TEST # 72 - C! - SOB
W. R. GRACE AND COMPANY
GRANULAR TRIPLE SUPERPHOSPHATE STORAGE
BARTOW, FLORIDA
JUNE 14-15, 1972
. nc.
2324 S. W. 34th STREET / GAINESVILLE, FLORIDA 32601 / PHONE 904/372-3318
-------
TEST # 72 - C! - SOB
W. R. GRACE AND COMPANY
GRANULAR TRIPLE SUPERPHOSPHATE STORAGE
BARTOW, FLORIDA
JUNE 14-15, 1972
Test Conducted by:
Environmental Engineering, Inc.
Contract # 68 - 02 - 0232
-------
TABLE OF CONTENTS
Page
List of Figures iii
List of Tables iii
Introduction 1
Summary of Results 1
Location of Sampling Points 4
Sampling and Analytical Procedures 6
Appendix
A. Emission Calculations and Results
B. Field Data
C. Standard Analytical Procedures
,D. Project Participants
-------
LIST OF FIGURES
Page
V. Location of Sampling Point 5
2. Sample Port Location 5
3. Fluoride Sampling Train 8
LIST OF TABLES
1. Summary of Results
-------
I. INTRODUCTION
Under the direction of the Environmental Protection Agency, Environmen-
tal Engineering, Inc. conducted emission tests at the W. R. Grace and Com-
pany phosphate works in Bartow, Florida. On June 14 - 15, 1972, three test
runs of two hours each were conducted on the granular triple superphosphate
storage building. The purpose of the test was to obtain emission data for
the use of both the Industrial Studies Branch and the Performance Standards
Branch of the Environmental Protection Agency.
Measurements for soluble and insoluble fluorides were made at the outlet
stack of the storage building scrubber. Grab samples of the scrubbing liquid
and storage product were analyzed for fluoride and P?0r content. A schematic
flow diagram of the process operation and the sampling location is given in
Figure 1. Complete test results are listed in Appendix A.
II. SUMMARY OF RESULTS
The amount of granular triple superphosphate located in storage during the
test runs was approximately 4500 tons P<>0,-. Normal production and shipping
operations were taking place during the test runs.
No irregularities occurred during the sampling; all tests went smoothly.
A complete summary of the stack conditions and emission levels for each test
run is given in Table 1.
-------
FIGURE 1
W. R. Grace and Company
GTSP Storage
'To Atmosphere
Sample
Point
ro
GTSP
Product
Storage
Building
Pond Water
off-gas -
Shipping
Scrubber
To Pond
Stack
-------
TABLE 1
SUMMARY OF RESULTS
FLUORIDES
W. R. GRACE
STORAGE OUTLET
Run No.
Date
Barometric pressure, inches Hg
Stack pressure, inches Hg
Stack g'as moisture, % volume
Average stack gas temperature, °F.
Stack gas flow rate @ S.T.P?S 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
Tons, product stored
Fluoride, water soluble, Ibs/hr/ton P20g
Fluoride, total , Ibs/hr/ton P?05
Scrubber efficiency, %
1
6/14/72
30
30
3.9
81
64587
75.359
2.4
2.47
0.0005
0.0005
0.0005
0.0005
0.27
0.28
4318
Less than
Less than
_
2
6/15/72
30
30
. 3.5
80
62633
74,336
2.2
2.2
0.0005
0.0005
0.0004
0,0004
0.24
0.24
4625
J.0001
1.0001
3
6/15/72
30
30
.'3.6
81
63658
75.197
2.4
2.47
0.0005
0.0005
0. 0005
0.0005
0.27
0.28
4685
Dry, 70°F., 29.92 inches Hg.
-------
V. LOCATION OF.SAMPLING POINTS
The sampling sites and number of traverse points were
selected as per "Method I - Sample and Velocity Traverses fbr Sta-
tionary 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.
Figure 2 is the schematic diagram of the stack configura-
tions near the sampling location, and the sampling points traversed
during the emission tests. -
-------
STORAGE SCRUBBER OUTLET
60
PORT 2
PORT i
A'-A'
PRAVER^T"DISTANCE"
POINT NO. MvROM pORT
I "—-~4-^-L!lS±l££)
i n/is
s 3/e
"7/IG
573 i
13/321
19/3Z
27/3E
9
i^
ao
26
5 |
GO
-------
SAMPLING AND ANALYTICAL PROCEDURES
A. 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).
B. 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.
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 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.
-------
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 D. 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.
D. 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.
-------
19
Stainless Steel Nozzle
Heated Glass Probe
Glass Connector
Ice Bath
livipinger with 100ml FLO (Modified Tip)
Impinger with 100 ml H«0 (Standard Tip)
Irnpinger, Dry (Modified Tip)
In-pinger with 180 grams Silica Gel (Modified Tip)
Filter Holder with No. 1 Whatman Filter
Thermometer
Flexible Sample Line . . . '
Vacuum Gauge
Main Control Valve .
By-Pass Control Valve-
Air Tight Vacuum Pump ' .
Dry Test Meter
Calibrated Orifice
Inclined Manometer
S-Type Pi tot Tube
17
Figure 3
FLUORIDE SAMPLING TRAIN
-------
E. Laboratory Analysis Procedures
Water soluble fluorides were done by a sulfuric acid distil- f
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.
All analyses were done by EPA personnel.
For more details of exact methods used, see Appendix C.
-------
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 zen
TS - Stack temperature, °R
TM - Meter temperature, °R _ -
_H - Average square root of velocity head, '/inches 1^0
A,H - Average meter orifice pressure differential, inches H^O
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 13.6_|
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, lbs/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 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
t
VWV = (0.0474) x (VC)
VSTPD = (17.71 x (VM) x (PB + -AIL. ) 4- TM
13.6
VT = (VWV) + (VSTPD)
W = (VWV)-f-(VT)
FDA = (1.0) - (W)
FMOJST = Assumed moisture fraction
MD = (0.44 x %-CO ) + (0.32 x % 02) + (0.28 x % N2) + (0.28 x % CO)
MS = (MD x FDA) + (18 x W)
GS = (MS)-5- (28.99)
EA = [(100) x (% 02 - ^2^-)] -r- Qo.266 x % N2) - (% 02 - %2CO)
U = (174) x (CP) x (H) x V(TSx29.92)-T-(GS x PS)
QS = (U) x (AS) '
QD = (QS) x (FDA)
QSTPD - (QD) x (-J-^) x (||) /
PISO = (o. 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
Grains/SCF = (0.01543) x (MG) -~ VSTPD
Grains/CF, Stack Cond. = (17.71) x (PS) x (FDA) x (Grains/SCF) -~- (TS)
Lbs/hour = (Grains/SCF) x (0.00857) x (QSTPD)
P20 Stored = Tons, determined from plant data
(Lbs/hour) /Ton P^ Stored = (Ibs/hour) -t (Tons P 0- Stored)
-------
TEST NO -
PLANT - J/.tf. GRACE BAPTOW,
SOURCE - STORAGE OUTLET
TYPE OF PLANT - Storage
CONTROL EQUIPMENT -
POLLUTANTS SAMPLED ~ Fluorides
NO OF RUUS - 3
FLA.
1)RUU NUMBER
2) DATE ' '
4 ) TIME END
^}BAROMETEIC PRESSURE, It! 1!G
b)!>JETER ORIFICE PRESSURE DROP, IH ^
7) VOL DRY GAS, METER COND, CUBIC FEET
Q) AVER AGE GAS VETER TEMPERATURE, DEC F
) PERCENT 02
11) PERCENT 7/2
1B)PERCE!>:T EXCESS AIR
1<3)VOLECULAR l-JEIGHT OF STACK GAS, DRY
2Q)IIOLECULAR WEIGHT OF STACK GAS, STK CONl
2DSTACK GAS SPECIFIC GRAVITY
22)AVG SQUARE ROOT (VEL HEAD), III H20
23)AVERAGE STACK GAS TEMPERATURE , DEC F
2^)AVG SQUARE ROOT (STK TEMPxVEL HEAD)
25) PI TOT CORRECTION FACTOR
2G)STACK PRESSURE, II! EG, ABSOLUTE .
21) STACK GAS VEL, STACK COND, F.P.M.
2Q)STACK AREA, SQ FEET
.. 29)EFFECTIVE STACK, AREA, SQUARE FEET
30)STACX GAS FLOV RATE, S.T.P. , SCFM'D
' 3l)NET TIME OF TEST, MIUVTES
32)SAi-:PLi;iG NOZZLE DIAMETER, INCHES
33) PER CENT ISOKINETIC
3^)FLUORIDE - WATER SOLUBLE, 11G
35) FLUOR IDE - TOTAL, MG
36)FLUORIDE -WATER SOLUBLE, GR/SCF
3rl)FLUGRIDE - TOTAL, GR/SCF
3B)FLUORIDE - VATER SOL., GR/CF, STK CUD.
39)FLU01UDE - TOTAL, CR/CF, STK CUD.
HO)FLUORIDE - VATER SOLUBLE, LB/HOUR •
HDFLUORIDE - TOTAL, LB/HOUR
42)Tons, product stored
^3)FLUORIDE ~ 17ATER SOL., lbs/hr/ton P2CL'
H 14) FLUORIDE - TOTAL, Ibs/hr/ton PgOg
It 1 2 1 -3-
1 p / *^ f * / T o ! C/^C/TO ! R /'1 c / *7 o
1 '• r- • IP 1 ia • 5.0. 1 J, J • °n
1 3JL_ _ 1 aa 1 J3U
1 "^ ''"'L 1 75.Q°2, i 7G 691
1 83 7 1 18-_5_ 1 83^.8
1 7 ri 3J-- ° 1 2.y_ 3.3_6u 1 75 1^7
1 Q_u 1 1 5-5. 3. 1 58^5
fl_JLJilL____l 2.^.6.7_ l-.2j>.ll
1_ 3 ^ 1_ 3,^ 1 3^0 _
1 4 „ It L 4
1 1 _ _ 1 „
1 1_ 1 _
1 „ „! 1 _._
1 _ „ _1 _ „_ 1 _
lo_ lo_ __lo
1 28_,85 1 ^,8_8^_ 1 28.85
?1 28_,43 1 28JI7 1 28. 4G
10.98 1 0^_98 I0-98
1 0.579 1 0._558 J0.5G9
1 Qi_,2 1 80 1 81.2
1 13_,45r) 1 12.977 1 13.22 R
10.83 10.83 10.83.
13 0 130 130
1 1 9 G 0_, 2 1 1888.5 1 1 9 2 5 . 4
134.91 J_ 34.91 _[34.91
J_ 34,91 J_ 34.91 J_34.9f
J_ 64587 J_ 6 2 6 3 3 _[_ 6"3 6 5 8
J_ 120 .J_120 I120
J_ "0 . 2 5 J_ 0 . 2 5 _[ 0~. 2~5
J_ 09.6 J_ 101. 3 J_ J-0~0~. 8~
J_ 2 . 4 12.2 _[ .2". 4
J_ . 2 . 4 7 1 2 • 2 1 2~. 'r/
j_ 0 . 0 0 0 5 J_ 0.00 0 5 J_ 0". OTTO~5~
J[ 0 , 0 0 0 ;] J_ 0 . 0 0 0 5 J_ 0". 0~0 0~T
1 """'oTj'n'H" i 0~"oT)"o~t~ ' 1 ~0~.~OTro~^
i "0 . 'O 0 0 '; i 00004 l 0~. OTTO~5~
j j; ^_n L__r_! __.__. J. __._„_,-,._
1 ••-'—" J^ < 1
1 Tj.^v'ju j_ T>.2446 j_ crrrnr
1 43,15 1 4.625 1 46S5
J_~". 00006 1 '.00005 1 .00005
l 700006 J~v. 00005" ~1 VQO'dOB "
~~
I
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***S.y.P.4-+DRYt 70 DEGREES F, 29.92 INCHES VERCURY***
-------
APPENDIX B
Field Data
-------
LNL.O
Gainesville, Florida
SOURCE SAMPLING FIELD DATA SHEET
t_^
Sampling r
Date &~lt{-'7Z~ Run No,
Time Start "2-.'3(3 Time End
Sampling Time/Point
<, VF @ DP
Mo i s ture*/-Q%, FDAfj^L^Gas Density F act or
Barometric Press_j!30"Hg, Stack Press
Weather
CF> W/D
Sample Box No.
Meter AH@_/^/_t?itot Corr. Factor Q>g3
Nozzle Dia. /jn., Probe Length
Probe Heater Settin
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 2 ££#"•" 2. 3 f'7^
Silica Gel Container No.
Orsat: C02
02
CO
Meter Box No.
Excess
Air
.Test Conducted by:
/f? D
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.
0'H20)
Calc. Actual
Stack Gas
Temp.
TO
Gas Sample
Temp,@ Dry
Gas Meter
In
Out
Sample
Box
Temp.
Last
Impinge r
Test
Vacuum;
on
Samplej
Train j
C'Hg)
12
JM.
Go
2J
O.7.6
-03
J^
qz7
I.
go
3
•2;
>. 27
- 4-
0.0-7
go
H
SO
-------
Port and
raverse
Point No...
s
5"
Distance
from End
of Port
(in)
2.0,0
7
9
n
/2J
Clock
Time
3.V5-
_|.V20_
_3>:A£
3: So
3:5-0
Gas Meter
Reading
(ft3) ..
2.
y.
L
Stack
Velocity
Head'
("H20)
Meter
Orifice
Press. Diff ,
("H20)
jStack Gas
Temp*
Calc.
Actual
/
<
Gas Sample] Sar
Temp, QDry
Gas Meter
In
Out
Box
Temp -
.&>
35"
fi^s)
ir?o
^J /'ST2.
S
85
jR&T]7£o
_O_-sJ J_
...
Rf
#5
Last )'
Impingerj en
Temp .
Sample
Train
,57
• •- 'f >, r
hsTT
_--Z_i-__ _!___.
i I ~y
Y^ j ^O
7
•• O
a
0,^7
S
0,
€>
fo
-------
Gainesville, i-j.orida
SOURCE SAMPLING FIELD DATA SHEET
?lant [jj t /?, GffflC£ &)ftT6tifJLA,
Sampling Loc
Date £>~l
.ation /££)•*-$ S7P£$£& QDTUEJ'
'^-72. Run No. 2.
lime Start *%\ So Time End /£> ?££>
Sampling Tii
DB |fO0F.
Moisture Y,C
Barometric I
Weather ^
Sample Box I
Meter AH§ J,
Nozzle Dia.
Probe Heate"
Stack Dimen,
Port and
Traverse
Point No.
rt/^/rf # 1
' !
2^
1,
3
3
! a
« f\
Tp / pf\ T T1 T" 1 *^ jf**^ ^-' " *^ ^*. _/ /^"J » "**
\VBjF -^ °F, YF ? DP "^-. "Hg
2T~T~\ ft fjt,^ « O
, j,FDA y£j«O>G<
?ress3y) "Hg,
is Density F
Stack Prc
actor *"*""*'
Sf'"8
'F, W/D — ,iV/S —
40, ~.~.^- Meter Box No. /
7^fPitot Corr. Factor
|
y'*!/ in. , Probe Length "ST ft
f... i , .
r Setting
5 ions: Inside
Inside
Height
Distance
from End
of' Port
(in.)
f^-k
'
s%
cj7/[&
/¥%2-
tfo%
/ /"
Diameter $5£> in
Area ft^
ft
Clock
Time
<%:££
9:^-0
9!o5"
q-.|O
q : /^
9'2^>
^;-Zb
jM — «
DP~ 7^
;
Gas Meter
Reading
(ft^)
QQ(0» ty~7(o
qqq. /
Oo I ,. 7
oo5^, M-
oo7» 2-
O/O-2.
OI3-!
O 15"-^
Stack
Velocity
Head
("H20)
O»2,Q
Ov2LO
0.2-3
0<2<3
o. 2,5"
O, 2.5*
0. 25-
Mat'l Processing
Final Gas M<
Initial Gas
Total Condei
Moisture in
Silica Gel
Orsat: C02
02 .
CO
N2
Excess
Air
Rate
2ter Reading /O~7 /" 5^^" ft3
Meter Readii
ig ^9^£/7£ft^
is ate in Impingers 2-€> ml
Silica Ge^
Container No
^'4^—2-J7' y^-?^g^
,2<5C?/ Filter No. 7^5
Test Conducted by: f\, £>u/&£/i},i*<>
Remarks :
Meter
Orifice
Press. Diff,
t"H20)
Calc.
0-80
o-Sa
o^i
o.*)t
l'-0t>
licl>
j,(n)
Actual
o-?o
O<8O
o«9/
0.9!
\>cm
I.GD
I.OD
/_8 /^/C/ /£ 7" JT
Stack Gas
Temp .
8O
c^ /^
&
&*£*
*5-.5~"
-------
•'ort and
Traverse
Point No,
5
7
_5
10
Distance
from End
of Port
(in)
20.
a ,7
70
3- '
Clock
Time
*30
Gas Meter
Reading
(ft3)
_au
0^7.7
63.3.^
lo:io
joi
Stack
Velocity
Head
C'H20)
Meter
Orifice
Press. Diff,
Gale, Actual
1,
?^i_/'A®
0^3?'
.3.5"
» \ / -"y
/_, _3pi _/^3o_
Stack Gas
Te.r.p.
Gas Sample
Temp,8Dry
Gas Meter
ra-
In [""Out
7*. 77
77
Sajriple
Box
Temp .
20 \
I.
./•££
Vo
go
m
Last
Impinger
Temp.
ra
Vacuum
on
Sample
Train
~~3r!
i /*• O
I. i - *
r~T. t**v
sr 2
-------
Gainesville, t-lonua
SOURCE SAMPLING FIELD DATA SHEET
Sampling.Location j
Date A-/5-7"*- Ran No
Time Start //'
Sampling Time/Point
Moisture ^0 %, FDA 9^,6,Gas Density Factor
Barometric Press 5'O"Hg, Stack Press3Q "Hg
Weather
Ternp._2O_°F, W/D .— ,U7S —•
Sample Bex No, Meter Box No.__J[
Meter £H(§ /,7¥ Pitot Corr. Factor <^},, %3
Nozzle Dia. /li in., Probe Length '$7 ft
Probe Heater Setting
Stack Dimensions: Inside Diameter
Inside Area
Height
in
Tt2
ft
Mat'l Processing Rate
Final Gas Meter Reading. ' / if,*% * ^ 5^ ft3
Initial Gas Meter Reading (7 ~?/1 ,S^^_ ft0
Total Condensate in Impingers 3&i,Q ml*"--^'
Moisture in Silica Ge£^,3.^ ^3 73 =• ^/ •
Silica Gel Container No,O,QOO Filter No7^537
Orsat: C02
02 :
CO •
NT
Excess
Air
Test Conducted by:
ft
Remarks:
Port and
Traverse
Point No.
Distance
from End
of Port
(in.)
Clock
Time
Gas Meter
Reading
'. Stack
Velocity
Head
("H20)
Meter
Orifice
Press. Diff.
("H20)
Calc. Actual
Stack Gas
Temp.
Gas Sample
Temp.0 Dry-
Gas Meter
no
"IH~
Sample
Box
Temp .
TO
Out
Last
Impii'ger
Test
x'acuiun
en
Sample
Train
("Hg)
-^-^
7^ /
4_
5
go
5%
//135-
a
loo
/. oo
s
HI
UL
5
3
23
S
hi
M
-------
Port and
Traverse
Point No.
Distance
from End
of Port
(in)
Clock
Time
Gas Meter
Reading
(ft3)
Stack
Velocity
Head
C"H20)
Meter
Orifice
Press. Diff,
(f!H20)
Calc, | Actual
Stack Gas [Gas Sample) Sample
Temp.
Temp,@Dry
Gas Meter
In
Out
Box
Temp .
C°F)
Last
Irnpinger
Temp .
Vacuum
on
Sample
Train
Z
7
a
LXJ=f—
U3J V£ I £
lt^.u
^.
A5
/.&?
- c"
> f-Jf'
A
0,3
, 3
M^
13$. 7
Ji4^.
.37^
—+.
tf 30
,.g4_Jg^.
I T\>
x
9 /
5£
7
a
i
0.2-Z
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APPENDIX C
Standard Analytical Procedures
-------
Reply to
Altn of:
ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park, 'North Carolina 27711
n ,
Datf: 12-21-72
Subject: summary of Fluoride Analysis •
*T"
''
•
R." Neul'icht, EM3, 1RL
This memorandum is in response to your request for a brief
summary of our SPADNS-Zirconiuin 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
r.i'nsed 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 :;rrL.
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 or a sxurry or CAU, tmu then luscju. w
,
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, Q7vEML
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 dryness.-
r . . • >
The sample is cooled to room temperature, transferred to a
c . -
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.
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APPENDIX D
Project Participants
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PROJECT PARTICIPANTS
Environmental Engineer]ng,Inc.
Name Title
John Dollar, E.I.T., M.S. Project Manager
George Allen Environmental Specialist
Bob Durgan Environmental Specialist
Larry Wurts Environmental Specialist
Environmental Protection Agency
Name
Jerome J. Rom
John Reynolds
Roy Neulicht
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