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

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    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

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                          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

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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.

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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.

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       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.

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  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

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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

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           APPENDIX  A
Emission Calculations and Results

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              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)

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               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)

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                           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 *? •
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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
                    ^

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APPENDIX  B



Field Data

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                                               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)

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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).

























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                                          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
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                                                                        *~*
                                                                       3IJ

-------

-------
Port and
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Distance
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-




















Clock
Time
























Gas Meter
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Stack
Velocity
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-




















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,



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Sample
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                                                                       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
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Distance
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Clock
Time







, .
















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Reading
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Stack
Velocity
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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)














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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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