TEST NO. 73 - FRT - 10
C. F. CHEMICALS, INC.
RUN-OF-PILE TRIPLE SUPERPHOSPHATE
PLANT CITY, FLORIDA
SEPTEMBER 14 - 15, 1972
environmental engineering, inc.
2324 S. W. 34th STREET / GAINESVILLE/FLORIDA 32601 / PHONE 904/372-3318
-------
TEST NO. 73 - FRT - 10
C. F. CHEMICALS, INC.
RUN-OF-PILE TRIPLE SUPERPHOSPHATE
PLANT CITY, FLORIDA
SEPTEMBER 14 - 15, 1972
Test Conducted By:
Environmental Engineering, Inc.
Contract No. 68-02-0232
-------
TABLE OF CONTENTS
Page
List of Figures iii
List of Tables iii
Introduction 1
Summary of Results 3
Process Description 5
Process Operation 5
Location of Sampling Points 6
Sampling and Analytical Procedures 8
Appendices
Appendix A: Emission Calculations and Results
Appendix B: Field Data
Appendix C: Standard Analytical Procedures
Appendix D: Project Participants
n
-------
LIST OF FIGURES
Page
1. Schematic Process Diagram 2
2. Description of Sample Point 7
3. Fluoride Sampling Train 11
LIST OF TABLES
Page
1. Summary of Results 4
in
-------
I. INTRODUCTION
Under the direction of the Environmental Protection Agency,
Environmental Engineering, Inc. conducted emission tests at the
C. F. Chemical phosphate works in Plant City, Florida. On September
14 and 15, 1972, three two-hour test runs were performed on C. F.
Chemical's Run-of-Pile Triple Superphosphate production facilities.
The purpose of the test was to obtain data for the use of both the
Industrial Studies Branch and the Performance Standards Branch of
the EPA.
Measurements were made for soluble and insoluble fluorides at
the off-gas outlet to the atmosphere. In addition, grab samples of
the scrubbing liquids, the process reactants, and the process pro-
ducts were analyzed for fluoride and P205 content.
A schematic flow diagram of the process operation and the
sample location is presented in Figure 1. Pertinent test results
are listed in Table 1; complete results are given in Appendix A.
-------
Stack Sample Location
Rock Acid
cone
Pond Water
V
Scrubbers
t
To Atmosphere
|
Y
To Pond
/
Curing Den
s
Storage
Figure 1
Schematic Flow Diagram
C. F. Chemicals
-------
II. SUMMARY OF RESULTS
The plant was operating under normal process conditions during
all of the test runs. During the first test run, the plant shut down
for three hours due to a process malfunction. However, advance warn-
ing was given and the test was simply stopped prior to the shut down
and then resumed when the plant once again achieved normal operation.
No other test problems were encountered.
A complete summary of the stack gas conditions and the
fluoride emissions for each test run is given in Table 1.
-------
TABLE 1
SUMMARY OF RESULTS
FLUORIDES
C.F. CHEMICALS
R.O.P. OUTLET
Run No.
Date
Barometric pressure, inches Hg
Stack pressure, inches Hg
Stack gas moisture, % volume
Average stack gas temperature, °F.
Stack gas flow rate @ S.T.P?, SCFM
Volume of gas sampled @ S.T.P.
Fluoride, water soluble, mg
Fluoride, total , mg
Fluoride, water soluble, gr/SCF
Fluoride, total, gr/SCF
Fluoride, water soluble, gr/CF stk. cond.
Fluoride, total , gr/CF stk. cond.
Fluoride, water soluble, Ib/hour
Fluoride, total, Ib/hour
Fluoride, water soluble, Ib/ton P00C Fed.
C 0
Fluoride, total, Ib/ton PpOj- Fed.
1
9-14-72
30
30
4.8
101
60485
88.185
51
51
0.009
0.009-.'-
0.008
0.008
4.6
4.6
0.1
0.1
2
9-15-72
30
30
5.1
101
59578
86.482
53
53
0.009
0.009
0.009
0.009
4.8
4.8
0.1
0.1
3
9-15-72
30
30
. 5.3
103
58156
83.932
54
54
0.01
0.01
0.009
0.009
4.9
4.9
0.1
0.1
Dry, 70°F., 29.92 inches Hg.
-------
III. PROCESS DESCRIPTION
R.O.P. triple superphosphate is made by reacting 32 - 34 %
P20(. rock with phosphoric acid in a TVA cone-type continuous mixer
to yield a product containing 46% P^Oc . The principal reaction
is as follows:
Ca3(P04)2 + 4H3P04 + 3H20 -> 3CaH4(P04)2 H20
The cone discharges to a slowly moving belt called the "den"
on which the reactions continue until the slurry solidifies and is
discharged to the storage pile. The reactions go to near comple-
tion in the pile where, after sufficient curing, the product is
ready for shipment.
IV. PROCESS OPERATION
Three test runs were conducted; one on Thursday, September
14, from 2:30 pm to 4:30 pm and two on Friday, September 15, from
8:15 am to 10:15 am and from 12:00 pm to 2:00 pm. Plant operation
was normal for all three runs.
\
-------
V. LOCATION OF SAMPLING POINTS
The sampling sites and number of traverse points were
selected as per "Method I - Sample and Velocity Traverses for
Stationary Sources, Part 60, Subchapter C, Chapter 1, Title 40,"
Federal Register, No. 247-Pt. II-l.
Figure 2 is a schematic diagram of the stack configuration
near the sample location, and the sampling points traversed during
the emission tests.
-------
N
o-
T
20'
A.
J
80'
12
y » x
X » X
j
TRAVERSE'
POINT NO
I J
2, S
3,9
4V 10
5,11
6, 12.
Figure 2
SAMPLE PORT DESCRIPTION
7
' DISTANCE .
FROM INSIDE
WALL (FT)
0. Z6
O.6B
1.T7
4.23
-------
VI. SAMPLING AND ANALYTICAL PROCEDURES
Preliminary Moisture Determination
The preliminary moisture content of the stack gas was deter-
mined by wet bulb-dry bulb thermometry as referred to in the Federal
Register (Volume 36, Number 247, Part II, December 23, 1971).
Preliminary Velocity Determination
Method 2 of the above referenced Federal Register was used as
a guide in determining the preliminary stack gas velocity. The major
difference was that only the maximum and minimum velocity heads across
the stack area were determined so 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 determination.
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 con-
taining the filter holder directly following the glass probe. The samp-
ling 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 3
is a schematic diagram of the sampling train used.
8
-------
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.
After each run, the liquid volume in the first three impingers
was measured volumetrically and the silica gel was reweighed. The
impinger liquid, the filter, plus the water washings of the probe and
other sampling train components up to the silica gel were placed into
a single polyethylene container.
Field data sheets are included in Appendix B.
Liquid and Product Grab Samples
Periodically, during each test run, grab samples of the raw
materials, finished product, and scrubber liquid were taken, and
the temperature and pH were determined at the site. The samples
were split with the plant personnel so that comparative analyses
could be performed.
-------
E. Laboratory Analysis Procedures .
Water soluble fluorides were done by a sulfuric acid distil-
lation followed by the SPADNS-ZIRCONIUM LAKE METHOD. Water insoluble
fluorides were first fused with NaOH followed by a sulfuric acid dis-
tillation then by the SPADNS-ZIRCONIUM LAKE METHOD.
PpOg analysis of the stack effluent was done by EPA personnel
All other P^Or analyses were done by plant personnel.
For more details of exact method used, see Appendix C.
10
-------
Stainless Steel Nozzle
Heated Glass Probe
Glass Connector
Ice Bath
Ii.:pifiOer with 100 ml
Iinpiryjer with 100 ml
I:,.pinger, Dry
Ir.-pincjc-r with
19
M90
(Modified Tip)
)
(Standard Tip
(Modiflea Tip)
180 grams Silica Gel (Modified Tip)
Filter Holder with Mo. 1 Whatman Filter
Flexible Sample Line
Veci.:ii:n Gauge
Main Control Valve
By-Pass Control Valve
Air Tight Vacuum Pump
Dry Test Meter
Calibrated Orifice
Incli ned Manometer
S-Type Pi tot Tube
17
Figure 3
FLUORIDE SAMPLING TRAIN
-------
APPENDICES
-------
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.
AS'- 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, finches H20
A,H - Average meter orifice pressure differential, inches 1^0
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, fP~B + A H] 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 sampled, 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, Ibs/lb-mole (stack conditions)
GS - Specific gravity of stack gas, referred to air
EA - Excess air, %
Average square root of velocity head times stack temperature
U - Stack gas velocity, feet per minute
QS - Stack gas flow rate, cubic feet per minute (stack conditions)
QD - Stack gas flow rate, cubic feet per minute (dry conditions)
QSTPD - Stack gas flow rate, cubic feet per minute (STP)
PISO - Percent isokinetic volume sampled (method described in Federal Register)
-------
EQUATIONS FOR CALCULATING FLUORIDE EMISSIONS
VWV = (0.0474) x (VC)
VSTPD = (17.71 x (VM) x (PB + -^-H_ )-i- TM
13.6
VT = (VWV) + (VSTPD)
W = (VWV)-HVT)
FDA = (1.0) - (W)
FMOIST = Assumed moisture fraction
MD = (0.44 x % C02) + (0.32 x % 02) + (0.28 x % N2) + (0.28 x % CO)
MS = (MD X FDA) + (18 x W)
GS = (MS)-^- (28.99)
EA = [(100) x (% 02 - ^2^)] -r- Qo.266 x % N2) - (% 02 -
U = (174) x (CP) x (H) x 1/(TS x 29.92)-r(GS x PS)
QS - (U) x (AS)
QD = (QS) x (FDA) '
QSTPD = (pD) x (^1^) x (||)
PISO = (o.oo267 x VC x TS) + (PQ x TS x VM-i-TM) ~ (Time x U x PS x AN)
Fluoride Emissions:
MG = Milligrams of fluoride from lab analysis
Grains/SCF = (0.01543) x (MG)-r-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)
-------
S.QURQ& Z£
TEST 110 -
PLA11T - C.F. CrrpMICALS
SOURCE - P.O.P. OUTLET
TYPF. OF PLAI1T - R.O.P. '
CONTROL EQUIPMENT -
POLLUTANTS SAMPLED - FLUORIDE
NO OP P.VFS
PLANT CITY
- 3
2
3
5
6
7
8
9
11
12
13
15
NUMBER
)DATE
)TIME BEGAN
)TIME END
^BAROMETRIC PRESSURE, 111 EG
)METEH ORIFICE PRESSURE DROP, IK HG
)VOL DRY CAS, METER COUD, CUBIC FEET
)AVERAGE GAS METER TEMPERATURE, DEC F
)VOL DRY GAS, S.T.P. , CUBIC FEET
)TOTAL !!20 COLLECTED, ML
)VOL U20 VAPOR COLLECTED, S.T.P. , CU FT
)STACK GAS MOISTURE, PERCENT VOLUME
^ASSUMED STACK GAS MOISTURE, PCT VOL
)PER CENT C02
)PERCENT 02 '
)PERCENT CO
) PER CENT 112
)PERCENT EXCESS AIR
)MOLECULAR WEIGHT OF STACK GAS, DRY
)MOLECULAR WEIGHT OF STACK GAL
1 ___ 1
l_2Zl
1-lliifl ____ l-.aj.2S.
l-lJLi22
l_3o
L
1
LjJL-JiJL ___ 1
LJ
L_LJL1_ ____
L.92J3. _____ i_aa..j ______ LJJULJL ___ i
l_8o^is.s. ___ j.aa^iLa.2. ___ L_^_9_3IL__1
_
.'1 iL^t
L
L
7
JL.5
1
1
1
.1.
.1.
L_JL
-I
18
19
20
2DSTACX GAS SPECIFIC GRAVITY
22
23
L°
1 2
STK COHDljJW
-_i.
lL
1
1
1
1
!i
.1
20._95
"
J._2_8 J
25
20
27
28
29
30
31
32
33
35
37
38
40
42
43
)AVG SQUARE ROOT (VEL HEAD), IN H20
)AVERAGE STACK GAS TEMPERATURE, DEC F
)AVG SQUARE ROOT (STK TEMP*VEL HEAD)
)PITOT CORRECTION FACTOR
)STACK PRESSURE, IN HG, ABSOLUTE
)STACK GAS VEL, STACK COND, F.P.fi.
)STACK AREA, SQ FEET
)EFFECTIVE STACK AREA, SQUARE FEET
)STACK GAS FLOW RATE, S.T.P. , SCFMD
)NST TIME OF TEST, MINUTES
)SAMPLING NOZZLE DIAMETER, INCHES
)PERCE!-1T ISOKINETIC
WATER SOLUBLE, HG
TOTAL,
.1 °_--.9JL—
J[ 0 . G 0 G_
" i jroo".~8_~
' J_ 1G"."25l"
'j_~o~.~8ir
!iI3I°II_II
' J_"2~.~2~7~~
[ilLOJiZCIIIJ.IIi'-3-'"3-
a -1C Ann I "IT "7 r*
J^-Jl^SL L _ _fJ-: J^:
.1
.1
.1
I 60T85
' I fTo
' i T.-25
| TDD-^
1 -hn
_[2 827
"l €€• 2~7
"1J9_57?T
" i~2
I
20 .27
1 0 03
)FLU011IDL'
) FLUORIDE
)FLUORIDE
)FLUORIDL'
)FLUORIDE
)FLUORIDE
) FLUORIDE
)P205 FED
IFLUORIDE
WA TER
TOTAL
MG
SOLUBLE, GR/SCF
I 120
, "5T-25
[.m-i
I "54
GR/SCF
- WATER SOL., GR/CF, STK CUD.
- TOTAL, GR/CF, STK CND.
.- WATER SOLUBLE, LB/HOUR
- TOTAL, . LB/UOUR
1 1T.DT!T>T)
h
TT;
" i~o~ no~~"
" |1T.~00~9~"
" ~""
' prnrnr?
"j""^0""'
L-^^^
.1
.1
.1
.1
.1
.1
.1,
.1
.1
.1
.1
.1
.1
.1
WATER SOL., LB/TON P205 FED
TOTAL, LB/TON P205 FED
.11
.11
.1!
***S.T.P.+-*DRXt 70 DECREES F, 29.92 IKCHES MERCURY***
-------
APPENDIX B
Field Data
-------
^ ROrl»AL
Gainesvilie, Florida
SOURCE SAMPLING FIELD DATA SHEET
Sampling Location *c_O» Oorcjfr
Date *?- /^ '?«. Run No. /
Time Start ft] (9 Time End J6~?'3
Sampling Time/Point »O x^/O^C ("£ |pfj?)cl2^*i
DB/d>2.°F, WB °F, VP @ DP " "Hg
Bar- Press. 30 "Hg, Stack Press. 3<=> "Hg
MoisturejT_^>FDA_/vVV/y
Temp. ^ C? °F, W/D ^5 ,W/S O— \O
Sample Box No. £""" Meter Box No, /
Meter AH@ /»^Pitot Corr. Factor £7. #"7
Nozzle Dia.^.Z^in. , Probe Length ^ ft
Probe Heater Setting 2-^Nomograph Cf
Stack Dimensions *? Z in
Stack Area ?S&*1~7 f£2
Stack Height tO& ft
Sketch of Stack
//
^>
*,
*v flr
£/*./* 'x ^**V
x^/
Mat'l Processing Rate
Final Gas Meter Reading
Initial Gas Meter Reading
.o
Condensate Increase in Impingers
Moisture in Silica Gel ^ / 2 « /
Silica Gel Container No, 73'
Orsat:
Filter No .7>--
: CO,
CO
Hy
Excess
Air
i
Test Conducted by:
Remarks :
^ PC CSS
Port and
Traverse
Point No.
Distance
From Inside
Stack Wall
1.77
, I 2-
Clock
7 i me
//
-UTT
JL
I
1455-
Gas Meter
Reading
(ft3)
Stack
Velocity
Head
("H20)
o
Meter
Orifice
Press. Diff.
Calc. Actual
MO
Ui.
|."7O
Stack Gas
Temp.
IGd
SO
Gas Sample
Temp.@Dry
Gas Meter
In
n
*7
Out
$(,
Sample
Box
Temp.
Last
Imp inger
Vacuum
on
Sample
Train
("Hg)
0.
O
-------
Port and
Traverse
Point No,
9
r
?
(*>
//
/ 2-
Distance
From Inside
Stack Wall
(in.)
O> 2^
•o**
t, 77
1.2?
f.iz
**74
Clock
Time
/r 2^0
75" 30
/S~4o
)X&0
'y i jj
/£o2»
/6/3
Gas Meter
Reading
(fts)
7^3,63
73^ . ^6
-?^^.4r
146>A
ZM_^_
/^>Z3 762. o /
.
^
Stack
Velocity
Head
("H20)
,4--?
.5"0
,r3
. ro
,5Z?
/-•ra
Meter
Orifice
Press. Diff.
("H..-0)
Calc,
l,7o
A^o
i.^o
/Jo
/.&
/•KD
i
Actual
/.~7O
L$o
no
t.to
i.?o
/. y&
Stack Gas
Temp,
(°F)
/
-------
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
Plant C- F GtfL.W6tfL. . Mat'l Processing Rate
Sampling Location Pi~AM~r Cr/y/7?oP OorU
Date 9-/r-7Z.Run No. 2,
Time Start O8-3S~ Time End /O 4O
Sampling Time/Point |Q /5} jo t^.-n f ;> , ~ !2r>KV
DB /00°F, WB °F, VP @ DP "Hg
bar- Press. ^O "Hg, Stack Press.;?/? "Hg
Moisture ^-S^FDA^k 5Gas Density Factor /
Weather J5"uwy - C ^€V?£
Temp. ^ °F, W/D 5E ,W/S O- 3 wvy.^
Sample Box No. Meter Box No. S~
Meter AH@ l.^g Pi tot Corr. Factor ,%$
Nozzle Dia. /4 in., Probe Length & ft
Probe Heater Setting ^o Nomograph Cf ,^1
Stack Dimensions "7 2 " P in
Stack Area . ft2
Stack Height ' ft
r\ Sketch of Stack
Final Gas Meter Reading ? 5*7 • ^ ft3
Initial Gas Meter Reading ~7<£ 2 ,? ftj
Condensate Increase in Impingers ^^3 nil
Moisture in Silica Gel /^. Z- gm
Silica Gel Container No,_^^> Filter No^_Z^j^2_
Orsat: CO, I i
0,
. CO
N,"
Excess
Air
Test Conducted by: /?.t. W/L.55*A/
^5" Ayc'C-'f
Remarks:
Port and
Traverse
Point No.
7
%
1
10
11
/l*
Distance
From Inside
Stack Wall
Citw)
^•/-.)
/Z-k
/7
' o i
/ ... *.,
(. / 1
4-23
3T./Z
Clock
Time
£?^r
o *3.y
5We\
c -,• <•• tT
O^ / O
Gas Meter
Reading
(«3)
7^,3o
77J.3ZS-
\3h-tes
-7?3,72,
093
-------
Port and
Traverse
Point No,
/
2_
3
4-
5-
C
Distance
From Inside
Stack Wall
^ / n • 'y
/ lljT-J* 1
,Z £»
' . #£
/. 77
SV2.
<, 7 4
Clock
Time
/o9^o
/£> <0 O
£ /£?
<92-6>
o3o
fO^o
j
Gas Meter | Stack
Reading Velocity
(ft3) Head
("H20)
$/4.7b
%?,3.-jO
VZa^'d
^57. fO
. 36
.5"^
, 56
,33
•^44. 2^, I . 38
85V. ?^>
4*Q
.
Meter
Orifice
Press. Diff.
("H~0)
Calc.
/. 30
l.o
2. D
\.1~
L37
/.73
Actual
/• 30
3.0
°LP
L2^.
/•37
/. 73
Stack Gas
Temp.
tf~0
/ cri)
/ OO
/Q ^
/O 2,
JO ^
Gas Sample
Temp.@ Dry
Gas Meter
In
?3
%>
78
/so
1 01
/04.
Out
cx c^
C) O'
^^
(^\ /
7^
^4-
-------
lONMML
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
Plant C.f.
C/ry
Sampling Locati on
Date ^-/r
ft Q P O U TLL 7
Run No.
3
Time Start /'/£& Time End_
Sampling Time/Point /£(g
b
WE
F, VP @ DP_
_"Hg
"Hg
Bar- Press. ._3.<;iL_''Hg, Stack
Moisture^JS,FDA_2jfe_,Gas Density Factor 7
Wea th e r StJsJ'lY ~ ./•/£> T
Temp °
_3JL°F ,
Sample 6ox No. __ Meter Box No.
Meter A.HQ/.6 ^ Pi tot Corr. Factor
Nozzle Pi a. N/4- in. . Probe Length ff
Probe Heater Setting 4<> Nomograph Cf
Stack Dimensions
Stack Area
Stack Height
- 3
T3
ft
Sketch of Stack
Mat'l Processing Rate
Final Gas Meter Reading *? JrQCjO Q ft3
vs-Zos-f ftj
Initial Gas Meter Reading y5
Condensate Increase in Impingers_
Moisture in Silica Gel /<<7.
jnl
_gm
Silica Gel Container No. 71
Orsat: C02
02
CO
ilter
Excess
Air
Test Conducted by: A I. \Ui l $ <®
ft2
ft
Remarks:
Port and
Traverse
Point No.
/
i
3
ft
c~
(ft
Distance
From Inside
Stack Wall
JU-M
(r-r}
• 2/,
M
/•77
4-*3
?. /Z.
S'.7 ^r
Clock
Time
1200
-L2LD
1%3Q
/Z :-• 0
> -.
' .-. ••* i'1
t *i •»*. /*\
M :> O
Gas Meter
Reading
(ft3)
t-*S"3>J.%
L?^"Li>oJ
3"? 5". ^0
tti. 1 4
fat. 2?
%cl^ U ?
Stack
Velocity
Head
("H20)
,40
5-J
• •$€
, 30
'•^Tj
.44
Meter
Orifice
Press. Diff.
("H20)
Calc.
(*$
/lo
2-0
A/
t.1%
I.CflO
Actual
/.45-
/_29
^ .0
_A/
/.a 2
££0
Stack Gas
Temp.
(°F)
/<93
/Q3
/03
/O^L
lot.
te>3
Gas Sample
Temp.@Dry
Gas Meter
(OF)
In
>04
tt>(«
^07
fnk
/OC,
iO(*
Out
103
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APPENDIX C
Standard Analytical Procedures
-------
ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park, North Carolina 27711
Reply to ..""..'
Altn of: n ,
Datt: 12-21-72
Subject: summary of Fluoride Analysis
7"
"' R.* Neulicht, EMB, IRL • .
This memorandum is in response to your request for a brief
summary of our SPADNS-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 Ag2So. is added to the still. SPADNS solution is added
to an aliquot of the distillate and the absorbance is read at 570 nm.
The concentration of the sample is determined from a calibration curve
prepared from standard fluoride solutions. It is very important that
the temperature of the samples be the same as that of the standards
when absorbances are recorded.
The water insoluble fraction of the sample is evaporated to dry-
ness in the presence ot a sxurry of UH.O, and uuen Tu^eJ «iLli"i;ACII. The.
fusate is dissolved with distilled water, neutralized with dilute H So.,
distilled and analyzed as described for the soluble portion.
Paper filters containing particulate are cut into small pieces,
suspended in a slurry of CAO, evaporated to dryness and ashed prior
to the alkali fusion and distillation.
If you have any questions about this procedure, let me know.
Howard L. Crist
Chief, Source Sample Analysis Section
SSFAB, QAEML .
cc: R. E. Lee
-------
Phosphorous Pentoxide Determination
Coloriraetric 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 pento::ide is de-
termined from a calibration curve prepared with standard solutions.
f
-------
APPENDIX D
Project Participants
-------
PROJECT PARTICIPANTS
Environmental Engineering. Inc.
Name Title
John Dollar, E.I.T., M.S.E. Project Manager
George Allen Environmental Specialist
Marvin Hamlin Environmental Specialist
Steve Neck Environmental Specialist
A. L. Wilson Environmental Specialist
Environmental Protection Agency
Roy Neulicht
John Reynolds
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