TEST NO. 72 - CI - 1
W. R. GRACE AND COMPANY
WET PROCESS PHOSPHORIC ACID
BARTOW, FLORIDA
JANUARY 4 - 5, 1972
<>iirinniim>iittil
2324 S. W. 34th STREET / GAINESVILLE/FLORIDA 32601 / PHONE 904/372-3318
-------
TEST NO. 72 - CI - 1
W. R. GRACE AND COMPANY
WET PROCESS PHOSPHORIC ACID
BARTOW, FLORIDA
JANUARY 4 - 5, 1972
Test Conducted By:
Environmental Engineering, Inc.
Contract # CPA - 70 - 82
-------
TABLE OF CONTENTS
Page
List of Figures II
List of Tables H
Introduction • -j
Summary of Results -j
Process Description 2
Process Operation 8
Location of Sampling Points 9
Sampling and Analytical Procedures 14
Appendixes 19
A. Emission Calculations and Results
B,. . Field Data
C. Standard Analytical Procedures
D. Laboratory Results
E. Project Participants
-------
List of Figures
Page
1. Flow Diagram and Sampling Stations 3
2. Scrubber Design 7
3. Port Location - Station C 11
4. Port Location - Station D 12
5. Port Location - Station E 13
6. Moisture Sampling Train 17
7. Fluoride Sampling Train 18
List of Tables
Page
1. Summary of Results - Station C 4
2. Summary of Results - Station D 5
3. Summary of Results - Station E 6
4. Sampling Points 10
II
-------
INTRODUCTION
Under the direction of the Environmental Protection Agency, Environmen-
tal Engineering, Inc., conducted emission tests at the W. R. Grace and Company
wet process phosphoric add plant located 1n Bartow, Florida. Three test runs
were conducted on January 4-5, 1972. The purpose of the test was to obtain
data to be used by both the Industrial Studies Branch and the Performance
Standards Branch of the EPA.
*•
Measurements for soluble and Insoluble fluorides were made in the Inlet
ducts and outlet stack of the crossflow scrubber. The Inlet leading from the
attack tank and the Inlet leading from the filtration system were sampled.
Numerous grab samples of the process reactants and products were taken and
analyzed for fluoride and P20g content. A schematic diagram of the process
flow and all sampling locations is given in Figure 1.
Pertinent results of the test are listed in Tables 1 - 3; complete test
results are given in Appendix A.
SUMMARY OF RESULTS
Although no major problems were encountered with process operation, some
of the filter pans were not dumping dry. This condition had existed for some
time before the tests were begun. Other operating conditions were typical of
normal operation. There were no apparent irregularities in the actual sampling
or analytical procedures.
"• For runs one, two, and three, respectively, the scrubber Inlet from the
-------
attack tank showed fluoride emissions of 0.033, 0.182, and 0.187 Ib/ton
PpOg fed. Emissions at the Inlet from the filtration system were 0.031,
0.025, and 0.024 Ib/ton P205 fed, while at the scrubber outlet to the atmos-
phere, total fluoride emissions were 0.004, 0.008, and 0.004 Ib/ton P205 fed.
From this data, scrubber efficiency was calculated to be 93.3%, 96.0%, and
97.7% for runs one, two, and three, respectively.
Tables 1 - 3 give a complete summary of stack gas conditions, sample
volumes collected, and fluoride emissions.
PROCESS DESCRIPTION
The first step 1n the basic process involves mixing phosphate rock,
sulfuric acid, and water to form a reaction slurry.
The basic reaction is the acidulatlon of tricalcium phosphate in the
rock with sulfuric acid and water to produce phosphoric acid and calcium sul-
fate dihydrate (gypsum). The reaction is:
Ca3(P04) + 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 sili-
cates in the digesting slurry to form fluosiliclc acid as follows:
CaF2 + H2S04 + 2H20 + CaS04 ' 2H20 + 2HF
6 HF + S10, •*• H0SiF, + 2H90
e. c. o L
The fluosiHcic acid in turn can decompose:
v H2S1F6 + heat and/or Add •+ S1F4 + 2 HF
2.
-------
Stack Sample
( ) Grab Sample
Water from Pond
H2S04
Phosphate
rock
Pond Water
(A)
_f\
Attack
To Atmosphere
t!
Scrubber
(B)-
To Pond
_f\
Filtration
To Pond
Barometric condenser hot wells, and
miscellaneous
Evaporation
Water
to
Gypsum
to
Pond
(cake)
Schematic Flow Diagram with Locations of Sampling Stations
W. R. GRACE
Wet Phosphoric Acid
Phosphoric
Acid
Figure 1
3
-------
TABLE 1
SUMMARY OF RESULTS
FLUORIDES
STATION C
Scrubber Inlet from Attack Tank
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
i _- . . . , .
r luonae, 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 P00,. Fed.
c t>
Fluoride, total, Ib/ton PpOr Fed.
Scrubber efficiency,' %
1
1-4-72
29.92
r
29.92
10.4
150
5813
78.951
106.95
106.95
0.020
0.020-
0.016
0.016
1.01
1.01
0.033
0.033
2
1-5-72
29.92
29.92
28.2
151
4867
97.143
837
837
0.132
0.132
0.082
0.082
5.51
5.51
0.182
0.182
3
1-5-72
29.92
29.92
27.2
154
5010
83.965
603
737
0.108
0.132
0.067
0.082
4.62
5.65
0.153
0.187
Dry, 70°F., 29.92 inches Hg.
-------
TABLE 2
SUMMARY OF RESULTS
FLUORIDES
STATION D
Scrubber Inlet from Filtration System
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?05 Fed.
Fluoride, total, Ib/ton P^Or Fed.
Scrubber efficiency, %
1
1-4-72
30
29.68
6.6
103
11686
77.449
47.7
47.7
0.009
0.009
0.008
0.008
0.92
0.92
0.031
0.031
2
1-5-72
30
29.68
6.2
103
11231
77.631
39.165
39.755
0.008
0.008
0.007
0.007
0.71
0.75
0.025
0.025
3
1-5-72
30
29.68
6.9
105
11407
78.343
38.1
38.1
0.007
0.007
0.006
0.006
0.71
0.71
0.024
0.024
Dry, 70°F., 29.92 inches Hg.
-------
TABLE 3
SUMMARY OF RESULTS
FLUORIDES
STATION E
Scrubber 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
Vol. dry gas @ S.T.P. , SCF
Fluoride', water soluble, mg
Fluuriue, 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 PpO,- Fed.
Fluoride, total, Ib/ton P?05 Fed.
Scrubber efficiency, %
1
1-4-72
30
30
4.9
93
15981
55.057
3.6
3.6
0.001
0.001
0.001
0.001
0.13
0.13
0.004
0.004
93.3
2
1-5-72
30
30
5.2
94
16832
63.498
7.2
7.2
0.002
0.002
0.002
0.002
o.z^
0.25
0.008
0.008
96.0
3
1-5-72
30
30
5.2
96
16825
63.282
3.535
3.609
0.001
0.001
0.001
0.001
0.12
0.12
0.004
0.004
97.7
Dry, 70°F., 29.92 inches Hg.
-------
FUME SCRUBBSR: -WEr PROCESS PHOSPHORIC Acto
GAS TO
AM AMD
STACK.
GAS TO
GAS
. FLOW
PLA.KJ
«ao
Fiqure 2
-------
The reactor consists of a series of tanks with the slurry alternately
overflowing and underflowing from one compartment to the next. The multl-
compartment design allows temperature and agitation to vary throughout the
reaction sequence as slurry redrculates through the tank arrangement. The
addulation or digestion step 1s a highly exothermic reaction requiring con-
siderable apparatus for cooling. A vacuum flash cooler maintains temperature
1n the reactor and degasifies the recirculated slurry of dissolved air, car-
bon.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 byproduct 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% P-,0C.
e. D
The crossflow 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 1n the secon-
dary scrubbing section.
PROCESS OPERATION
Run 1 was conducted from 2:15 p.m. to 4:15 p.m. on January 4, 1972, on
WRG's "V" train phosphoric acid plant. This test Involved three sampling points
(2 Inlets and one outlet). Process operation was normal except that some filter
pans were dumping wet. This condition had existed for several days.
-------
Less than optimum filtration continued throughout Run II, which was be-
gun at 9:00 a.m. on January 5. Other process conditions were essentially
normal. No. 1 and 2 evaporators were brought on stream at the beginning of the
run, thereby doubling the production rate of 54% acid. With all four evapora-
tors running, the production of fluosiliclc acid was also Increased.
Scrubber conditions changed slightly during Run II. The booster water
pump discharge pressure decreased from 42 psig during Run I to 40 psig just
prior to Run II. This was caused by reduced pond water header pressure. Pres-
sure drop through the scrubber remained constant at 5" H«0 during Run II.
The third run got underway at 12:00 p.m. the same day. Process conditions
remained basically the same as for Run II except that evaporation rates were
increased slightly.
LOCATION OF SAMPLING POINTS
The sampling sites and number of traverse points were selected as per
"Method I - Sampling and Velocity Traverses for Stationary 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. The suggested number of traverse points per dia-
meter was used where possible without sampling within one inch of the inner wall.
Figures 3 through 5 are schematic diagrams of the stack configuration near
the sampling location, and the sampling points traversed during the emission tests.
9
-------
TABLE 4
DESCRIPTION OF SAMPLING POINTS
Sampling Point Sampling Point Number of Stack Diameter
Description Identification Traverse Points (Ft.)
Attack tank effluent
Filtration effluent
Scrubber outlet
C
D
E
6
20
6
1.72
2.70
3.9
-------
Inner Stack Diameter = 20.75 in.
Sampling Port
>20D
Sampling
Point
1
2
3
4
, 5
6
Distance From
Inner Wall (in.)
1
'3
6
14 5/8
17 3/4
19 3/4
FIGURE 3
LOCATION OF PORT AND SAMPLING POINTS
STATION C, W.R. GRACE
-------
6 1/2'
In;, r Stack Diameter = 32.4 in.
9 1/2'
Sampling Port
Sampling
Point
1
2
3
4
5
- 6
7
8
9
10
11
12
13
14
15 '
16
17
18
19
20
Distance from
Inner Wall (in.)
1 1/8
1 15/16
2 13/16
3 3/4
4 23/32
5 27/32
7 1/16
8 15/32
10 7/32
12 3/4
19 11/16
22 3/16
23 15/16
25 11/32
26 9/16
27 11/16
28 21/32
29 19/32
30 15/32
31 1/8
FIGURE 4
LOCATION OF PORT AND SAMPLING POINTS
STATION D, W.R. GRACE
12
-------
>4D
29'
L
Inner Stack Diameter = 47 in.
G
Sampling Port
\ /
FAN
Sampling
Point
1
2
3
4
5
. 6
Distance From
Inner Wall (in.)
2 1/16
6 7/8
13 7/8
33 1/8
40 3/32
44 15/16
FIGURE 5
LOCATION OF PORT AND SAMPLING POINTS
STATION E, W.R. GRACE
13
-------
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 test's 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 through the fourth impinger were placed
in an 8 ounce polyethylene container. The samples were held by EPA
personnel for further analyses.
Field data sheets are contained in Appendix B.
B. Preliminary Velocity Determination
Method 2 of the above mentioned Federal Register was used as a guide
v in determining the preliminary stack gas velocity for each source tested.
The major difference was that only the maximum and minimum velocity heads
14
-------
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 carryover. 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 parameters necessitated
additional adjustments to maintain an isokinetic flow rate. Nomographs were
used to aid in the rapid adjustment of the sampling rate. The traverse points
were selected to maintain at least one inch from the inner stack wall.
15
-------
.After each run, the liquid volume in the first three impinqers 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 in-
to polyethylene containers. During some runs the different sample
fractions were placed in separate containers, while during others, all
of the recovered sample was placed into one container.
D. Liquid and Product Grab Samples
Periodically during each test run, grab samples of the raw mate-
rials, finished product, and scrubber liquid were taken, and the tem-
perature 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. Field data sheets are included in Appendix B.
E. Laboratory Analysis Procedures
Water soluble fluorides were done by a sulfuric acid distillation
followed by the SPADNS-ZIRCONIUM LAKE METHOD. Water insoluble fluorides
were first fused with NaOH followed by a sulfuric acid distillation then
by the SPADNS-ZIRCONIUM LAKE METHOD.
P205 analysis of the stack effluent was done by EPA personnel. All
other PpOg analyses were done by plant personnel.
For more details of exact method used see Appendix C.
16
-------
<%-,
1. Heated Glass Probe
2. Glass Connector
3. Ice Bath
4. Midget Impinger With
5. Midget Impinger With
5. Midget Impinger, Dry
7. Midget Impinger, Dry
3. Flexible Sample Line
9. Vacuum Gauge
10. Main Control Valve
11. 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
17
-------
1. Stainless Steel
2. Heated Glass
3. Glass Connector
4. Ice Bath
5. Impinger with
6. Impinger with
7. Impinger, Dry
8. Impinger with
9. Filter Holder
10. Thermometer
11. Flexible Sample Line
12. Vacuum Gauge
13. Main Control Valve
14. By-Pass Control Valve
15. Air Tight Vacuum Pump
16. Dry Test Meter
17. Calibrated Orifice
18. Inclined Manometer
19. S-Type Pi tot Tube
/>•«£ ,
,^
/r
19
?1 Nozzle -£
'robe ^j^., .
if*7
TOO ml H«0 (Modified Tip) \
100 ml H,0 (Standard Tip) t
(Modified Tip) *
180 grams Silica Gel (Modified Tip)
with No. 1 Whatman Filter
_ ,., 1
. I
V^- »
~> 1
t !\
* !
*- 3 i 1
" 1 1 '
'- L
L » i r
J li
L
N
i
•4
i
j
j
|
\
5
^
if
M
Yf
y I
^ c
1 *
-~3
TT
i i
IP
i i ,
i
!
6
•••«•*
Figure 7
FLUORIDE SAMPLING TRAIN
18
-------
APPENDIX
19
-------
APPENDIX A
Emission Calculations and Results
-------
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 zer
TS - Stack temperature, °R
TM - Meter temperature, °R
_
H - Average square root of velocity head, -/inches
. A,H - 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 13.6]
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 airj %
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)
VSTPD = (17.71 x (VM) x (PB + AH_ ) 4- TM
13.6
VT = (VWV) + (VSTPD)
W = (VW)-v-(VT)
FDA = (1.0) - (W)
FMOIST = Assumed moisture fraction
MD = (0.44 x % CO ) + (0.32 x % 02) + (0.28 x % N2) H- (0.28 x % CO)
MS = (MD x FDA) + (18 x W)
GS = (MS)-r- (28.99)
EA = '[(100) x (% 02 - ^^)] -r- £(o.'266 x % NZ) - (% 02 - 1^2) ]]
j
U = (174) x (CP) x (H) x v'CTS x 29.92)-7-(GS x PS)
QS = (£) x (AS)
QD = (QS) x (FDA)
QSTPD = (QD) x (. 53°) x (ii)
29.92 TS
PISO = (o.oo267 x VC x TS) + (Po x TS x VM-l-TM) -;- (Time x U x PS x AN)
Fluoride Emissions:
MG = Milligrams of fluoride from lab analysis
Grains/SCF = (0.01543) x (MG) -j- VSTPD
Grains/CF, Stack Cond. = (17.71) x (PS) x (FDA) x (Grains/SCF) -~ (TS)
Lbs/hour = (Grains/SCF) x (0.00857) x (QSTPD)
P205 Fed = Tons/hour, determined from plant data-.
Lbs/ton P20 Fed = (Ibs/hour) -^- (Tons/hour'P20 Fed)
-------
FLUORIDE EMISSIONS
-------
SOURCE TEST DATA
. TEST NO.
NAME OF FIRM W. R. Grace
NO. OF RUNS 3
LOCATION OF PLANT Bartow, Florida
T'fPE OF PLANT Wet Phosphoric Acid
CONTROL EQUIPMENT
SAMPLING POINT LOCATION Station "C" -- Inlet to the Scruhhpr
POLLUTANTS SAMPLED Fluoride
DRUH NO.
2)DATE
3) TIME BEGAN
4)7'.i:..T EHD
S)EA1WMETRIC PRESSURE, "Hg ABSOLUTE -
»)MEfER ORIFICE PRESSURE DROP, "I^O 7
7)yOL DRY GAS @ MUTER CODDITIOUS, ff*
8)AVERAGE GAS METER TEMPERATURE, °F
S) VOL DRY GAS Q S.T.P.*, ft3
xQV/'OT/lL 7/20 COLLECTED, ml
11) VOL IMTEfl WIPOfl COLL. @ S.T.P., ft3
.12)ST4CK C/15 MOISTURE, ^VOLUME
13) ASSUMED STACK GAS MOISTURE, ^VOLUME
16)% CO
iv;^ .fo
18)% EXCESS AIR
1S)MOLECULAR 1-/T. OF STACK GAS, DRY
20)UOLECULAR WT..OF STACK GAS, STACK COND.
21) STACK GAS SP. GRAVITY, REF. TO AIR
22)AVG~VVr;L. HEAD OF STACK GAS , "H20
2 3 )/i VERA GE STA CK GAS TEMPERA TURE , °F
21) PI TOT CORRECTION FACTOR
2S)STACK PRESSURE, "Hg ABSOLUTE
2OST4CA' GAS VEL @ STACK COND., fpm
27 )5 TACK AREA, ft2
28)STACK GAS FLOW RATE @ S.T.P., scfm
2 9 ) /Vi'T TIAf/i1 OF TSS T , m i n .
3 0 ^SAMPLING 1,'OZ ZLE DIAMETER , in.
31) PERCENT ISOKINETIC
32)FLUORIDE - WATER SOLUBLE, MG
33)FLUORIDE - TOTAL, MG
3H)FLUORIDE - WATER SOLUBLE, GE/SCF '.
35)FLUORIDE - TOTAL, GEfSCF
36)FLOURID'£J - WATER SOL. GR/CF STK COND.
3T)FLOURID£ - TOTAL GR/CF STK COND.
38)FLUORIDE - WATER SOLUBLE, LB/HOUR
2 o M>£ nn o T n r _ TOTAL LB /EOVP
M)FLOURIDE - WATER SOL. LB /TON P205 FED.
H2)FLUORIDE - TOTAL, LBS/TOU P205 FED.
1
1/4/72
14: 18
15: 58
29.92
2.02
81.085
87
78.951
193.5
9. 17
10.4
1850
0
28. 99
27.85
0.96
.0.873
150.4
0.83
29. 9
3178. 9
2. 35
5013
100
0.25
93.7
106.95
106.95
0. 0203
0. 0203
0. 0158
0.0158
1.0119 •
1. 0119
I *
0. 0335
0. 0335
2
1/5/72
9 :00
11 :A5
29. 92
2.29
97.605
75. 5
97. 143
803. 0
38. 1
28. 2
1050
0
20. 99
25.09
0. 89
00 o
. 8 0
151 . R
0. 83
29. 9
3320
2. 35
4067
120
0. 25
114.7
837
037
0.1321
0.1321
0. 082
0.082
5. 5083
5.5083
0.1824
0. 1824
3
1/5/72
12: 00
14:05
29. 92
1.63
86.296
86.9
83.965
661.9
31. 37
27. 2
3000
0
28.99
26
0. 9
0007
. o •) /
154
0.83
29.9
3392. 1
2.35
5010
120
0.25
96 . 3
603
737
0.1076
0. 1315
0. 0675
0.0025
4.6203
5.647
0. 153
0. 187
0 r
o o no
-------
SOURCE TEST DATA
. TEST NO.
NAME OF FIRM W. R. Grace
NO. OF RUNS 3
LOCATION OF PLANT Bartow, Florida
TYPE OF PLANT Wet Phosphoric Acid
CONTROL EQUIPMENT
SAL1PLTUG POINT LOCATION Station "D" — Inlet to the Scrubber
POLLUTANTS SAMPLED Fluoride
DRUM NO.
2 )DATE
3) TIME BEGAN
U)2T/./2 END
S)BAR01-1ETRIC PRESSURE, "Hg ABSOLUTE '
b) METER ORIFICE PRESSURE DROP, "I^O
7) VOL DRY GAS @ METER CONDITIONS, ft5
B) AVER AGE GAS METER TEMPERATURE, °F
9) VOL DRY GAS Q S.T.P.*, ftj
10) TOTAL 11-20 COLLECTED, ml
11) VOL IMTER VAPOR COLL. @ S.T.P., ft3
.12)S1MC# (MS MOISTURE, ^VOLUME
13)ASSUUED STACK GAS MOISTURE, % VOLUME
14)% C02
16)% CO
17)2 11 2
18)? EXCESS AIR
1V)MOLECULAR 1-/T. OF STACK GAS, DRY
20)MOLECULAR VT..OF STACK GAS, STACK COND.
2DSTACX GAS SP. GRAVITY, REF. TO AIR
22)AVG'l/~Vl-JL. lit AD OF STACK GAS , "H20
231AVERAGE STACK GAS TEMPERATURE ,° F
24)PirOi" CORRECTION FACTOR
2S)STACK PRESSURE, "Hg ABSOLUTE
26)S2VtC7i: GAS VEL % STACK COND., fpm
27) STACK AREA, ft2
28)8TACK GAS FLOW RATE @ S.T.P.f scfm
23) NET TIME OF TEST, min.
3Q)SAMPLIi-lC NOZZLE DIAMETER, in.
3 1 ) PERCENT ISOKINE'TIC
32)FLUORIDE - WATER SOLUBLE, MG
33)FLUORIDE - TOTAL, MG
WFLUORIDE - WATER SOLUBLE, GR/SCF
35)FLUORIDE - TOTAL, GR/SCF
3G)FLOURIDE - WATER SOL. GR/CF STK COND.
3DFLOURIDE - TOTAL GR/CF STK COND.
3B)FLUORIDE - WATER SOLUBLE, LB /HOUR
3Q)FLUORIDE - TOTAL, LB /HOUR
HDFLOURIDE - WATER SOL. LB/TON P205 FED.
*2)FLUORIDE - TOTAL, LBS/TON P205 FED.
1
1/4/72
14:20
16:20
30
10 O
• \ j O
79.552
87.7
77.449
116. 3
5.51
6.6
9
0. 2
2
1/5/72
9 :05
11 :05
30
1.33
78.054
76.1
77.631
109
5.17
6.2
670
0.2
20.5 |20.5
0 |0
79.3
3452
79. 3
3452
28.85 |28.85
28.13 J28.17
0.97 |0.97
-0.665 J0.637
1-03.1 |103.4
0.83 |0.83
29.68 (29.68
2322.9 J2223.7
5n f\
. 73
11686
120
0.25
93. 5
47.7
47.7
0. 0092
0. 0092
0, 008
0.008
0. 9248
0.9248
0. 0306
0. 0306
5*7 o
• / O
11231
120
0.25
97. 5
.39. 165
39. 755
0. 0077
0. 0078
0. 0068
0. 0069
0.7437
0.7549
' 0.0246
0.025
3
1/5/72
12:00
14 :00
30
1. 38
80. 261
86.3
78. 343
121.9
5. 78
6.9
670
0.4
20.4
0
79. 2
3058
28. 88
28.13
0.97
n R R o
u . D o /;
105
0.83
29.68 ,
2280. 5
5*7 O
» / O
14 | , X\ n
1407
120
0^\ r-
. 2 b
96.9
38. 1
38. 1
0. 0073
0. 0073
0. 0063
0. 0063
0.7146
0.7146
• 0. 0237
0. 0237
-------
SOURCE TEST DATA
. TEST NO.
NAME OF FIRM W. R. Grarp
110. OF PUNS 3
LOCATION ,:-F PLANT Bartow, Flprida
TYPE OF PLANT Wet Phosphoric Acid
CONTROL EQUIPMENT Fume Scrubber
SAMPLING POINT LOCATION Station "E" -- Outlet frnm thp Srnihhpr
POLLUTANTS SAMPLED Fluoride
DRUN NO.
2)DATE
3) TIME BEGAN
H)TIME END
S)DAHOMETRIC PRESSURE, "Hg ABSOLUTE
b)METER ORIFICE PREFCU^v DROP, "I^O '
T)VOL DRY GAS Q 't'JTER COUDITIOUS, ft3
8 ) A VERA GE GA S . M£ TET. TEMPERATURE , ° F
9) VOL DRY GAS Q S.T.P.*, ft3
10) TOTAL U^O COLLECTED, n,l
11) VOL WATER VAPOR COLL. $ S.T.P., ft3
.12)STACK GAS MOISTURE, ^VOLUME
12)ASSUMED STACK GAS MOISTURE, ^VOLUME
14)2 C02
15)2 02
16 )§ CO
1 7 ) y ii "
18)| EXCESS AIR
19)l-10LECULAR UT. OF STACK GAS, DRY
20)MOLECULAR VT..OF STACK GAS, STACK COND.
2DSTACK GAS SP. GRAVITY, REF . TO AIR
22)AVG-VVEL. HEAD OF STACK GAS , "H20
22) AVERAGE STACK GAS TEMPERATURE ,° F
2H)PITOT CORRECTION FACTOR
2S)STACK PRESSURE, "Hg ABSOLUTE
2^) STACK GAS VEL @ STACK COND., fpm
27 )S TACK AREA, ft2
2B)STACK GAS FLOW RATE Q S.T.P.f scfm
23)iIET TIME OF TEST, mitl.
20)SAUPLIt'lG NOZZLE DIAMETER, in.
31) PERCENT ISOKINE'TIC
22)FLUORIDE - WATER SOLUBLE, MG
23)FLUORIDE - TOTAL ,MG
2H)FLUORIDE - WATER SOLUBLE, GR/SCF
25)FLUORIDE - TOTAL, GR/SCF
2&)FLOURIDE - WATER SOL. GR/CF STK COND.
2DFLOURIDE - TOTAL GR/CF STK COND.
2Q)FLUORIDE - WATER SOLUBLE, LB /HOUR
33)FLUORIDL' - TOTAL, LB /HOUR
HDFLOURIDE - WATER SOL. LB/TOH P205 FED.
*2)FLUORIDE - TOTAL, LBS/TON P205 FED.
1
1/4/72
14:15
16:15
30
0. 58
56.293
84.1
55.057
60.1
2. 85
4. 9
1200
0
28.99
28. 45
0. 98
Oil O C
. <4 2 b
' '
0. 83
30
1457. 8
1f\ f\ r*
2.05
15981
120
0. 25
1f\ A r\
U X • 2.
3.6
3. 6
0. 001
0. 001
0. 0009
0. 0009
0. 1349
0.1349 -
0. 0045
0. 0045
2
1/5/72
•» f *•* / i ft
9 : 00
11 : 00
30
0. 76
63.593
73 . 2
63.498
74.2
3. 52
5. 2
500
0
28.99
28.41
0. 98
0.45
94.2
0. 83
30
1541.7
12. 05
16832
120
0. 25
110. 8
.7.2
7.2
0.0017
0. 0017
0. 0016
0. 0016
0, 2515
0.2515
0.0083
0.0083
3
1/5/72
12:00
14:00
30
0. 76
64.278
80. 8
63.282
73. 8
3.5
5.2
50
0
28.99
28.41
0. 98
Oti r
. " 3
96.4
0. 83
30
1547.2
12.05
16825
190
U. ^ ',/
0. 25
1A f\ C
10,5
3.535
3.609
0. 0008
0. 0009
0. 0008
0. 0008
0. 1221
0. 1247
0.004
0. 0041
I
70
29.92 in.
-------
SCRUBBER EFFICIENCY
-------
Flow: 5813 (jSCFM)
Total
Fluorides: 1.01 (#/HR)
11686
0.92
W. R. Grace
Wet Acid
Run 1
Pond
o
-0
17499
1.93
Scrubber
Efficiency: 93.3%
Pond
H2°
To atmosphere
15981 .
0.13
-------
Flow: 4867 (uSCFM)
Total
Fluorides: 5.51 (#/HRj-
11231
0.75
-O
16098
6.26
W. R. Grace
Wet Acid
Run £
o
Pond
H2°
Scrubber
Efficiency: 96.0%
Pond
To atmosphere
16832
.25
-------
Flow: 5010 (USCFM)
Total 4.62 (#/HR)
Fluorides:
11407
0.71
16417
-o
5.33
W. R. Grace
Wet Acid
Run 3
o
Pond
H00
Scrubber
Efficiency: 97.7%
Pond
H£0
To atmosphere
16825
.12
-------
APPENDIX B
Field Data
-------
PRELIMINARY MOISTURE DETERMINATION
-------
PRELIMINARY CHECK FOR STACK GAS
MOISTURE CONTENT AND SPECIFIC GRAVITY
Date
Sample Time
suet
Barometric Pressure
* *
Moisture Content -— Method 1
Final Dry Test Meter Reading
Initial Dry Test Meter Reading_
Dry Test Meter Volume Sampled
Average Meter Temperature
Average Meter Vacuum __________
Average Meter Orifice A H
Sampling Rate
Barometric Pressure 9 Meter Orifice
Dry Gas Volume Sampled 3 70 °F, 29.92 "Hg_
Condensate Volume
Water Vapor Volume % 70 °F, 29,92 "Hg_
Moisture Fraction, HoO &» -
Moisture Content — ?-f°thod 2
Dry Bulb Temp. /$3 °F Wet Bulb Temp..
F Dew Point
Vapor Pressure Of K20 § DP
Moisture Fraction, H20__^
Stack Pressure
Fraction Of Dry Air, FDA_
Specific Gravity
Dry Molecular Weight, Kd = [o.^4(^C02')] + JO^C
Molecular Weight S Stack Conditions, Ms = [^Md)
Specific Gravity (Referred to air), Gs = (Ms)
Jt-'
.Ft3
Pt3
."Hg
"HoO
LPM
Ft3
ml
Fraction Of Dry Air. FDA
"Kg
|o.28(^N2 + Col) =
+ [7l8)x(H20)]
(28.99) =
-------
Plant_
Date /~4
PRELIMINARY CHECK FOR STACK GAS
MOISTURE CONTENT AND SPECIFIC GRAVITY
Stack >
***
Sample Time /CT
Barometric Pressure
'Hg
Moisture Content -- Method,!
Final Dry Test Meter Reading
Initial Dry Test Meter Reading
Dry Test Meter Volume Sampled
Average Meter Ternparature
Average Meter Vacuum
Average Meter Orifice A H
Sampling Rate
Barometric Pressure <§ Meter Orifice
Dry Gas Volume Sampled & 70 °F, 29.92 "Hg_
*
Condensate Volume
Water Vapor Volume '§ ?0 °F, 29,92 "Hg_
Moisture Fraction, H20 Q_
Moisture Content — "°thod 2
Dry Bulb Teap. /&/ JF Wet Bulb Temp.
Dew Point Ternp._
FtJ
Ft3
"He:
_LFM
J'Hg
nl
Fraction Of Dry Air, FDA £&_
Vapor Pressure Of H20 3 DP A
Moisture Fraction, H20 Qo O^
."Hg
Stack Pressure ^/Q &B "Hg
Fraction Of Dry Air, FDA_
Specific Gx'avity
Dry Molecular Weight, Md = [O.^^CO,^] +^.32(^022J +(0.28(^N2 + Co]] = .
Molecular Weight @ Stack Conditions, Ms =[(Md)x(FDA)] + [?18)x(H2Ci)[ =
*
Specific Gravity (Referred to air), Gs = (Ms) -f- (28.99) =
-------
PRELIMINARY CHECK FOR STACK GAS
MOISTURE CONTENT AND SPECIFIC GRAVITY
Stack ftf&T P/?**. fM
Barometric Pressure
"Hg
Moisture Content — Method 1
Final Dry Test Meter Reading
Initial Dry Test Meter Reading
Dry Test Meter Volume Sampled
Average Meter Temperature
Average Meter Vacuum
Average Meter. Orifice A. H
Sampling Rate
2.
Barometric Pressure 3 Meter Orifice
Dry Gas Volume Sampled $ ?0 °F, 29.92 "Hg_
Condensate Volume
Water Vapor Volume @ ?0 °F, 29,92 "Hg_
Moisture Fraction, H20 £%> &> $%
Moisture Content — • Method 2
Dry Bulb Teap./flO °F V/et Bulb Temp.
°F Dew Point
Vapor Pressure Of H20 3 DP
Moisture Fraction, HoO 0
"Hg Stack Pressure
Fraction Of Dry Air, FDA
"HoO
_LPM
"Her
ml
Fraction Of Dry Air, FDA_
"Hg
Specific Gravity
Dry Molecular Weight, Hd = ^.W-(^C02^] +J0.32(^02M +|o.28(#N2 + CO)] =
Molecular Weight © Stack Conditions, Ms = [(M,j)x(FDA)] + j0.8)x(H2ol] =
Specific Gravity (Referred to air), Gs = (Mg) ~- (28.99) =
-------
FLUORIDE EMISSIONS
-------
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
Plant
Sampling Location COg|/^eg .
j ^^
.. i _ Run No,
Ag
|i>
Time End
Hg
, Gas Density F act or
Time Start
Sampling Time/Point(,_
DB_|£JL°F, WB_]4}°:
Moisturel&£XFDA_,:
Barometric Press^/^Hg. Stack Press2.9,?0'Hg
he a ther -C^'l/Qr Ld£t
Temp. £&*?, 1V/D ,W/S
Sample Box No, ^r Meter Box No._
Meter AHe/.fe&Pitot Corr. Factor. L
Nozzle Dia._,^5j-n., Probe Length ^
Probe Heater Setting
ft
Stack Dimensions: Inside Diameter
Inside Area
He i ght
V
Mat'l Processing Rate
Final Gas Meter Reading
Initial Gas Meter Reading
Total Condensate in
Moisture in Silica Gel
ft5
ft3
Silica Gel Container No.Jg^TFilter
Orsat: C02
02 _
CO _
N2 _
Excess
Air
Conducted by: /?.
-
Remarks:
£ t
Port and
Tr avers e
Point No.
f
•
A
£
!L
'%.-
Distance
from End
' of Port
(ft!)
.03
*-25"~
.^5
•^5^
Clock
Time
Too
an
/^13~
/42S
I43&
Gas Meter
Reading
(ft3)
C>£oS& 7
H\4, O
^Ll 7» 4
'
2 20*^
£2.3,6
• Stack
Velocity
Head
("H20)
\D LiJtoll
oA
(\$ft
£>. *\
Meter
Orifice
Press. Diff.
C'H20)
Calc,
I.OF;
l.o
i-o5
Actual
\t&£
LD
1 OS"
Stack Gas
Temp.
/
1S1U
1$$^
Gas Sample
Temp.@ Dry
Gas Meter
In
S^
r?7
$1
Out
S 7
#7
81
Sample
Box
Temp.
.„
^—
<= —
Last
Impirger
Test
33
S^>
£3
Vacuum
on
Sample
Train
("Hg)
'is
It
11
-------
fcort and
(Traverse
Point No,
Distance
from End
of Port
(in)
Clock
Time
Gas Meter
Reading
(ft3)
Stack
Velocity
Head
("H20)
Meter
Orifice
Press .Diff.
("H20)
Calc.
Actual
Stack Gas
Temp.
Gas Sample'
Temp «(§ Dry
Gas Meter
In
Out
Sample
Box
Temp,
Last
Impinger
Temp.
Vacuum
on
Sample
Train
2.
/I
__3_
3
.SI
.ft
St>
L&
3
_*£/_
^LL
/.Z1L
.ZZ.
£31;
37
&BO.
O^A.
€7
\Z7
f/
J?
s
s
1.4$
5
.0
f
27
$7.%n
2Zi!5
S'J
'3
6
O48
03s
z
3
b
I5SS
2£3.Q8f
S?/
-------
- '2
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
, /
Plant U-X Fv . ^ £A(!S
Sampling Location 6^4- ^£& AcwSfftT'lC*
Date J&±G
-WvlS Run No, 2u
Time Start tfl OO Time End //'05"
Sampling Tin
DB °F,
Moisture,/^
Barometric F
Weather
le/Point /2£? yyiZ^i, te<^%&**J^,
WB °F, VF @ DP "Pig
!,FDA ,G
'ress "Hg,
/^ />
is Density F
Stack Pre
:tx3uf
actor
ss "Hg
Temp. °F, W/D ,W/S
Sample Box No, Meter Box No. 4*
Meter AHS^j^Pitot Cor
Nozzle Dia. , ^6 in. , Pro
r. Factor
• *3
oe Length ^f- ft
Probe Heater Setting 3S~ /t>
Stack Dimensions: Inside
Inside
Height
Port and
Traverse
Point No.
/
/
/
/
2,
2.
&
Distance
from End
' of Port
(^
&g +
A ^/ ?\ • i
^S^t Jri
XN/7 *y "**
» CXt/ r
'2^
.25
,25
Diameter 2^.7^ in
Area 2. . 35" f &
ft
Clock
Time
FfiOO
ftfyS'
Olio
£><\15
d^JZO
Q
*^s*
"&5
Mat'l Processing
Final Gas M
Initial Gas
Total Conde
Moisture in
Silica Gel
Orsat: C02
02
CO
N2
Excess
Air
Rate
3ter Reading
Meter Readii
is ate in Imp
Silica Gel
Container No
^9^0 4 os ft'
ig ^9^ ^TZTD ft"
Lngers V S^S"" nil
|CJro S111
• StTlS" Filter No.?<2.(2^-
Test Conducted by: /f v £, , &JE} 1 LS-^A/
Remarks: _^!W^"-'
Meter
Orifice
Press. Diff.
0'H20)
Calc.
m
MS
/./\&
\.!B
\,lg
t / o
1 1 I O
\*1 £
/,<7
//?
S\ j 4^"-
«^-
mi^£__h^v_^
Stack Gas
Temp,
\$Q
I.^P
L5D
15"^
tS'o
ts'o
/^ ^
UJt ft J2^y\^j2y
T
-V^-,,_
-*v
^_3&
> x/uJ^r^ ^r *&&$&
Gas Sample
Temp.@ Dry
Gas Meter
In
7"?
?3
•73
73
93
11
Out
7-f
^^
7^
^4
74
7'T
Sample
Box
Temp.
«— .
— .
T~
"^.
—7
.*-»
Last
Impirger
Test
7f>
7O
7O
r?O
r?O
no
75
Vacuum
on
Sample
Train
("Hg)
£
^
(6
^2
9
/D
/^5
-------
[Port and
[Traverse
(Point No,
Stack
Velocity
Head
C"H20)
Stack Gas
Temp.
Distance
from End
of Port
(in)
Clock
Time
Gas Meter
Reading
(ft3)
Meter '
Orifice
Press,Diff,
("H20)
Gas Sample
Temp.@Dry
Gas Meter
TO
Sample
Box
Temp,
TO
Last
Impinger
Temp.
on
Sample
Train
Gale. Actual
3<=5> *' 1
31. J
-------
Plant_
Sampling LocationJ
«#"* /-*
Date sJ&sJ 5 Run No,.
Gainesville, Florida' 3/~/<7*^ /"
V.'e a th e r (y\J*LT \2
Temp. J5 °F, W/D ,W/S
Sample Box No. Meter Box No.
Meter iHSj^pJ^Pitot Corr. Factor
Nozzle Dia.j-jSyTjLn., Probe LengJ;h_
Probe Heater Setting
ft
Stack Dimensions: Inside Diameter
Inside Area_
Height
^^X6
Final Gas Meter Reading
Total Condensate in Impingers
Moisture in Silica Gel
ml
Silica Gel Container N
Orsat: C07
Li '• i i . i . . i .
gm
Filter No.4
02
CO
Excess
Air
Test Conducted by:
Remarks:
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.
("H20)
Stack Gas
Temp.
Gas Sample
Temp.@ Dry
Gas Meter
("F)
Sample
Box
Temp.
TO
Last
Impiiger
Test
Vacuum
on
Sample
Train
("Hg)
-------
Clock
Time
Stack
Velocity
Head
C"H20)
Meter
Orifice
Press.Diff
C"H20)
Stack Gas
Temp.
Gas Sample
Temp.@Dry
Gas Meter
TO
Sample
Box
Temp,
Port and
Traverse
Point No
Distance
from End
of Port
(in)
Gas Meter
Reading
(ft3)
Last
Impinger
Temp.
Vacuum
on
Sample
Train
-------
Plant
'. eg.fte.&
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
Sampling Location
| /$/?3L Run No,
^JL-4*
Time Start.
Time End
Sampling Time/Point
°F, WB
DB
°F, VF @ DP
» 7/ ,Gas Density Factor
'Hg
Moistun#0£,nP
Barometric Press3£)_"Hg, Stack Press
Weather &/M$.$Lt
Temp, %5* cF, W/D , W/S
Sample Box No
Meter AHS/
Nozzle Dia.
'Hg
Meter Box No.
Pitot Corr. Factor
in. , Probe Length
Probe Heater Setting _
3
.ft
Stack Dimensions: Inside Diameter ^
Inside Area
Height^
Mat'l Processing Rate
Final Gas Meter Reading
Initial Gas Meter Reading
Total Condensate in Impingers
Moisture in Silica Gel
Silica Gel Container No.
Orsat: C07
m
Filter
N2
Excess
Air
Test Conducted by:
&1GL
'i^M^L.
Port and
Traverse
Point No.
Distance
from End
of Port
(in.)
Clock
Time
Gas Meter
Reading
(ft3)
Stack
Velocity
Head
("H20)
Meter
Orifice
Press, Diff.
("H20)
Calc. I Actual
Stack Gas
Temp,
Gas Sample
Temp, 8 Dry
Gas Meter
In
Out
Last
Impirger
Test
Vacuum
on
Sample
Train
C"Hg)
3
±
La
£3-
u&~
104
« v*k
-------
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,
("H20)
Gale. Actual
Stack Gas
Temp.
Gas Sample
Temp. @ Dry
Gas Meter
TO
In
Out
Last
Impinger
Temp.
Vacuum
on
Sample
Train
Z-
/
*•
/3
/r
n
IS
t?
•&
IS
/o//
ion
/.OZ3
/04/
&§&.
&S3,
/01L
4£
IMS, 4
f
o
I01U
m—,
2WMJ
/OS'
11
2K.
$>£!
fd
.&>,
/
xs"
-------
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
\
Plant /A) •> pC- (•T'.f^-FV't^jgf
Sampling Loc
Date / /&
ation ST/37Tt O^ 0
/7J5U. Run No. *7
Time Start £) *?D £ Time End / ( ', O 3
Sampling Tin
le/Point £y-Flv*>& <3.Opk l^-Ot
KB"""* CF, VT @ DP . "Hg
Moisture £'7% ,FDA ££3 ,Gas Density Factor -f 7
Barometric Press J?0 "Hg,
feather
6 &/-&*.<£
Stack Pre
ss^^'Hg
Temp. 7^ °F, Iv/D .W/S
Sample Box No, JV— Me
Meter AH@ /»',
ter Box No. 1
H Pitot Corr. Factor .<2-$J5
Nozzle Dia0M;i5"in. , Probe Length 4~ ft
Probe Heate;
" Setting
Stack Dimensions: Inside
Inside
Height
Port and
Traverse
Point No.
/
z
3
i
s
&
Distance
from End
of Port
(in.)
^
fY^1 y
~VY?y
V y
ff
-X»
-^_
Diameterv^^ >y in
Area ^5** 7'-2. ft 2
ft
Clock
Time
^?^<
Of /i
0? /7
^1-^-3
(9*7^
& JP\
p^"
^^
£r
Gas Meter
Reading
9"^- 30^
^^f/.fDO
7 f ^C ^
Mat'l Processing
-
Final Gas M
Initial Gas
Total Conde
Moisture in
Silica Gel
Or sat: C02
02
CO
N2
Excess
Air
Rate
3 ter Reading J Q &?&> + 3^> •*/ ft-5
Meter Reading ^ & # . ZOO f t^
nsate in Impingers / fc> ml^
Silica Gel^
Container No
. Z
?^'£~23?.&rA5gm
^Fss
^
.s^?"/ Filter No72.-^>3*«<^
Meter
Orifice
Press. Diff.
("H20)
Calc.
» 9 /
A 05"
1. 1
*tfl
Q»°K
Actual
. ?/
l*o£
/< I
* ^ 1
c-75"
Hb
-^r/t?Mo
U^\cJsr/^
s^w ^ /
*
Stack Gas
Temp .
Ito1~
J61^
/& t>
10 *L*
/&£?t
Gas Sample
Temp.@ Dry
Gas Meter
In
"IS
1<;
is
~a>
Out
?$
f<
7^
T^fo.
^
4
/a
3
^s^ 43
Last
Impirger
Test
i<
75
^T
?S—
/^y
Vacuum
on
Sample
Train
("Hg)
^t_l?_
3.>5
B.fl
&*£
*$*@
-------
Port and
Traverse
Point No,
7
/o
/*-
JV
Distance
from End
of Port
(in) .
L
Clock
Time
09 4 f
Gas Meter
Reading
(ft3)
Stack
Velocity
Head
C"H20)
o^LU
/o//
704 /
13&3L
f
iO&L^
Meter
Orifice
Press, Diff,
("H20)
Calc.
Jb*&
Actual
Ojlp
Stack Gas
Temp.
Gas Sample
Temp. @ Dry
Gas Meter
In" I Out IS^-P
Last
Impinger
Temp.
_3
-Z.
1-7
L^LA2t
i /I ^\i 7 /^ /«>i
23;
Vacuum
on
Sample
Train
SJ
3.0
AT
ff>
S>0
?/
-------
Plant
U3 .
R,,
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
Mat'l Processing Rate
Sampling Locati<
Date ll5|7:
Dn ^S"Tft TX o f\i £hy
!L» Run No. ^"3
Time Start /2.00 Time End /t^'f)O
Sampling Time/Point ^'W-v^*lOjafc"~ i^ofc-f
DB y— °F, WB
* 9F, VF @ DP __^- "Hg
Moisture_^J_%,EDA9d»2> >Gas Density Factor
Barometric Press ^C)"Hg, Stack Press29.&£ "Hg
Weather OU^AQ^x%
Temp. 7^-°F, W/D " ,W/S
Sample Box No,
Meter AH@_]V
Nozzle Dia.
"^^ Meter Box No.' $
74 Pi tot Corr. Factor O**?^
• SjS'in. , Probe Length -4* ft
Probe Heater Setting
Stack Dimensions: Inside
Inside
Height
Port and
Traverse
Point No.
1
±>
J?
4
*r
£
Distance
from End
'of Port
(in.)
X
^
*
^
^
/>,
^
Diameter <32T» 11 in
Area s5^7;2^. ft^
Clock
Time
1&i@Q
l^cfa
!%'(¥'&
f$,\f$
(&j4
v-
Gas Meter
Reading
(ft3)
&&• -2,^
l&*8
fjt ^
i #.< Vtf
%/L*b£
fts c4#
Stack
Velocity
Head
C'H20)
X.
* %£'
* fc^^J
' &*} , ^^f
fl* t~~' O
Final Gas Meter Reading /^& ' ^LS* ft3
Initial Gas
Total Condej
Moisture in
Silica Gel
Orsat: C02
02
CO
Excess
Air
Meter Readir
us ate in Imp]
Silica Gel^
Container No
O.4
ig e? p « j2^T* ft
ingers /O^/ ^ ml
-« *— / /
i^6> «242.-6>-
\$Aw
<2©7 Filter No .73-0^
2.0&4
o
7f .2*
Test Conducted by: 3~* T^,~,\\rt r-
Remarks : ^i
Meter
Orifice
Press. Diff.
C'H20)
Calc.
/o?'2"
^o
}.^]g
f*~) /*7
v»/^Cj>
Actual
/ /^
*£.0
1 ^6
* 77
c^iAj
/\ft jp^rcx-A.O
^ ,. lx) iCL-^<>fer'
'
vO J.-V-H
1jSi_, \C_!L>-^— * "vV" »
— • i
Stack Gas
Temp.
TO
tfl£
fog
/d£~
fO^
Gas Sample
Temp. 8 Diy
Gas Meter
TO
In
$7
$fa
B
fit
•&&
Out
J?^
5^^-
g^
^3
o^i
Sampl^
T^iL.
/£
&
tfL>
A
^
Last
Impinjer
Test
(°F)
B?
1?
$2^
&l
Vacuum
on
Sample
Train
("Hg)
^7 ^\^
^^C **••-*
2^f
,lfjA-
2^°j&
3«5T
-------
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.
("H20)
CalCc Actual
Stack Gas
Temp.
Gas Sample
Temp. @ Dry
Gas Meter
TO
In
Out
Sample
5^ '7
Box
Last
Impinger
Temp.
Vacuum
on
Sample
Train
15
6
Q'5,3- }
fv
... <>•
10
3
I
6 ,35"
/./I,
$9
•#?
JS
v?
^7-7
S
fft
ft
3
1
7
/6
. go
lo sr
•
/OS"
15
/OS'
LJL
M
- IP
-------
Plant UJ g, .? HU& (toJtt i
vu, L\u,
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
Sampling Location g bxfec»^ £x j
Date I ///yy£ R1211 No. /
Time Start ^./f /^^Time End
Sampling Time/Point pl^f^ti
BB9_3 °F, IVB _°F, VF @ DP_
'Hg
Mo is ture jJLj; , FDAo. 7& Gas Density F act or
Barometric PressJ^c?_"Hg , Stack Press 3 O "Hg
Weather &itfl?v _
Temp. _ °F, W/D _ ,W/S __
Sample Box No, _ Meter Box No.
Meter AH@ _ Pitot Corr. Factor ^
Nozzle Dia. , ^"in. , Probe Length
Probe Heater Setting
ft
Stack Dimensions: Inside Diameter
Inside Area
Height
in
f t2
ft
\
/• r
Mat'l Processing Rate
Final Gas Meter Reading
Initial Gas Meter Reading 7 ' &•£_
?., ff £
ft5
Total Condensate in Impingers^
Moisture in Silica G
ml...
/£J gmr
Silica Gel Container No.3<23 Filter
Orsat: C0 <^>
°2
CO
N2
Excess
Air
/~v
Test Conducted by: (_>-.
Remarks:
Port and
Traverse
Point No.
Distance
from End
'of Port
(in.)
Clock
Time
Gas Meter
Reading
Stack
Velocity
Head
("H20)
Meter
Orifice
Press. Diff.
Calc. Actual
Stack Gas
Temp.
Gas Cample
Ternp.8 Dry
Gas Meter
Sample
Box
Temp .
In
Out
Last
Impinge r
Test
Vacuum
on
Sample
Train
("Hg)
Zl
O-
3*0
w
/O
3'*
A
v.Sl
G.58
^_a.
3.0
a 59
9 a
O./Z
SO
-------
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.
C°F)
Gas Sample
Temp, i? Dry
Gas Meter
TO
Sa
B
X
tol
Boh
Last
Impinger
Temp.
Vacuum
on
Sample
Train
.
f/
* //
-------
/~v
Plant &J£ G- YtiUHt fa&t ,
Sampling Loc
Date //\5/
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
&k&? / ,
Time Start Q,e° Time End (( ,G&
Sampling Time/Point 2Of**J», (rt;{&L/l&$8&'
DB °F.
KB °F, VF @ DP ^ '" "Hg
Mo i s ture jTj5 , FDA ,95^ Gas Density P
Barometric Press o?(2"Hg , Stack Pre
Weather (L^ <^V^H
actor
'ssjj^ "Hg
T^no */?) °F lv/D W'S
Sample Box No, Meter Box No. 1?
^
_ _ . _ .
&> %3
<^ ft
Area Ft 2
ft
Clock
Time
?.(^0
^/^
^ 7^
q3°
G ^0
CfgD
/&-&0
-
Gas Meter
Reading
(ft3)
^J/ 5 ^x.
/«^*^ * '
**y ^? n
/(p& " ^
^7J, ^
17& &
1$3. tf
rj®$ 9
W 7
Stack
Velocity
Head
("H20)
0,/S
o,/5
n,/ff
0.2-1
'Of ^..
_QiQo_
Remarks :
/•— >f^^».t
CT^ t -Jj <^-^z
*"
Stack Gas
Temp,
9^
93
93
G T3
9"^
95
Gas Sanple
Temp.g Dry
Gas Meter
In Out
73 7?
*7O ^*>
/ C< / e*-
-7«? -7a
fj r. "7^L
?3 7%
nd rfQ
y c^" ^7// y^2_
Sample
Bo^/
Teinp.
Xs!
5^p
^
^jTO
6"
/&
/£
&
/5
Last
Impinge r
Test
_-
t?o
?3
8^
^-'
—
Vacuum
on
Sample
Train
("Hg)
3-7
^(7
d/
?'^
J^q^
rt&
Lfr7
-------
Port and
Traverse
Point No.
5-
£
»
Distance
from End
of Port
(in)
•
Clock
Time
/o/o
/0-Z&
/o^O
/o */o
10 ^o
_j//i_^>
Gas Meter
Reading
(ft3)
Roo.4
/
L/ / ^~) £3
(j I *^
-------
Plant
£
L,,-
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
Sampling Location^
Date f IS 171
Run No,
Time Start \
o o
Sampling Time/Point ^p,
DB _°F, WB °F, VF @ DP
Hg
Mo i s turaS
% ,
, Gas Density F act or
Barometric Press3o"Hg, Stack Press 3 & "Hg
V.'e athe r (^/g^-*- 2et?~^_
°F, W/D ,W/S
Meter Box
Sainpie Box No,
Meter £H3 A*^? Pitot Corr. Factorj^jgJL
Nozzle Dia. /^in. , Probe Length
Probe Heater Setting
ft
Stack Dimensions: Inside Diameter
Inside Area ft2
Height ft
Mat'l Processing Rate
Final Gas Meter Reading
Initial Gas Meter Reading % 2.1.,
Total Condensate in Impingers £ £> ml
Moisture in Silica Gel^V^^ 3$$. % J3...Bg™
Silica Gel Container No,\jTcO Filter
Orsat: CO
02
CO
N2
Excess
Air
Test Conducted by
Remarks:
: (L
Port and
Traxrerse
Point No.
Distance
from End
of Port
(in.)
Clock
Time
Gas Mete
Reading
Stack
Velocity
Head
("H20)
Meter
Orifice
Press, Diff.
C"H20)
Calc, Actual
Stack Gas
Temp,
Gas Sample
Temp.@ Dry
Gas Meter
In
Out
ipj
Saj
B6x
T/knp.
Last Vacuum
Mpiiger on
Test Sample
Train
("Hg)
f
^7-3
0$
TL
79
&./£
^
-/V
o,
&.
32.
3
/
-------
Port and
Traverse
Point No,
S
6
,
Distance
from End
of Port
(in)
Clock
Time
//o
/2.0
/3o
A40
/5o
Q,oo
Gas Meter
Reading
(ft3)
?CS. <3
270- 7
#7£-0
2X/^
J ££.?£/
^j^d
Stack
Velocity
Head
C"H200
/^ £j
^.^o-
. ZL&
Meter
Orifice
Press. Diff,
C"H20)
Calc.
0$b
vrt5
-------
GRAB SAMPLE COLLECTION
-------
il-
655
&i
r/o.
557
5s/
5s/
Ran Mo,
y
M.
Dafe.
iwe.
. '3-0
foo
'/no
Poml"
fl
(rt fZ*
v r
77
PH
uon
.fe
-------
D^ f
B
Rim Mo,
a
3
o
inl"
-------
ftf
an Mo,
u
afe.
A !/=»
op
i t
'fa-
/
ci.O
-------
EPA Sawole. Ho.
Run Mo.
Daft
C-
p H
-------
1 <<
o5o
I-*::;"
EPA
*l
140.
P
Rtm Wo.
n,%!
Daf
A
Ti
iwe
Poinl"
r
-
, ° F
^Jt
1,9-5
A 7
-------
un M
Dafe
Pomi"
G-
(3-
as
Me-t^l
-------
YClC O
Ha v WU) __f/Cf.
w\ e> Mo.
un
Woo
/?
/?
?/
/9
a,/
Trace.
-------
G-YAC.fi. ftfiy /G
Mo,
:? 75
/// 0
a./
-------
— I
IU) /? Gr
O6 v A
ft »
feo.
373PO
73 PO
3 73
3 73
a.
Daft
n^
/0:50
L«S»
6
$7
c
-------
U) £ £
p
EPA
o.
3
Run Me.
Dafe
u^
_
7
-, o
(?
-A • v-
-------
__l :.
(j.)
fry fit-
Pi
r/o.
3 9% P/3
395
un Mo.
Dftfe,
,
-------
--H-
li /,/.)
3
3 7., /^
Dafe
/o,'5o
o •
.O
H
Fluorides
t & ***. i
M era i
-------
/p
C.
«*e. e.
3
Daf
/-SOX
/; /s
Poivxi"
?5
95
7
( O
. o
A
a s
-------
Piavr£_4L£
afe,
39/A)
3
3
/-S-73-
31 /Pb
3
AS- -7
IS', /B
r> 0 5
s,
z
/,#
A?
"froce.
-------
MA
c r-
C/
rf4
um . Mo,
3
/;
-------
//J p
3
afe
3
3
e.
/ : so
-------
/ • ii • Lrm
o.
3
Dafe
r
r
r
A
.- 9
ories
OQ.^1.--! ") /C. 7* /Cr.-^ -r',-.•'><-, /UJ rt A/o-^ 'tj-r^
-------
r ,'< r r
&,/.
MQ.
3
3
Dafc.
-' -5-*?^-
/-$-?!
Cr
© EP
i »"
=
//=?
<}'/' /
-------
APPENDIX C
Standard Analytical Procedures
-------
ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park, 'North Carolina 27711
A tin of: r> ,
J . Dale:- 12-21-72
Reply to
Aim of.
Subject: summary of Fluoride Analysis
°: 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 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 ox a siurry of CAG, ctuu Lhcji I^odi vith "A?". 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 sma.11 ni.scr
suspended in a slurry of CAO, evaporated to dryness anu asn^ci JJI.-I.L.
to the alkali fusion and distillation.
If you have any questions about this procedure, let me knov;.
Howard L. Crist
Chief, Source Sample Analysis Section
SSFAB, OAEML
cc: R. E. Lee
-------
Phosphorous Pentoxidc I:otermination
Colorimetric Molybdovanadc.ihosphate Method
An aliquot of sample is hydrplyg-•?. in the presence of HC1 and
HNO acids by boiling almost to dryne;-_-,.
*5 *
r ,
The sample is cooled to room terac. rature, transferred to a
250 ml volumetric flask and diluted to volume with distilled water.
A 20 ml aliquot is transferred to a 1C-'' ml volumetric flask, 20 ml
of molybdovanadate reagent is added sr-.C. 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 pento::ide is de-
termined from a calibration curve prepared with standard solutions.
-------
APPENDIX E
Project Participants
-------
PROJECT PARTICIPANTS AND TITLES
John Dollar Project Manager
Bill Demery Environmental Specialist
A.L. Wilson Environmental Specialist
George Allen Environmental Specialist
Bob Durgan Environmental Specialist
Eric Johnson Environmental Specialist
Russ Wicker Environmental Specialist
Tony Arroyo Computer Analyst
Jerome Rom • EPA
John Reynolds EPA
Roy Neulicht EPA
------- |