
PIERCE, FLORIDA
MARCH 1-2, 1972
Prepared by:
Richard W. Gerstle, P.E.
By
PEDCo-Environmental specialists, Inc
Cincinnati, Ohio
Contract No. 68-02-0237, Task 2
-------
TABLE OF CONTENTS
SECTION PAGE
I. Introduction ' 1
II. Summary of Results 4
III. Process Description 6
IV. Sampling Procedures 8
V. Analytical Procedures 12
VI. Appendix 13
Part A - Emission Calculations and Results
Part B - Field Data
Part C - Analytical Procedures
Part D - Test Log
Part E - Project Participants
-------
I. INTRODUCTION
Stack emission tests were conducted, and related process
samples were taken during the period March 1 and 2, 1972 at
the Farmland Industries' phosphoric acid plant in Pierce,
Florida.
According to the terms of PEDCo's contract with EPA,
only stack gas measurements, selected feed and product samples,
and scrubber water samples were to be -taken by PEDCo. All
process data and operating procedures were obtained by EPA
personnel. Sample analyses and emission calculations were
also to be performed by EPA staff.
Three tests were made to determine total fluoride
emissions entering the atmosphere from the phosphoric acid
manufacturing process after a primary and secondary scrubbing
system.
Stack gas samples were taken in the duct after the
scrubber. Figure 1 shows the location of the sampling point.
Three sets of samples were taken at this site to determine
total fluoride content of the gas stream. Moisture, carbon
dioxide, and oxygen content of the gas stream was also
measured; velocity, temperature, and total gas flow were
determined for each test. Samples of feed materials,
-------
41.5"
Detail of Sampling Site
41.5" Diameter
Stack
Secondary Knockout
Scrubber Chamber
o i
CN
= 1" Sampling port
0 i
00 I
.V_
O
r-H
Fan
FIGURE 1. SAMPLING SITE ON PHOSPHORIC ACID PROCESS
-------
phosphoric acid product, and scrubber water were also taken
during each run. Each stack gas sample extended over a two
hour period except for the last test which was cut short
because of a process malfunction.
-------
II. SUMMARY OF RESULTS
The plant was operating under normal process conditions
during the first two test runs. However, during the third
run, one of the filter cloths tore and the plant had to shut
down. For this reason, the third test was cut short.
Even though the sampling site was more than eight
diameters downstream from any obstruction, gas velocities at
the sample point varied widely and the flow pattern was very
tangential. Therefore, total gas flow and related emission
calculations are based on fan performance data and not on
pitot tube measurements. A pressure drop of 24 to 25 inches
of water was measured across the fan. Note that because of
the wide variation in velocity, the probe nozzles had to be
changed from 0.250 inch to 0.125 inch in the middle of each
run.
A complete summary of stack gas conditions and emission
levels for each test run is given in Table 1.
-------
TABLE 1.. SUMMARY OF RESULTS
Run Number
Date
Stack pressure, inches Hg
Stack gas moisture, % volume
Average stack gas temperature, °F.
Stack gas flow rate @ S.T.P.*, SCFM**
Vol. gas sampled @.S.T.P.*, SCFj
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^Or Fed.
Fluoride, total, Ib/ton P205 Fed.
1
3/2/72
30.14
5.3
106
15307
43.79
16.7
16.83
0.006
0.006
0.005
0.005
0.77
0.77
0.04
0.04
2
3/2/72
30.09
5.9
108
15307
80.62
18.5
18.6
0.004
0.004
0.003
0.003
0.46
0.46
0.02
0.02
3
3/2/72
30.09
4.9
106
15307
46.14
18.5
18.67
0.006
0.006
0.006
0.006
0.81
0.81
0.04
0.04
Dry, 70UF., 29.92 inches Hg.
** Flow Rate Derived From Fan Curve
-------
III. PROCESS DESCRIPTION
The first step in the basic process involves mixing
phosphate rock, sulfuric acid, and water to form a reaction
slurry. ;
The basic reaction is the acidulation of tricalcium
phosphate in the rock with sulfuric acid and water to produce
phosphoric acid and calcium sulfate dihydrate (gypsum) . The
reaction is :
Ca3(P04)2 + 3H2S04 + 6H20 -* 2H3P04 + 3CaS04 ' 2H20
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 f luosilicic acid as follows :
' 2H20 + 2HF
6HF + Si0
2
The f luosilicic acid in turn can decompose :
H2SiFg + Heat and/or Acid -» SiF4 + 2HF
The reactor consists of a series of tanks with the
slurry alternately overflowing and underflowing 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.
The acidulation or digestion step is a highly exothermic
reaction requiring considerable apparatus for cooling. A
vacuum flash cooler maintains temperature in the reactor and
degasifies the recirculated slurry of dissolved air, carbon
dioxide, and fluorides.
The acid slurry from the last attack compartment of
the reactor is pumped to a rotating-tilting-pan filter where
the phosphoric acid is filtered from the gypsum. The by-
product gypsum is repulped'and pumped to a nearby pond. The
product acid is pumped to a storage vessel and then to vacuum
evaporators in which the acid can be concentrated from 30 to
54% P2°5'
The cocurrent scrubber design has a primary scrubbing
section consisting of countercurrent sprays of gypsum pond
water. The gases then pass through a section of irrigated
baffles before flowing through the packing in the secondary
scrubbing section.
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IV. SAMPLING PROCEDURES
The gas stream was sampled isokinetically by using a
modified EPA particulate sampling train and following the
sampling procedures described in Method 5 of the Federal
Register of December 23, 1971. The sampling train as shown
in Figure 2 consisted of a stainless steel buttonhook nozzle,
a heated Pyrex-glass probe contained in a steel sheath, a
Greenburg-Smith impinger without a tip, a second impinger
with a tip, a third impinger without a tip, an 80 millimeter .
Whatman No. 1 paper filter, and a final impinger containing
approximately 200 grams of indicating type silica gel. The
first and second impingers contained 100 ml each of distilled
water at the beginning of each test. The third impinger was
initially dry. All impingers were contained in an ice-water
bath and the temperature of the gases leaving the fourth
impinger was in the 65 to 75°F range. The filter was not
heated. An air tight vacuum pump, dry gas meter, orifice,
and associated valves, connectors, thermometers, and
manometers completed the train.
A type 'S' pitot tube was attached to the probe to
measure the velocity head of the stack gas. The sampling
rate was continually adjusted to maintain isokinetic sampling
-------
THERMOMETER
HLIEH HOI Dill
REVERSE-TYPE
PHOT TUBE
STACK
WALL P|TOT MANOMETER
ORIFICE
-L
BY-PASS VALVE VACUUM
OQ_ /MAIN VALVE °AUGE
DRV TEST METER
FIGURE 2. SAMPLING TRAIN USED TO DETERMINE
FLUORIDE CONCENTRATIONS
-------
rates by means of nomograph which related the pressure drop
across the orifice after the meter with the velocity head
measured by the pitot tube. Stack gas temperatures were
measured with long stem dial'thermometers.
In a typical run to determine fluoride concentrations,
the train was assembled and checked for leaks by plugging
the first impinger and drawing a vacuum of 15" of Hg. The
probe and nozzle assembly was then attached to the impinger
and the train positioned at the first sampling point. Each
point along the stack diameter was sampled for ten minutes.
A two hour sampling period was used. At each point the
velocity head, stack gas temperature, final impinger
temperature, meter temperatures, meter reading, pump suction
pressure, and orifice pressure drop 'were measured and recorded,
All data sheets for these tests are attached in Part B of the
Appendix.
Upon completion of sampling, the train was completely
disassembled, the condensate volume measured, and the silica
gel weighed on a triple beam balance at the site. The water
in the impingers was poured into plastic (Nalgene) wide mouth
bottles. The paper filter and all washings from the probe
10
-------
and all glassware was also placed in this same container. When
necessary the probe was also brushed to remove solid matter.
All train components were then dried with acetone and the
!
train reassembled for the next run. Each container was
immediately labeled.
Feed, product, and scrubber water samples were also
placed in plastic bottles and labeled. All samples were
submitted to Mr. J. Rom of EPA for future analysis.
Carbon dioxide and oxygen content of the gas stream were
measured with a standard Orsat apparatus by drawing samples
from the stack directly into the Orsat apparatus through a
one-quarter inch diameter stainless steel probe. The probe
was carefully purged with stack gas before taking the sample.
This procedure was deemed sufficiently accurate to determine
the molecular weight of the stack gases.
11
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V. ANALYTICAL PROCEDURES
Water soluble fluorides were determined by a sulfuric
acid distillation followed by the SPADNS-ZIRCONIUM LAKE
METHOD. Water insoluble flubrides were first fused with
NaOH followed by a sulfuric acid distillation then by the
SPADNS-Zirconium Lake Method.
For more details of exact method used, see Appendix,
Part C.
12
-------
VI. APPENDIX
13
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APPENDIX A
EMISSION CALCULATIONS & RESULTS
-------
NOMENCLATURE
PB - Barometric pressure, inches Hg
PS - Stack pressure, inches Hg
As - Stack area, sq. ft.
TS - Stack temperature, °R <
TM - Meter temperature, °R
H_ - Average square root of velocity head, /inches HpO
AH - Average meter orifice pressure differential, inches hLO
AN - Sampling nozzle area, square feet
CP - S-type pitot tube correction factor
VM - Recorded meter volume sample, cubic feet (meter conditions)
VC - Condensate and silica gel increase in impingers, milliliters
Po - Pressure at the dry test meter orifice, PB + ,-- > inches Hg
STP - Standard conditions, dry, 70°F, 29.92 inches Hg
VWV - Conversion of condensate in milliliters to water vapor in cubic feet (STP)
VSTPD - Volume sampled, cubic feet (STP)
VT - Total water vapor volume and dry gas volume samples, cubic feet (STP)
W - Moisture fraction of stack gas
FDA - Dry gas fraction
MD -.Molecular weight of stack gas, Ibs/lb-mole (dry conditions)
MS - Molecular weight of stack gas, lbs/lb/-mole (stack conditions)
GS - Specific gravity of stack gas, referred to air
EA - Excess air, %
U - Stack gas velocity, feet per minute
OS _ Stack gas flow rate, cubic feet per minute (stack conditions)
OD - Stack gas flow rate, cubic feet per minute (dry conditions)
OSTPD - Stack gas flow rate, cubic feet per minute (STP)
P1.SO - Percent isokinetic volume sampled (method described in Federal Register)
Time - Total sample time, minutes
-------
EQUATIONS FOR CALCULATING FLUORIDE EMISSIONS
VWV = (0.0474) x (VC)
VSTPD = (17.71 x (VM) x (PB + 0 H_ ) -f. TM
13;6
VT = (VWV) + (VSTPD)
W = .(VWV)-HVT)
FDA = (1.0) - (W)
FMOIST = Assumed moisture fraction
MD = (0.44 x % CO ) + (0.32 x 7, 02) + (0.28 x %. N2) + (0.28 x % CO)
MS = (MD x FDA) + (18 x W)
GS = (MS)-f- (28.99) . .
EA = [(100)' x (% 02 - -^^)] -r- Qo.266 x % NZ) - '(% 02 - %2CO
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)-H(TS).x (PS) v (29.92)
PISO = Qo. oo267 x VC x TS) -} (PQ x TS x VM + TM)] -=- [[(Time x U x PS x AN)]
Fluoride Emissions:
MG = Milligrams of fluoride from lab analysis
Graips/SCF = (0.01543) x (MG) -7- VSTPD
Grains/CF, Stack Cond. = (17.71) x (PS), x (FDA) x '(Grains/3CF) -7- (TS>
Lbs/hour = (Grains/SCF) x (O.OOS57) x (QSTPD)
P20^ Fed = Tons/hour, determined from plant data
Lbs/ton P20 Fed = (Ibs/hourj -^- (Tons/hour P205 Fed)
-------
EMISSION DATA
FARMLAND INDUSTRIES
1) Run Number
2) Date
3) Time Began
4) Time End
5) Barometric Pressure, In Hg
6) Meter Orifice Pressure Drop, in H^O
7) Vol Dry Gas, Meter Cond . Cubic Feet
8) Average Gas Meter Temperature, Deg F
9) Vol Dry Gas, S.T.P., Cubic Feet
10) Total H20 Collected, Ml
11) Vol H20 Vapor Collected,, S .T.P . ,. Cu.Ft .
12) Stack Gas Moisture, Percent Volume
13) Assumed Stack Gas Moisture, Pet Vol
14) Percent C02
15) Percent 02
16) Percent CO
17) Percent N2
18) Percent Excess Air
19) Molecular Weight of Stack Gas, 'Dry
20) Molecular Weight of Stack Gas, Stk Cond.
21) Stack Gas Specific Gravity
22) Avg. Square Root (Vel Head) , in H20
23) Average Stack Gas Temperature, Deg F
24) Avg. Square Root (Stk Temp x Vel Head)
25) Pitot Correction Factor
26) Stack Pressure, in Hg , Absolute
27) Stack Gas Vel, Stack Cond, F.P.M,
28) Stack Area, Sq . Feet
29) Effective Stack Area, Square Feet
30) Stack Gas Flow Rate, S.T.P., SCFMD
31) Net Time of Test, Minutes
32) Sampling Nozzle Diameter, Inches
33) Percent Isokinetic
34) Fluoride - Water Soluble, MG
35) Fluoride - Total, MG
36) Fluoride - Water Soluble, GR/SCF
37) Fluoride --Total, GR/SCF
38) Fluoride - Water Sol ., GR/CF , STK CND .
39) Fluoride - Total, GR/CF, STK CND.
40) Fluoride - Water Soluble, LB/HOUR
41) Fluoride - Total, LB/HOUR
43) Fluoride - Water Sol., LB/TON P20s FED
44) Fluoride - Total, LB/TON P205 FED
1
3/2/72
9:00
11:30
30.1
0.31
44.316
80
43.791
52.1
2.47
5.3
6
0.1
20.6
0.1
79.2
3973
28.84
28.26
0.97
0.969
106
23.044
0. 83
30.14
1825
9.38
9.39
15307
120
.250-. 125
74.2
16.7
16.83
0. 0059
0.0059
0. 0052
0.0053
0.7739
0.7739
0.0383
0. 0383
2
3/2/72
11:38
13:40
30.05
1.30
84.301
99
80.62
106.6
5.05
5.9
6
0.1
20.6
0.1
79.2
3973
28.84
28.2
0.97
0.954
108
22.725
0.83
30.09
1846
9.39
9.39
15307
120
.250-. 125
116.5
18.5
18.6
0.0035
0.0035
0.0081
0.0081
0.4592
0.4592
0.0227
0. 0227
3
3/2/72
13:50
15:11
30.05
0.95
47.562
90
46.139
49.9
2.37
4.9
6
0.1
20.6
0.1
79.2
3973
28.84
28.31
0.98
0.722
106
17.123
0.83
30.09
1820
9.39
9.39
15307
76
.250-. 125
117
18.5
18.67
0.0062
0. 0062
0. 0055
0. 0056
0.8133
0.8133
0.0403
0. 0403
***S.T.P. «-+DRY, 70 DEGREES F, 29.92 INCHES MERCURY***
^Velocity calculated using fan curve
-------
FLOW CALCULATIONS
Pressure Drop Across Fan 24-25" H?0
From Fan Curve:
Flow, 140°F, 31.3" Hg, saturated (18.8%) 20,400 CFM
Flow, Dry ( 16565 CFM
Flow, Standard Cond.(Dry, 70°F, 29.92" Hg) 15307 SCFM
Run 1:
Flow . 15307 SCFM
Flow, stack Conditions 17136 ACFM
Velocity, Stack Conditions 1825 ACF
Run 2:
Flow 15307 SCFM
Flow, Stack Conditions 17335 ACFM
Velocity, Stack Conditions 1846 - ACF
Run 3:
Flow 15307 SCFM
Flow, Stack Conditions 17092 ACFM
Velocity, Stack Conditions 1820 ACF
-------
APPENDIX B
FIELD DATA
-------
Field data sheets are included in this section for the
three tests conducted at the scrubber outlet at Farmland.
These data sheets are presented as follows:
Preliminary velocity traverse sheet.
Meter data sheet for fluoride determination - Test 1.
Meter data sheet for fluroide determination - Test 2.
Meter data sheet for fluoride determination - Test 3.
Velocity traverse data (taken from meter data sheets) - Test 1
Velocity traverse data (taken from meter data sheets) - Test 2
Velocity traverse data (taken from meter data sheets) - Test 3
Orsat Analysis
-------
GAS VELOCITY AND VOLUME DATA
VELOCITY TRAVERSE DATA
Point
1
2
3
4
*s
* (o
7
8
2>
/O
n
12.
Position
Inches3
0.°>
2.8
4,<3>
7.4
;o,4
/4.7
E6-ft
S/.O
34.2
36.G
3,34
40.6
Total
Average
Reading, Ap
"H2°
o.-fc
0,4-0.7
O-4 -*-O.6
O- 3 -*-G>.5
O- 1 -»-
V
105
Stack Inside Dimensions 4-1,5"" |,p.
Stack Area, A = 9. 4. sq. ft.
5
Barometric Pressure, P, =
Stack Gage Pressure =
Stack Abs. Pressure, P =
s
Test No. PRELIMINARY
Location RAFPMIAMD 1ND,
OUTLET
4-0.
_ "Hg
"H2°
"H?0 + P,_ =
Stack Gas Temp., T
o
\O5
13.6^
>F + 460 4
b
'R
Molecular Weight of Stack Gas, M =
b
V = 174 V^Ap Cp V Ts x 29.92
C
V = /74C-88) .
O
x 29 ft/min;::.
M ^
Q, Volume ='
3i3,2.4
ft/min. x
= 30 7£
9>,4 sq. ft. =
Q , Standard Volume at 70°F and 29.92 "Hg(Wet Basis)=
Q x 530 x PC
= 17.7 x
x.
T 29.92
s
= Qtr x (100-W)/100 =
2-74 ><2>
a) From outside of port to sampling point.
S
Pitot tube
Manometer
Thermometer
o -\c>'
O/&L.
W.B.= IOO°F
.= ]05°F
20
-T ROOF
XXX KX X x
x x x. x.
80'
10'
Data Recorder R.(J-,
Date -3-I-7Z.
ACROSS FAN =
PEDCo - ENVIRONMENTAL
SUITE B ATKINSON SQUARE
CINCINNATI. OHIO 4524-6
j." H20 513/771-4330
0.&5" @
-------
PARTICULATE FIELD SAMPLING METER DATA
Plant FARMLAND IND.
Run Number
I
Location ?HOS. ACID OUTLET
Date 3-2.-7Z Time ?:-
Operator CT.P.
Sample Train Number
Meter Number
AH@
Filter No.
Barometric Pressure, in. Hg ~*>o,\
Assumed Moisture, % <^
Assumed Meter Temp., °F
Stack Gage Pressure -fo.S
Probe Tip Diameter, in. '/^ '
52., I
Condensate Collected, ml.
'C1 Correction Factor O.78
Point
1
Z.
3
4-
5
£
7
8
5
10
1!
IE.
E.ND
Total
Avg.
Time
Min.
ip
*
t
izo
\0
Dry Gas Meter
Volume
ft3
Vm
424. &86
4^7.64
431. /fc
434,45
437,57
440.5^
445,£^
450-49
454,37
45fl,ZL£
4-6>2, £4
4£5.5&
4fc^.oo4
4.4. 3;^
Inlet
Temp.
OF
72
-75
(50
SZ
«4-
sa '
82.
ft4
fift
°3O
<3Z
9E-
65
Outlet
Temp.
op
6>8
&9
7O
72-
74
75
76
ra
7A
80
RO
BO
7S
Velocity
Head Ap
"H2°
0.7/
O.75
-0.73
'O.66
0,5ft
0-2-3
.30
,^D
1,50
.40
,ZO
1,1(0
Orifice AH
"H2°
o.z.4
o, as
0. Z'4
o.zis
o. le
n.66
O. E85
0.35
0.32
cO.BO
o.-zfe
O.E4
Pump
Vacuum
"Hg
5
5
S
5
S
9
5
5
5
5
5
S
Filter
Temp.
op
,
.
,
,
Impinger
&£
Go-nd-efts-e-r
Temp. , °F
57
57
57
- 58
55
Sfe
&o
G>0
63
64
64
64
Stack Gas
Temp. , °F
T
s
IOA
05
10ft
OB
05
IO5
IO5
105
105
' 105
105
105
Leakage Rate @ |5 "Hg =
cfm
STOPPED TEST TO CHANGE TO V&" N'OS^
V-s = 43.316, x-x-fii =4Z.6
PEDCo-ENVIRONMENTAL-
SUITE 8 - ATKINSON SQUARE
CINCINNATI. OHIO 45246
513 / 7 7 1-4330
NOTE; SA^APLEP BELOW ISOKIMETIC RATE FOR FIRST FIVE POINTS
- DUS TO ERPOp. |N READIfv'fr
-------
PARTICULATE FIELD SAMPLING METER DATA
Plant FARMLAND IND.
Run Number g_
Location PHOS. ACfD O/JT/-ET
Date 3-2.-7Z Time /).' 3ff /,'
Operator Q..F.
Sample Train Number
Meter Number
AH@
Filter No.
Barometric Pressure, in." Hg
Assumed Moisture, % &
Assumed Meter Temp., °F g,Q
Stack Gage Pressure -ho. 3
Probe Tip Diameter, in. v^."A
-"H2°
Condensate Collected, ml. I Ob. Co
'C1 Correction Factor . 0.75
Point
!
2.
25
4-
.S
(o
7
£
<3
IO
!
Z,
END
Total
Avg.
Time
Min.
10
i
7^
IZO
10
Dry Gas Meter
Volume
ft3
Vm
4£9./!6
4-77. Z!
4S7.-35
4 "57, /£
i5ofe.3B
.5/4.2.1
513.57
k532. S6
537, 5> 9
542,12.
545.39
5"49..6I
553,5iD?>
84,3e>|
Inlet
Temp.
OF
102.
I \O
HA
12-2.
\ZC>
1 1 2.
130
IO4
IOO
9^
«5^
^<6
/306
|O9
Outlet
Temp.
op
/54
^35"
a*
91
01
<^0
92
5»O
«e
8B
R7
Aft '
IC63
P.O
Velocitv
Head Ap
"H2°
0.43
^.P>3
O.7I
o.fcl
0.43
o. 18
r .30
1 ,70
1.6x3
/.4^ .
/ *3O
\.2.O
Orifice AH
"H2°
1,5?.
2, SO
z.ao'
i.eo
l,.7,5
0.56
4.00
0.~^?5
n,34
.0,3(*
<*b
kfr
&7
b&
6>°>
70
Stack Gas
Temp . , ° F
T
105
\OS
105
ro7
1 10
no
/Oft
IOR
!OA
I OR
105
l<55
Leakage Rate @ 15 "Hg = o
cfm
TEST TO CKANCTE TO
= 84351
SCF
- 85.4! ecF
PEDCo- ENVIRONMENTAL
SUITE 8 ATKINSON SQUARE
CINCINNATI. OHIO 45246
513 / 7 7 1-433O
-------
lant FARMLAND IMP.
PARTICULATF, FIELD SAMPLING METER DATA
Filter No.
Run Number
Location PHOS , ACI D OUTLET
Date 3-Z.-72. Time/.'-S'O-- 3,' //
Operator Gr.p. '
Sample Box Number
Meter Box Number__
AH@ ' |.3s
Barometric Pressure, in. Hg 3o,o5
Assumed Moisture, % 4
Assumed Meter Temp., °F
Stack Gage Pressure +o.s
Probe Tip Diameter, in.
Condensate Collected, ml.
'C' Correction Factor
j /6"
o,-7&
-"H2°
Point
!
2L .
S. _
4
5
&
7
8
3>
10
M
12.
_ EMD
To-h^l
AVT
Time
Min.
10
^
MX>J^
ZiA
7£
Dry Gas Meter
Volume
ft3
553,&0fe
^foE.3ft
571- 2.5
51^>. Z.V
5/?^5.5| .21
534 . 87
53S. 54
601.16,8
4-7.56^
Inlet
Temp.
oF
°)6
04-
lOfc
5>ft
3ft
2>0
ftfo
87
76.7
%
Outlet
Temp.
oF
84
85
ft5
84
84
S^,
8Z-
ft3
670
S4
Velocity
Head Ap
"H2°
O.64
0.59
0-42.
0.2.7
0.21
aos
I.2LO
1.60
Orifice AH
"H2°
2. .00
l.ftS
1. 40
0,ft3
0.6A
0.17
O.Z6
0.35
7.60
O^5
Pump -
Vacuum
"Hg
L2_
12.
10
7
6
5
5
5
Box
Temp.
op
.
.
Impinger
.err
Condenser
Temp. , °F
fo^
76
fo8
70
/^B
^8
68
67
Stack
Temp.
oF
105
105
105
IO5
105
\OS
\OP>
no
Leakage Rate @ 15 "Hg =
CFM
TEST TO CHANGE TO''/s'7^OZ:2.L-E
STOPPED ALL TESTIN& WITH 44 MIN. LEFT-PROCESS SHUT
PEDCo- ENVIRONMENTAL.
SUITE 8 ATKINSON SQUARE
CINCINNATI. OHIO 45346
-------
GAS VELOCITY AND VOLUME DATA
VELOCITY TRAVERSE DATA
Point
1
2.
3
4
S
6
7
6
S
10
n
11
Total
Averac
Position
Inches3
fe
Reading, Ap
"H2°
0.11
O.HS
0.13
Q.(o(a
0.5&
o.za
,30
,foO
.50
.40
,20
.to
-
^/Ap
-&M-3
.»(ofo
.ftSM-
.01^-
,nfc2.-
.s?°\
l.l^-O.
i.ZfcS".
1,22.5".
Mftf
1.0^ S"
I.OM-CI
u^a^f
^fc0!
T °F
s
\os
\05
ioe>
ice
I OS
I OS
IQS"
105
\os
lOuC
I OS
lOb
\^^
\0(*
Test No.
Location
Stack Inside Dimensions
Stack Area, A = S,3°
U-US "
OUTLET- ?HOS. l\C(D
Barometric Pressure, P, =
Stack Gage Pressure =
Stack Abs. Pressure, I
4- O.S
_sq. ft.
30. 10 "Hg
"H2°
= 4-O.S
Stack Gas Temp.,
|06?
^ "H20 +
13.6
'F + 460 =
"Hg
Molecular Weight of Stack Gas, M =
V = 174 \fbp Cp V T x 29.92 x 29n ft/min.
s P M
, s
V =
s
Q, Volume =' 3 "3^*7 ft/min. x
sq. ft. =
cfm
V
Standard Volume at 70°F and 29.92 "Hg (Wet Basis) =
Q x 530 x P
= 17.7 x
Qs = Qw
T.g 29.92
(100-W)/100 =
3Q.Hf =
a) From outside of port to sampling point,
Pitot tube "s" TVPti
Manometer
Q-IQ"
Thermometer
Data Recorder
Date 3-2-
6.F.
PEDCo - ENVIRONMENTAL-
SUITE 8 . ATKINSON SQUARE
CINCINNATI. OHIO -45246
513/771 -A33O
-------
GAS VELOCITY AND VOLUME DATA
VELOCITY TRAVERSE DATA
Point
I
2
3
V
5"
6
"7
8
q
16
II
11
Position
Inchesa
Total
Average
Reading, Ap
"H20
O.Ltf
0,P>3
(5, HI
(5, M
0, U-3
o, \P>
1,30
Mo
f.feO
I.U6
1.30
1,2.0
-
-
\MP
,7^0
,qii
if?1*'*
,T8i
.(/;$&>
,W
1,1146
1.303
I.TfoS
i.t&y-
\.\<40
1,0^5
I.^Z
,^S^-
T °F
s
IDS"
16?
IO_S
10")
110
no
fo8
106
106
168
los-
10^
\1SM
107
Stack Inside Dimensions 4-|,S " <|
Stack Area, A^ = c/,l>c; sq.
Barometric Pressure, Pv = 30.0
Stack Gage Pressure = 4 6-.S '
Stack Abs . Pressure, ? = 40,5"
Stack Gas Temp., T_ = | 01 °
Molecular Weight of Stack Gas, M
V = 174 \/Ap Cp V T^ x-29.92 x
s s p
s ' ' \pk 1 x 30'.oci/~
Q, Volume =' 3>^>b"0 ft/min. x
Q , Standard Volume at 70°F and
Q x 530 x Ps = 17.7 x
Test No. 2.
Location 0uiLCT- PH-oS
>
ft.
S "Hg
"H00
"H20 + Pw = 30 lO6) "Hg
13.6 D
F + 460 = £{01 °R
s ^-
29' ft/min.
Ms
Zi - ^i.S'O
T G ~"
^,3^ sq. ft. = 3/, Ub7 cfm
29.92 "Hg(Wet Basis) =
T 29.92 r-^T " 'w
o ~^ *
Qe = 0.. x (100-W)/100 =
a) From outside of port to sampling point.
Pitot tube "s" THpg
Manometer o-/0"
Thermometer
Data Recorder
Date ^-Z
PEDCo- ENVIRONMENTAL
SUITE 8 ATKINSON SQUARE
CINCINNATI. OHIO -*5246
5 1 3 / 7V 1 -4 33O
-------
GAS VELOCITY AND VOLUME DATA
VELOCITY TRAVERSE DATA
Point
I
I
3
4
S
4 I, "T
Stack Area, A = c
Barometric Pressure, P, =
Stack Gage Pressure = + (
Stack Abs. Pressure, P = -+
sq. ft.
,0 £ "Hg
"H2°
"H20 + P.
13.6
"Hg
Stack Gas Temp., T =
F + 460 =
'R
Molecular Weight of Stack Gas, M = Q.^
V = 174 \/Ap* Cp V T x 29.92 x 29' ft/min.
S P.
. _. i
V =
s
Q, Volume =' 7533
:andard
Q x 530
Qw, .Standard Volume at 70°F and 29.92 "Hg(Wet Basis) =
Qs =
x (100-W)/100 =
a) From outside of port to sampling point
Pitot tube "j" T^PE
Manometer
Thermometer
O-lO"
"Pi AU
Data Recorder
Date B-I-
PEDCo - ENVIRONMENTAL
SUITE 8 ATKINSON SQUARE
CINCINNATI. OHIO 45346
513 /7V 1-4330
-------
PEDCo-ENVIRONMENTAL
SUITE 8 ATKINSON SQUARE
CINCINNATI, OHIO 45346
513 / 77 1-433O
COMBUSTION GAS ANALYSIS
Plant
Comments
Location
V L.Q. ( Ptios.
Operator
Test
No . . Time
/ 2; to
%(co2)
< ai
%(o2)
3.0*6
% (CO)
^<5, 1
NOTE: Analyses are on a dry basis when performed by Orsat.
% EXCESS AIR- 100(%02-0.5%CO) %!
= 100-(%02 + \
0.264(%N2) - (%02 - 0.5%CO)
%C02 + %CO)
15
-------
ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park, North Carolina 27711
Reply to '
Attn of:
Date: 12-21-72
." Summary of Fluoride Analysis
To:
R. Neulicht, EMB, IRL
This memorandum is in response to your request for a brief
summary of our SPADNS-Zirconium Lake procedure for determination
of fluoride in stack emission samples.
Samples received in our laboratory are filtered through
fluoride free paper filters to yield water soluble and water insoluble
portions. The water insoluble particulate collected on the filter
is rinsed throughly to be sure that all water soluble fluoride is
rinsed through. The water soluble fraction is distilled from sul-
furic acid to a maximum temperature of 180 C. If chloride is suspected
in the sample Ag So is added to the still. -SPADNS solution is added
to an aliquot of the distillate and the absorbance is read at 570 nm.
The concentration of the sample is determined from a calibration curve
prepared from standard fluoride solutions. It is very imoortant 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 CAU, and then lusuJ wlLli l^CII. 1'l.c
fusate is dissolved with distilled water, neutralized with dilute H So ,
distilled and analyzed as described for the soluble portion.
Paper filters containing particulate are cut into small pieces,
suspended in a slurry of CAO, evaporated to dryness and ashed prior
to the alkali fusion and distillation.
If you have any questions about this procedure, let me know.
Howard L. Crist
Chief, Source Sample Analysis Section
SSFAB, QA'i ;;'.'.
cc: R. E. Lee
-------
Phosphorous"3 Pentoxide ' Determination
. r
Colorimetric Molybdovanadophosphate Method
An aliquot of sample is hydrolyzed in the presence of HC1 and
HNO acids by boiling almost to dryness..
The sample is cooled to room temperature, transferred to a
250 ml volumetric flask and diluted to volume with distilled water.
A 20 ml aliquot is transferred to a 100 ml volumetric flask, 20 ml
of molybdovanadate reagent is 'added and the flask is diluted to
volume.
The absorbance of the yellow color is determined after ten min-
utes at 400 nm. The concentration of phosphorous pentoxide is de-
termined from a calibration curve prepared with standard solutions.
-------
APPENDIX D
TEST LOG
-------
March 1, 1972
P.M.
2:30 Arrive at plant and meet with Bill Mahaney.. Proceed
to sampling site and make physical measurements.
;
3:15 Make preliminary pitot traverse and wet and dry
bulb measurements. Flow is very erratic.
3:30-5:00 Complete setting up equipment and make preliminary
calculations.
5:10 Leave plant.
March 2, 1972
A.M.
7:45 Arrive at plant
8:00 Check velocity readings again. Carefully check
pitot tube, tubing, and manometer system for
possible leaks. Everything is all right. Stack
gas flows are still erratic and high on far side
of stack and very low at center. Conclude that flow
is erratic because of tangential fan inlet location
and since there are no disturbances in the stack
the flow remains tangential all the way through stack,
-------
8:30-9:00 Complete setting up train and leak testing.
9:00 Start first run use 1/4" nozzle for first seven
points and 1/8" nozzle at last 5 points.
(
10:00 Scrubber water and feed, product, and recycle acid
collected by Bill Mahaney of Farmland.
Primary scrubber water discharge pH 2.6
Secondary scrubber water discharge pH 2.1 Temp.94°F
Scrubber water inlet pH 2.6
11:30 Complete first run (1/2 hour lost due to changing
nozzle). NOTE: First five points had been sampled
at too low a rate due to error in reading nomograph.
Concluded that this wasn't too serious since no
particulate is present.
11:38 Being Run 2. Second set of impingers was prepared
during Run 1. Therefore only had to rinse probe
with water and attach to new set of impingers.
P.M.
1:00 Take scrubber water and process samples
1:40 Complete Run 2
1:50 Start Run 3
-------
2:00 Orsat analysis
2:10 Opacity of exit gas is 0, and no odor observed
when stack gas is sniffed. Appears to be very low
concentration of fluorides.
3:00 Scrubber water discharge 88°F. Take water and
process samples
3:11 Process begins to shut down because of ruptured
filter. Discontinue sampling.
Process will not be able to restart for 8 to 10
hours. Decide to leave site.
4:30 Leave plant.
-------
APPENDIX E
PROJECT PARTICIPANTS
-------
Project Participants and Titles
PEDCo-Environmental Specialists, Inc.
Richard W. Gerstle, P.E., Engineer in Charge
Robert S. Amick, Engineer
Gene Forte, Technician
Joe Gieger, Technician
Environmental Protection Agency
J. Rom - In charge of sampling
John Reynolds - In charge of process data and liaison.
Farmland Industries Inc.
Bill Mahaney
------- |