TEST NO. 73 - FRT - 13
BORDEN CHEMICALS, INC.
DIAMMONIUM PHOSPHATE
PINEY POINT, FLORIDA
SEPTEMBER 26 AND 27, 1972
<>f»r/rnwrift*/. inc.
2324 S. W. 34th STREET / GAINESVILLE/FLORIDA 32601 / PHONE 904/372-3318
-------
TEST NO. 73 - FRT - 13
BORDEN CHEMICALS, INC.
DIAMMONIUM PHOSPHATE
PINEY POINT, FLORIDA
SEPTEMBER 26 AND 27, 1972
Test Conducted By:
Environmental Engineering, Inc.
Contract No. 68-02-0232
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TABLE OF CONTENTS
Page
List of Figures iii
List of Tables 111
Introduction 1
Summary of Results 3
Process Description 5
Process Operation 5
Location of Sampling Points 7.
Sampling and Analytical Procedures 9
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. Process Flow Diagram 2
2. Sample Point Description 8
3. Fluoride Sample Train 12
LIST OF TABLES
Page
1. Summary of Results 4
iii
-------
I. INTRODUCTION
Under the direction of the Environmental Protection Agency,
Environmental Engineering, Inc. conducted emission tests at the
Borden Chemical phosphate works in Piney Point, Florida. On Septem-
ber 26 and 27, 1972, three test runs of two hours each were conducted
on Borden's diammonium phosphate (DAP) process. This source had pre-
viously been tested by EPA in January 1972 for fluoride and ammonia
emissions; test #72-CI-3. The purpose of the second set of tests was
to obtain additional fluoride 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 process outlet to the atmosphere. In addition, grab samples of
the scrubbing liquids, the process reactants, and the process product
were analyzed for fluoride and P^O,- content. A schematic flow diagram
of the process operation and the sampling locations is presented in
Figure 1.
Pertinent test results are listed in Table 1; complete test data
are given in Appendix A.
-------
Q-N1J
Pond Water
To Pond
Surge Tank Acid
To Surge Tank
305 of P^Os
54°, of P205
NH3
To JJAP Storage
To Scrubbers Sump
To GTSP Storage
Stack Sample
Grab Sample
00
L.
SURGE
TANK
(G)
•w
0©
REACTOR
TO ATMDSPUI-RE
TAIL GAS
SCRUBBER
©C
— »
T ^ E
TAIL GAS
SCRUBBER
U>— •
-H*(z)
TAIL GAS
SCRUBPIIR
W-ACrOR
SCRUBBER
©
DRYER
SCRUBBER
CYCLONE
s*--'
i
AMMONIATOR
DRYER
COOLER
SCRUBBER
CYCLONE
SCREEN
CO
COOLER
(T)
FIGURE 1
DAP FLOW DIAGRAM, BORDEN CHEMICALS
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II. SUMMARY OF RESULTS
The plant was operating under normal process conditions during
all of the test runs. Only one deviation from standard sampling pro-
cedure was necessitated. Due to the physical configuration of the
sampling platform at the test point, it was impractical to traverse
the stack during the actual fluoride tests. Consequently, the tests
were conducted at a single point approximating average velocity. A
complete velocity traverse was taken before and after each test run
to determine the average stack gas velocity for that run. This devia-
tion from normal procedure should not affect the test results since
the test port was located after approximately 200 feet of straight
stack, and the gases would, therefore, be well mixed and uniform at
this point,
A complete summary of the stack gas conditions and the emission
levels for each test run is presented in Table 1.
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TABLE 1
SUMMARY OF RESULTS
FLUORIDES
BORDEN CHEMICALS
DAP 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 P,,05 Fed.
Fluoride, total, Ib/ton P205 Fed.
1
9/26/72
30
30
6.1
109
94225
96.349
5.1
5.2
0.0008
0.0008
0.0007
0.0007
0.66
0.67
0.03
0.03
2 '
9/27/72
30
30
6.3
109
85586
72.16
3,6
3.6
.0.0008
0.0008
0.0007
0.0.007
0.56 .
0.56
0.03
0.03
3
9/27/72
30
30
6.6
in
80346
90.38
4.6
4.6
0.0008
0.0008
0.0007
0.0007
0.54
0.54
0.03
0.03
Dry, 70°F., 29.92 inches Hg.
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III. PROCESS DESCRIPTION
The process consists of a preneutralizer for ammoniation of
wet-process phosphoric acid, an ammoniator-granulator, and accessory
equipment for drying, cooling, and screening the product. The pri-
mary reaction is as follows:
2NH3 + H3P04 -> (NH4)2 HP04
Unabsorbed ammonia gas flows out with exhaust gases; however,
most of this ammonia is returned to the process by means of a scrub-
bing system using weak phosphoric acid as the scrubbing medium.
The scrubber acid is mixed with 54 percent PpCL acid (from the
wet-acid plant) in the preneutralizer resulting in a solution usually
averaging about 39 percent P205-
The DAP slurry is pumped from the reactor to the granulator
where additional ammonia is added along with recycled product to form
a solid material averaging 18 percent N and 46 percent Pp^c- Then it
is dried, cooled, and screened before being conveyed to storage.
IV. PROCESS OPERATION
During a brief tour of the plant on September 26, 1972 (before
collection of the first samples) the writer noticed that particulates
generated at the DAP loading area were being collected and ducted to
the same stack which vents the controlled DAP process emissions. At
the writer's request, the loading emission collection system was shut
off during the collection of EPA's emission samples.
-------
The first test run was performed on September 26, 1972. The
second and third test runs were performed on September 27, 1972. All
test runs were performed while the process was operating at normal
production rate. The process operated normally throughout all test
runs. There were visible emissions of zero to five percent opacity
during collection of all emission samples.
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V. LOCATION OF SAMPLING POINTS
The number of velocity traverse points was 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.
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 was used-only for a velocity traverse be-
fore and after each test run. The configuration of the sample plat-
form prevented traversing the stack during the actual fluoride test.
The fluoride tests were conducted at one_ point only.
Figure 2 is a schematic diagram of the stack configuration
near the sampling location.
-------
T
3'
-—O
> 8D
A
J
A-.A-
"s A MPLE
"POINT
i
2.
3
4
5
G
7
S
9
10
II
12
"DISTANCE
FROM INSIDE:
WALL (INCHES)
1.8
5.8
IO.2
15-3
Z1.5
.30.5
55.8
G5.O
71.0
76-i
60.7
B4-7
Figure 2
LOCATION OF SAMPLING PORT OUTLET
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VI. SAMPLING AND ANALYTICAL PROCEDURES '
Preliminary Moisture Determination
The preliminary moisture content of the stack gas was found by
using the wet bulb-dry bulb method as referred to in the Federal
Register (Vol. 36, No. 247, Part II, December 23, 1971).
Preliminary Velocity Determination :
Method 2 of the above mentioned Federal Register was used as
a guide in determining the preliminary stack gas velocity for each
source tested. The major difference was.that only the maximum and
minimum velocity heads across each stack area were determined so that
a proper nozzle size could be selected. Before and after 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. . -
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 tv/o 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). Figure 3.
is a schematic diagram of the sampling train used.
After the selection of the sampling site, 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 every five minutes or when signifi-
cant 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.
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.
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.
10
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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 dis-
tillation, then by the SPADNS - ZIRCONIUM LAKE Method.
P^Og analysis of the stack effluent was done by EPA personnel.
All other PpOr analyses were done by plant personnel.
For more details of exact method, see Appendix C.
11
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2.
.3.
4.
5.
6.
7.
8.
9.
10.
•» i
i I .
14.
15.
16.
17.
19
Stainless Steel Nozzle
Heated Glass Probe
Glass Connector
Ice Bath
liv.pinger with 100 ml I-LO (Modified Tip)
Impjp.ger with 100 ml H^O (Standard Tip)
Impinger, Dry (Modified Tip)
In-.pinger with 180 grams Silica Gel (Modified Tip)
Filter Holder with No. 1 Whatman Filter
Than.IOmeter
Flexible Sample Line . '
VuCi:u:;i Gauge
Main Control Valve
By-Pass Control Valve •
Air Tight Vacuum Pump
Dry Test Meter
Calibrated Orifice
Ir;d i nc-d Kar.o-~.eter
19. S-Type Pi tot Tube
Figure 3
FLUORIDE SAMPLING TRAIN
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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 zero
TS - Stack temperature, °R
TM - Meter temperature, °R
Average square root of velocity head, Vinches
AH - Average meter orifice pressure differential, inches
AN - Sampling nozzle area, square feet
CP - S-type pitot tube correction factor
'VM - Recorded meter volume sample, cubic feet (meter conditions)
VC - Condensate and silica gel increase in impringers, milliliters
Po - Pressure at the dry test meter orifice, fPB +A H~[ inches Hg
L 13. 6J
STP - Standard conditions, dry, 70°F, 29.92 inches Hg
- Conversion of condensate in 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 air, %
- Average square root of velocity head times stack temperature
- Stack gas velocity, feet per minute
- Stack gas flow rate, cubic feet per minute (stack conditions)
- Stack gas floxj 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)
-------
EQUATIONS FOR CALCULATING FLUORIDE EMISSIONS
VWV = (0.0474) x (VC)
VSTPD = (17.71 x (VM) x (PB H- -^- ) -f- TM
13.6
VT = (VWV) + (VSTPD)
W = (VWV)-HVT)
FDA = (1.0) - (W)
FMOIST = Assumed moisture fraction
MD = (0.44 x % C0_) + (0.32 x % 00) + (0.28 x % N9) + (0.28 x % CO)
2. £. £•
MS = (MD x FDA) + (18 x W)
GS = (MS)-;- (28.99)
EA = [(100) x (% 02 - ^2^)] -r- Qo.266 x % NZ) - (% 02 - %2CO)
U. = (174) x (CP) x (H) x ^(TS x 29.92)-h(GS x PS)
QS = (U.) x (AS)
QD = (QS) x (FDA) •.
QSTPD = (QD) x (^3^) 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)
\
?2®5 ^ec* = Tons/hour, determined from plant data -
Lbs/ton P20 Fed = (Ibs/hour) -7- (Tons/hour P20c Fed)
-------
S.QWC.E
no -' : no OF nurs - . u
SOUVCF - D.A.P. OUTLET ' ' . . ' 'J
TYPE Or PLflUT - •'•",' ' . • .„?
CONTROL EOUll
POLLUTANTS St
I) RUN NUMBER ' ..'
2)DATE .. ;.
3)TIME BEGAN • •--•=.-.;:•• 'r. ' -
U)2TM£: END . ?/-; \-: :
^BAROMETRIC PRESSURE, Iff HG ' '•
&)METER ORIFICE PRESSURE DROP, IN. HG
7)VOL DRY GAS, METER C011D, CUBIC .FEET
8) AVER AGE GAS METER TEMPERATURE, DEG F
9)K0L DRY GAS, S.T.P. , CUBIC FEET
1Q)TOTAL 1120 COLLECTED, ML ' .
1DTOL //20 VAPOR COLLECTED, S.T.P. , CU F
12)STACK GAS MOISTURE, PERCENT VOLUME '
13)ASSUMED STACK GAS MOISTURE, PCT VOL
1 ii ^ P P 7? r* i? ij T c* o *? •
X^/Xultw{j
. 1 J__-,^
r i iT. \fii7V?,
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I
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1
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1
1
1
1
1
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1
1
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it O c -• i
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-' . :•• (. : •
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'•:,". . .:
'•....;• .
***S.T.P.4~+DRY, 70 DEGREES F, -23 . 92 -JXCUES MERCURY***
ISOKINETIC DETERMINED USING V£LOC1TY HEAD-READINGS FROM ACTUAL FLUORIDE TEST, NOT
^
-------
APPENDIX B
Field Data
-------
Gainesvilie, Florida
SOURCE SAMPLING FIELD DATA SHEET
/
2.***
V
Plant
Sampling LocationP
Date
Time Start
Sampling Time/Point^?
F, WB °F, VP @ DP
Bar- Press._J<2_j'Hg,Stack Press. 3^
Moistur::^^^.lFDAJ,5^.»Sas Density Factor_/_
Weather X&4&2&
: ">•" 0"~™ f
T, W/D
Sample Box No. Meter Box
Meter AHQj.o^ Pi tot Corr. Factor
Nozzle Dia.c-2
a.gjZS.in. , Probe Length
Probe Heater Setting ^O Nomograph
Stack Dimensions
Stack Area
Stack Height
ft
. 5-
in
200 ff
, M
Mat'l Processing Rate
Final Gas Meter Reading
Initial Gas Meter Reading
Condensate Increase in Impingers_
Moisture in Silica Gel n •*?
» 7%Q
_ft3
ml
/3J-;
im
Silica Gel Container No.
Filter No.
Orsat: CO-
02
CO
Excess
Air
Test Conducted by:
Remarks:
ft
Port and
Traverse
Point No.
Distance
From Inside
Stack Wall
FT.
Clock
Time
LUSL
Gas Meter
Reading
(ft3)
LTf..-!—
Stack
Velocity
Head
("H20)
Meter
Orifice
Press. Diff.
("H20)
Calc. Actual
a.
Stack Gas
Temp.
joo_
Gas Sample
Temp.@Dry
Gas Meter
In
4J^
LU^
88L.
Out
$ir
Sample
Box
Temp.
(°FJ
Last
Impi tiger
6^
Vacuum
on
Sample
Train
("Hg)
-------
P.ort.and
Traverse
Point No.
CAW*** s '
fifL.r&
j~
Distance
From Inside
Stack Wall
(in.)
•
#» i ^
"\
Clock
Time
/22S
/?$.*/
tun.r
Stack
Velocity
Head
("H?0)
&.fe©
o.6r
o.& 5
O.^^
ft.^»5
^ss.ssr lo.ds
il~ T~L_
Meter
Orifice
Press. Diff.
("H-0)
Calc.
J.Vd
<2-^e
2.41*
&<**
&«f& .
Z.10
Actual
8*va
l><*6
&.
ft A
//d
n o
//•
HO
Gas Sample
Temp.@ Dry
Gas Meter
(°F)
In
9«
9*
^e
9®
^*
f^
Out
M
ff
^9
P9
^7
9»
ample
Box
Temp.
(°F)
Last
Impinger
Temp.
(°F)
6J
CS
&5
cs
^r
43
Vacuum
on
Sample
Train
("Hg)
-------
Port and
Traverse
Point No.
Distance
From Inside
Stack Wall
(in.)
Clock
Time
Gas Meter
Reading
(ft*)
!
1
1 _ .
Stack
Velocity
Head
("H20)
Meter
Orifice
Press. Diff.
("H-0)
Calc.
Actual
•
1
Stack Gas
Temp.
(°F)
Gas Sample
Temp.@ Dry
Gas Meter
(°F)
In
Out
ample
Box
Temp.
(°F)
Last
Impinger
Temp.
(°F)
Vacuum
on
Sample
Train
("Hg).
-------
IIROH19lTAL"iflGIN9H
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
•ft
Sampling
Date $~ 2.7-72-Run No.
Time Start 0^3° Time End
Sampling Time/Point i^-Q
nR 190 °F '-JR
L/Q f fl *^ I 5 *»*-»
Bar- Press.
'SJo_
F, VP 0
.6
Sketch of Stack
"Hg
"h'g:Stack Press._2s>"Hg
Moisture_J?jb?FDA^flf ,Gas Density Factor /
Weather
Temp._
/
. F. W/ D_jC^_, W/ S
Sample Box No. Meter Box No.
Meter AH@f.
Nozzle D
Pi tot Corr. Factor_
in., Probe Length_
ft
Probe Heater Setting X Nomograph Cf 0<
Stack Dimensions
Stack Area
Stack Height
in
Mat'! Processing Rate
Final Gas Meter Reading "/
Initial Gas Meter Reading
Condensate Increase in Impingers
Moisture in Silica Ge1 ^ t O
Silica Gel Container No, (OS" Filter
Orsat:
ft3
: C02
o?
CO
N?"
Excess
Air
•
i
Test Conducted by:
_ft2
ft
Remarks:
/MSSA&fSi&S&UFP- *^*Z3'£X>£,Q&K3. &**f ^aegy.
Port and
Traverse
Point No.
Distance
From Inside
Stack Wall
(in.)
Clock
Time
(SJO-
Gas Meter
Reading
(ft3)
JL
Stack
Velocity
Head
("H20)
^J>^3&_
Meter
Orifice
Press. Diff.
("H20)
Calc.
IM ,
Actual
JLLLHL
U±.
Stack Gas
Tem.
4l.o-
ILQ_
IP'S
Gas Sample
Temp . @Dry
Gas Meter
In
Vs
Out
miL,
i?_
10.
Sample
Box
Temp.
Last
Impinner
60
Vacuum
on
Sample
Train
("Hg)
*~*
3IJ
-------
-------
Port and
Traverse
Point No.
Distance
From Inside
Stack Wall
(in.)
-
Clock
Time
Gas Meter
Reading
Stack
Velocity
Head
("H20)
-
Meter
Orifice
Press. Diff.
("H-0)
Calc. i
Actual
,
Stack Gas
Temp.
Gas Sample
Temp.@ Dry
Gas Meter
In
Out
ample
Box
Temp.
Last
Impinger
Temp.
(OF)
Vacuum
on
Sample
Train
("Hg)
-------
NC.
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
Sampling Location
r ^f\
Date /'^
Run No.
Time Stan
Time End
Sampling Time/Point_(<
Bar- press._3?L"HgJStack Press._^^Nomogra.ph Cf
Stack Dimensions
Stack Area
Stack Height
Sketch of Stack
Mat'l Processing Rate_
Final Gas Meter Reading
Initial Gas Meter Reading_
Condensate Increase in Impingers_
Moisture in Silica Gel /.S
_fi
fl
Silica Gel Container No.
Orsat: C0
Filter
CO
Excess
Air
Test Conducted by:
Remarks:
ft .
-------
-------
Fort and
Traverse
Point No.
Distance
From Inside
Stack Wall
(in.)
Clock
Time
, .
Gas Meter
Reading
(ftj)
Stack
Velocity
Head
("H?0)
Meter
Orifice
Press. Diff.
("H,Q)
Calc. i
Actual
Stack Gas
Temp.
(°F)
Gas Sample
Temp.@ Dry
Gas Meter
(°F)
In
Out
1
ample
Box
Temp.
(°F)
Last
Impinger
Temp.
(OF)
Vacuum
on
Sample
Train
("Hg)
, . _ja
-------
PA Sa«*le. W
fO,
Run Mo,
L
Y«:
\ u^
S A VA p ( if\ #• Po t w*\"
U-is
I p"
r
PH •
0
O
o
fluorides
P
Trace. AUtal
s
-------
EPA Sarnie. Mo.
RIM Wo,
us
0
o
o
o
-------
EPfl Sa^le. Afe.
Da'fe.
S A vH ^ f 1 Vi .•? Po f v\T
f V) \ \
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EPA Sample. Wo.
— :—'• r~ -~—
an Mo,
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X
-Or
| \0 I
V4
M
P H
t>
c>
Mescals
R
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EPfl SAw^le. Mo.
Mo,
A
IV're,
1 — —a
PlL
-------
Rtm Mo,
e. o.
tv' MA.',
Vs- ^l
\os
G-
°
ew p era.'T uf e ,
fluorides
PeOs
-------
avr
e-w
EPA Sarnie. Wo.
No,
Dafe.
T
# -^w>.
PH
Vv I
Us
I.I. s-
Me.tA(
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-------
EPR S/u^le, f\fo,
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APPENDIX C
Standard Analytical Procedures
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'«? ..• • "w .
. ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park, North Carolina 27711 .
Reply to '
Altn of: ^ .
J - • Date: 12-21-72
Subject: summary of Fluoride Analysis
fj-f
°: 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 td 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 nir..
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 or a slurry or OaO, and biien Iu=>eJ wiLl* 1,'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
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Phosphorous Pentoxide Determination
Colorimetric Molybdovanadophosphate Method
An aliquot of sample is hydrolyzed in the presence of HC1 and
HNO acids by boiling almost to dryhess. , ' . .-
. '. ' ' o
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.
f
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APPENDIX D
Project Participants
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PROJECT PARTICIPANTS
Environmental Engineering, Inc.
Name Title
John R. Dollar. Project Manager
George Allen Environmental Specialist
Marvin Hamlin Environmental Specialist
Jack Riggenbach Environmental Specialist
A. L. Wilson Environmental Specialist
Environmental Protection Agency
Leslie Beck
Roy Neulicht
John Reynolds
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