TEST NO.  73 - PSA - 1
                       TEXAS GULF, INC.
                     SUPERPHOSPHORIC ACID
                    AURORA, NORTH CAROLINA

                     AUGUST 29-30, 1972
                                                      .  nc.
2324 S. W.  34th STREET  /  GAINESVILLE, FLORIDA 32601 / PHONE  904/372-3318

-------
    TEST NO.   73 -  PSA -  1
       TEXAS  GULF,  INC.
     SUPERPHOSPHORIC  ACID
    AURORA, NORTH CAROLINA

     AUGUST 29 - 30,  1972
      Test Conducted By:

Environmental  Engineering, Inc,

     Contract  #68-02-0232

-------
                         TABLE OF CONTENTS

                                                                Page
Introduction                                                      1
Summary of.Results                                                3
Process Description                                               5
Process Operation                                                 6
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

-------
I.   INTRODUCTION
           Under  the  direction  of  the  Environmental  Protection Agency,
    Environmental  Engineering,  Inc.  conducted  emission  tests  at  the Texas
    Gulf,  Inc.  phosphate  complex in  Aurora,  North  Carolina.   On  August
    29 and 30,  1972,  three  2-hour  test runs  were conducted on TGI's
    superphosphoric acid  production  facilities.  The purpose  of  the tests
    was to obtain  data  for  the  use of  both the Industrial Studies  Branch
    and the Performance Standards  Branch  of  the EPA.
           The  outlet stack of  the off-gas scrubber  was measured for
    soluble and insoluble fluorides.   Grab samples of the scrubbing liquid,
    the process reactant, and the  process product  were  analyzed  for
    fluoride and  P^Or content.  A  schematic  flow diagram indicating the
    sampling location is  given  in  Figure  1.
           Complete test  results are listed  in Appendix A.

-------
             5     i
             ^
 54:4 P?Qu ACID !
     <- J     3

ro
                     CC
                     O
                     J~
                      STEAM
                   PRODUCT
                    COOLER
                   BARO';i:TRjC
                   CONDEUSER
                                                       SCRUBBER
•!' !
1 r-
HOT
WELL

i
i
5
!
                                                                               - EMISSIONS
                                               SEPARATOR
                                                 BOX
Test

  Location
                 STORAGE
                         Figure 1.  VACUUf/i EVAPORATION SUPERPHOSPHOHiC ACiD

-------
II.   SUMMARY OF RESULTS
            The plant was operating  under normal  process  conditions  during
     all  of the test runs.
            One deviation from standard  testing  procedure was  necessary.
     The  velocity of the exit gas was too low to be  measured by Method  2
     of the Federal  Register.  As an alternative, the  gas velocity was
     measured by igniting a colored  smoke bomb in the  stack and measuring
     the  time required for the smoke to  appear at the  stack outlet.   The
     length of the stack from the sample port to the exit was  known; conse-
     quently, the stack gas velocity could be calculated. Nine such tests
     were performed; the times from  all  the tests were averaged and  this
     average time was used to calculate  the gas  velocity.
            A complete summary of stack  gas conditions and emission  levels
     is given in Table 1.

-------
                                TABLE 1
                          SUMMARY OF  RESULTS
                               FLUORIDES

                           TEXAS GULF,  INC.
                     SUPER PHOSPHORIC ACID 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
if
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, .lb/hour
Fluoride, total, Ib/hour
1
8/29/72
30
30
2.8
80
305
86.813
11.7
11.7
0.002
0.002
0.002
0.002
0.005
0. 005
2
8/29/72
30
30
3.6
82
302
86.279
10.4
10.4
0.002
0.002
0.002
0.002
0.005
0.005
3
8/30/72
30
30
1.5
80
308
86.492
14.8
14.8
0.003
0.003
0.003
0.003
0.007
0.007
Dry, 70°F., 29.92 inches Hg.

-------
III.   PROCESS DESCRIPTION
             Texas Gulf, Inc.  operates two superphosphoric acid (SPA)
      production trains at their Lee Creek, North Carolina operations.
      Emissions were sampled from the south production train only.   Texas
      Gulf, Inc. produces SPA by concentrating 54 percent PpOr phosphoric
      acid to 68-72 percent PpOr-
             In concentrating the acid, 54 percent P^O,- phosphoric  acid
      is continuously fed to the vacuum evaporator.(Figure 1).  The over-
      heads, containing fluorides and water vapor, are condensed in a
      barometric condenser.  The barometric condenser water flows to the
      barometric condenser hotwell  after which it is sewered to the gypsum
      pond.  The .product acid (68-72 percent Pp^c) 1S continuously tapped
      from the evaporator and pumped to the product acid cooling tank  where
      it is cooled before being pumped to storage.
             Fluoride emissions from the barometric condenser hotwell  and
      the product acid cooling tank are controlled by a scrubber.

-------
IV.   PROCESS OPERATION
            The first two test runs  were performed  on  August  29,  1972.  The
     plant operated at design  production rates  during  these tests.   The
     third and final  test was  performed  on  August 30,  1972.   During  this
     test run, the plant operated  at 113 percent of the  design  production
     rate.  The process operated normally throughout the collection  of
     all  samples.

-------
V.  LOCATION OF SAMPLING POINTS
           The sampling sites and number of traverse points were selected
    as per "Method 1  - 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 neces-
    sitated the use of only one traverse diameter.
           Figure 2 is a schematic diagram of the stack configuration near
    the sampling location, and the sampling points traversed during the
    emission tests.

-------
                               FIGURE 2

                         SAMPLE PORT LOCATION
Port
 o
             20 1/2 ft.
           A1
             48 1/2 ft.
                                                        20.5  inches  I.D.
A-A'
Port and
Traverse
Point No.
1
2
3
4
5
6
Distance
From Inside
Stack Wall
(in.)
1
3
6 1/16
14 1/2
17 1/2
19 1/2-
                                 8

-------
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
            Because of such a low flow rate, the velocity could not be
     measured as per Method 2 of the above referenced Federal Register.
            The method used consisted of igniting ~a smoke flare in the
     stack at the sampling port and measuring the time required for the
     smoke to travel the known distance to the stack outlet.
            Several  smoke tests were made before each fluoride test began.
     The average time of nine smoke tests was used to calculate the velocity
     of the stack gases.
            The stack temperature and pressure measurements were also made
     during the 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 two methods was the configuration of the sampling train.
     The sampling train described in the Federal Register has a heated box
     containing the filter holder directly following the glass probe.   The
     sampling train used in these tests contained no heated'box, and the

-------
 filter  holder was placed between the third and fourth impingers  (between
 dry  iinpinger and silica gel impinger) to prevent sample carry over.
 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 referenced 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.
Because of the low  flow rate, it was decided to sample at the AHA of
the meter box (1.65 inches  HpO).   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 im-
pinger 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

-------
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.
       P20r 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, see Appendix C.
                                11

-------
                                  19
Stainless Steel Nozzle
Heated Glass Probe
Glass Connector
Ice Bath
Ircpinger with 100 ml H_0 (Modified Tip)
Iir.pinger with 100 ml H^O (Standard Tip)
lupinger, Dry (Modified Tip)
Inipinger 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 Tioht Vacuum Pump
Dry Test Meter
Calibrated Orifice
Incli ned Manometer
                            17
S-Type
Pi tot Tube
                                                   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
  E_  - Average square root of velocity head, Vinches H20
  AH - Average meter orifice pressure differential,  inches H£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, 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, 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 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)

-------
              EQUATIONS  FOR CALCULATING FLUORIDE EMISSIONS






   VWV =  (0.0474)  x  (VC)


 VSTPD =  (17.71 x  (VM) x (PB +  AH_  ) 4- TM
                                 13.6

    VT =  (VWV) +  (VSTPD)


     W =  (VWV)-r-(VT)


   FDA =  (1.0) -  (W)


FMOIST = 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) -r- (28.99)


    EA =  [(100) x  (% 02  - ^f^)] -7- Qo.266 x % NZ) -  (Z 02 - %2C
     U =  (174) x  (CP)  x  (H)  x V^(TS x 29.92)-i-(GS x PS)


     QS =  (U)  x (AS)


     QD =  (QS) x  (FDA)


  QSTPD =  (QD) x  ( 53°)  x &
                  29.92     TS


   PISO =   (o.oo267 x VC x TS) + (PQ x TS x VM-l-TM)   ~  (Time x U x PS x AN)



Fluoride Emissions:                                                  •


       MG = Milligrams of fluoride from lab analysis


       Grains/SCF =  (0.01543)  x  (MG) -~ VSTPD


       Grains/CF, Stack Cond.  =  (17.71)  x (PS) x (FDA) x  (Grains/SCF) -j- (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 P205 Fed)

-------
FLUORIDE EMISSIONS

-------
                             S.Q.U.RCE TES.T
PLAHT  - TT.XAS GULF  SULFVP
                                           NO  OF PUUS
                                           A ,  11. C.
    SOUP.CF,  -  SUPER  PVOS. ACID (,9.  STAC1')
    TYPF. OP PLAliT -    Super Phosphoric Acid
    C011TROL EQUIPilF.FT -
    POLLUTAI1TS SAl'PLPri -  Fluorides
                                                     -  3
l)RUi\' NUMBER
2 ) DA TE
3) TIME BEG A 11
UPTIME END
^BAROMETRIC PRESSURE, III EG
&)METEh' ORIFICE PRESSURE DROP, III 11 G
i i_ _

1 10:50
J_ 13 : 00
1 30
1 .1.63
7) VOL DRY GAS, METER C011D, CUBIC FEET 1 R7.52H
8) AVER AGE GAS METER TEMPERATURE, DEC
B)VOL DRY GAS, S.T.P. , CUBIC FEET
10)TOTAL 1120 COLLECTED, ML
11) VOL 1120 VAPOR COLLECTED, S.T.P. ,
12) STACK GAS MOISTURE, PERCENT VOLUME
F 1 77 . 9
• JL R 6 . 8 i 3
J_ 52.5
CU FT], 2.H9
1 2.0
13) ASSUMED STACK GAS MOISTURE, PCT VOL \ 5
1H)PERCENT C02
IS) PERCENT 02
lb)PERCL'llT CO
IT) PERCENT 112
IB) PERCENT EXCESS AIR
19)MOLECULAR WEIGHT OF STACK GAS, DRY
2Q)MOLECULAR WEIGHT OF STACK GAS, STK
2DSTACK GAS SPECIFIC GRAVITY

23)AVMAGE STACK GAS TEMPERATURE, DEC,
2S)PITOT CORRECTION FACTOR
2B)STACK PRESSURE, III UG , ABSOLUTE
2DSTACK GAS VEL, STACK COi-JD, F.P.M.
28)STACK AREA, SQ FEET
2V)EFFECTIVE STACK AREA, SQUARE FEET
30)STACK GAS FLOW RATE, S.T.P. , SCFM
3DNST TIME OF TEST, MIHUTES
3 2 )S AMP LIN G UOZ ZLE DIAMETER , 1 1! CUES
33) PERCENT ISOKIIJETIC
3H)FLUORIDE - WATER SOLUBLE, MG
3S)FLUORIDE - TOTAL, MG
3&)FLUORIDE - WATER SOLUBLE, GR/SCF
31)FLUO:UDE - TOTAL, GR/SCF
3B)FLUORIDE - WATER SOL., GR/CF, STK
39)FLUORIDE - TOTAL, CR/CF, STK
HO)FLUO!UDE - WATER SOLUBLE, LB/UOUP
HI) FLUORIDE - TOTAL, LB/UOUR
«42)P20S FED - TOi:S/!!OUR
H3)FLUORIDL' - VAT EX SOL., LB/TOi! P205
HH)FLUO!UDE - TOTAL, LB/TOi! P205
1 	
1 — _
1 - _
i 	
10 	
J_ 28.85
COIJDi 28-55
j_ o . a R
1 	
F J[ 80. 3
^
I 6~. 83
J_ 30
i r5"o . ,T
j^ 2". 7"7"
I

i
I
I
|
1
I
I
I
|
I
|
1
I
1
1
I
I
|
|
I

_[
j_
j^
_[
I
I
|
_[
I
—1
j^
	 J_
pr.-mrTi 	 j
CUD. l"T'2±£"IIIl
CUD. IJ^^I^
1 nr.njrrT) 'f^
• 1 1 ."fTTnr^P
i
.......t

I
1
FED l_p_. 	 1
FED 1. - — ~
I
?- - 1
rt_£? 0^-70 _[
i i'r • a 5 1
10:^5 	 1
30 _[
IJ.GH _ _1
87^6113 J.
02 	 j,
no A.27n _[
67.8 J_
3^21 J.
3^6 	 1
5 	 __1
	 1_
	 _1
_ 1
1
°- «1
28.85 _[
28.46 _[
0.98 J_
i
0 2.3 J_
_[
0.83 _[
30 J_
139 3 J.
2«_2°_ _- 1
.' . 29 I
s-sr — — '~-L
J.
(7*. 5~ i
' _' • 	 _[_
iij ~r i
^•"^ 	 j__
~Tr.~tTT71.T1 	 4~
~T7Y~7m~n ' i~
1 V J ' '_^' 	 . .i __
_^j __!_ L, 	 L_
'" run7' o j^
- _. _ 1
1
• 	 i
3
n/3
11 :
13 :
30
1. R
87 .
82
86 .
2 7 .
1. 3
1 . 5
5




0
20.
28 .
0 ,"?j

ffO

1) .1]
37)
13.2..

	 1

00 i
00 J_
1
.! __ 1
n c o i
1
'192 |
-° 1
2 1
1
._ _ i
1
_ [
._ _„!
1
.- _ 1
05 J_
J.
n 1
1

J_
?' 1
1
3_ - 1
: __ i.

TfTiTi
71 /-T!
ir:"5

.- 'r . •
j."*f . '
%£
1, ,
-(Sj— ^f


^- '* -

t
. _ _ 1
j_
	 L,
J.
^ 	 _[
J^"~Il
^ 	 J
_^j 	 L
[i
'.' i
js
Jl
- J1
***S.T.P. •<->/)/? Y ,  70
                           F,  29.92  IKCIIES MERCURY***

-------
APPENDIX  B



Field Data

-------
Plan lg<(ti
                                               Gainesville, Florida
                                         SOURCE SAMPLING FIELD DATA SHEET
                                         /?
Sampling Location
                            /?c.i &_ C5*
                   Run  No.
Time Start  /&3O  Time  End
                       /-/r/>;
Sampling Time/PointJ
D8      °F,  WB     °F,  VP  (?  DP
                                      _"Hg
                                                  Sketch of Stack
                                                      ff/
Bar-  Press.
Moisture 5
We a t h e r _
Temp. __ __
            %,FDA
                 11 Hg,Stack  Press._£o__"Hg
                    __,Gas  Density  Factor__
               //y
            F,  W/D
                        ,W/S
Sample Box No.   5   Meter Box  No.	5_	
Meter AH@_/j*5>itot Ccrr.  Factor    Q. S3
Nozzle Pi a. ^.Jfo'n., Probe Length    4—   ft
Probe Heater Setting Zl>% Nomograph  Cf  Q. 77
Stack Dimensions	2.O.!D	in
Stack Area       	'^±^^L	ft2
Stack Height     2.0• 6  / $-c!»^>	ft
                                                           ~t
                                                               I
Mat'l Processing Rate
Final Gas Meter Reading
Initial Gas Meter Reading
                           <3 / & ,  /33  ft3
                                                                                                                     ftj
                                                                                                       Filter No
Condensate Increase in Impingers
Moisture in Si 1 ica Ge 1	/S.,";
Silica Gel Container No,
Orsat:  C02	
        02 	
        CO
                                                                                                                     ml
                                                                                                                     9m
                                                                                 2.
                                                                             Excess
                                                                                Air
                                                                        Test Conducted by:
                                                                        Remarks:
Port and
Traverse
Point No,
/4W #/
/^. A
2
* 3
4-
$
(*
Distance
From Inside
Stack Wall
(in.)
/
3
& fa
///2
/7^
/9^/z
Clock
Time
/030
MJO
J/30
/^oo
£2ZO
J24-& LJ
/3^D
Gas Meter
Reading
(ft3)
*
7Z&.&/4-
74 3 .3
—
77^-2
78£>~£
8o/.o
B!(**/38
Stack
Velocity
Head
("H20)
tf, cf»/7
—
—
—
—
__
^_
Meter
Orifice
Press. Diff.
("H20)
Calc.
—
—
._
—
—
—
Actual
/;^5
/^
/.&o
[A^G
/, ^
/ ^
Stack Gas
Temp.
(°F)
_&f .
^5
74-
74
,.~"r,
/D
•Pf;
Gas Sample
Temp. @ Dry
Gas Meter
(°F)
In
5b
,-fc
75
7<
' /^~.
77
Out
80
So
78
78
?&
73
Sample
Box
Temp.
(°F)

—
—
—
—
^_
—
Last
Impinger
Temp ,
(6F)
S ^
/ '
(" ';•
& -
/ '
/• *
' "} '
£ .• '"
Vacuum
on
Sample
Train
("Hg)
o
/
/£
/#]
/Z
/£'
1/2
                                               /I34
                                                       -M4-4-

-------
                                        •PI/1 RUPNTA^RG i rUft NG flic.
                                               Gainesville, Florida
                                         SOURCE SAMPLING  FIELD DATA SHEET
Plant  *T
Sampling Location __$>.-
Da te-R u n No
                            Z.
Time Start/^,4jJ"  Time End /^.'
Sampling Time/Point_
        °F,  WB      °F, VP @ DP
                                                  Sketch of Stack
                                      "Hg
Bar-  press.  ffo  "Hg,Stack Press..,j?j±L_"H9
Moi s ture_Jif_*, FDA	 ,Gas Dens i ty Fac tor__	
Weather	Q^i/J^	
Temp.	°F>  W/D	,W/S	_'	
Sample Box No.	Meter Box No.	
Meter
Nozzle Dia.,
                     Corr.  Factor^?/
             i9_in.,  Probe  Length	
                                         ft
Probe Heater Setting	Nomograph Cf	
Stack Dimensions      £• & * ^	in
Stack Area            2.29	^t2
Stack Height     	   	ft
                                                                       Mat'l Processing Rate
                                                                       Final Gas Meter Reading
                                                                       Initial Gas Meter Reading
                                                                                                    o. 3.
                                                                                                      - 13
                                                                                                      F liter
                                                                       Condensate Increase in Impingers
                                                                       Moisture in Silica Gel    "   /6i B
                                                                       Silica Gel Container No ;
                                                                       Orsat:
                                                                               02
                                                                               CO
                                                                               C02
                                                                            Excess
                                                                               Air

                                                                       Test Conducted by:
                                                                        Remarks :
                                                                                                * V ' Vo
                                                                                                                   ml
Port and
Traverse
Point No.
fl£J
v „
/
2
J
i
s
i
Distance
From Inside
Stack Wall
(in.)
i
t





Clock
Time
/V.*T
f*'°S~}
tf/,£
Hfi 3
gl^^L 1
38%3

Stack
Velocity-
Head
("H20)
a en?'7!
	
. — .
^
—
--
—
Meter
Orifice
Press. Diff.
("H,0)
Calc.
-~
^^
-
-
, —
—
Actual
/^r
/^r
/.o-
A^
/
-------
                                              IR W NT/^fc I lIHl N
                                               Gainesville, Florida
                                          SOURCE  SAMPLING  FIELD  DATA  SHEET
Samp! i ng Locati on y^
Date  ^> -30'72, Run No.
Time
                     Time End  /<->»
Sampl i ng Ti me/Poi nt <£?£>^'
DB
F, WB
F, VP @ DP
                                       "Hg
Bar- press..tJo__"Hg,Stack Press. «Zfo	"Hg
Moisture_vJ:Pjc,FDA_	,Gas Density Factor_
Weather  . C._/-€a /^.
Temp.
  T, W/D
    ,W/S
Sample Box No.__>5^_Meter Box No.__J;f
Meter AH@/£^(f_Pitot Corr.  Factor
Nozzle Dia.A^^Jn., Probe Length
Probe Heater Settin
Stack Dimensions 	
Stack Area       	
Stack Height '    	
                                          ft
              /^Nomograph Cf €>-?"?

                                          in
                                          Sketch  of  Stack
Mat'l Processing Rate_
Final Gas Meter Reading
Initial Gas Meter Reading ^p3,
Condensate Increase in Impingers	
Moisture in Silica Gel	/ 7... <-{
Silica Gel Container No,. 4£*  Filter
Orsat:
                                                                                        /Q_
                                                     Test Conducted by :
                                                                                            c L /•••/./_
                                                                                                   Do LL
                                 - 4$,
                               _ft2
                                 ft
                                                                         Remarks ;
                                                                                                             ml'
                                                                                                             gm
: C07 \
o? i
CO
N2"
Excess
, Air



1 1








;




/ ? /> n ^/~ fa /-, 1
,/_'•<<* 1 L-'o-,'* C J
Port and
Traverse
Point No.
$: 7
t
5
4
X
"?
^
Distance
From Inside
Stack Wall
(in.)
/
^
& '//I,
14- l/z
J3. & \

Clock
Time
1 1*' 00
UL%°
//>'^°
/2, C/73
/z: -L^
12^^/0
Gas Meter
Reading
(ft3)
qj^ltlj
.^ '
-l$, ^
1^'J. $
1J&< 7_

Stack
Velocity
Head
("H20)
C5 O'Ol 7
. —
—
—
~-
L—
— .
Meter
Orifice
Press. Diff.
Calc.
—
—
—
—
—
_
Actual
/• 65
/. £s
/.6-f
Stack Gas
Temp.

80

/, if \ 8°
l&
/<^s-
So
ffo
Gas Sample
Temp. @ Dry
Gas Meter
In
ft C~S
CiJ *7
83
S3
ft 3

Out
0 o
fft
8 2-
g-?~
$2-
$3
Sample
Box
Temp.

—
— .
~
— .
— .
f—
Last
Impi nger
Ternp .
& o
7*

(> &
7 &
7o
Vacuum
on
Sample
Train
("Hg)
L,^ * ^J
6
6
&
£


-------
GRAB SAMPLE DATA

-------
I   I
                   T - C-
                      -*
                     Mo.
              o,
 I
                                                   1
       Dafe.
                                \ )-^ V-,cu «-,
                  Q «  .x.
                  roiv\T
\"\ -
IT <-\ (\ ^A^fc
        pluoricfes
               AUtals

-------
           \ -dr
                       r^»
        *k- Mo.
Run  Wo,
          Pom"t"
 Pa Os
Trace. AUtals

-------
                               c)v
          EPR
            Mo.
               Wo,
                                        1
          Dafe.
           iwe.
                                           ' A <
S
                                          \\-*\
                                 S5S
                                  A
   i-A
4LB.
!   u
                                                           u
           Re.tAfi.rks

-------
            T  0-    T
             » •  ^ -    o-
EPA  Sarnie,  tfo.
Ruvt  Mo.
L
                  r    i
                  «-*>•-»« PcS-t'TC
                         Vo <, Ac. >
                         u
Vis   !  \.A
        \-4
        AUtals
 Re^iUrks

-------
                               •)
                               *—
EPA
Mo.
Run  Wo.
Daf
  we.
           j -^ S>p^>->..
                               A
JfUi
 fluort'cle.s
        Me.1v\(
s

-------
    ani
EPR
Run Wo.
 ae.
           V°F
   H
 P^ Os
 Reworks

-------
           \"l.
           Os
EPA
o.
Run  No.
Dafe.
«™
hwe.
                        V
                      \A
                                 M.S

-------
          v--r—

           v
                          x>
                          H—
E.PA Sam^k  Mo.
Run  Wo.
S
  av
                      ~\ e v
 PH
Trace, AUt^ls
  u2.vwks

-------
            T-C-.
                O
                   - v X 4-  \r-v-"-"
EPA Sa«  ie. f/o.
Run Wo.
Dafe
fjj
  ^
Trace.

-------
          T-C-.  T.
                       >tK,  \ \
EPA Sample. No.
     Mo,
Dafe.
      M<7  Pe>iv\1"
   H
   Os

-------
             \
-> ^ P c *~ r**- ^
F-\L^^c ft
*\\_ *~~)
^
             f/0.
      o,
                          3
 ime-
                                     \
          ure
PH
  ,'evAArks

-------
            75 <-^-0 iv  Y\ »- ^ 
-------
         APPENDIX   C



Standard Analytical Procedures

-------
                        ENVIRONMENTAL PROTECTION AGENCY

                     Research Triangle  Park,  North  Carolina   27711

Reply to                     '
 Ann of:                 •                                             n ,          '
    J                              '                                Date:  12-21-72

 Subject:  Summary  of  Fluoride Analysis

   *y-
    °:  R.* Neulicht,  EMB,  IRL
            This memorandum  is  in  response  to your  request  for  a brief
        summary of our SPADNS-Zirconium  Lake procedure  for determination
        of  fluoride in stack  emission samples.

            Samples received in our laboratory  are  filtered through
        fluoride free paper filters to yield water soluble and water insoluble
        portions.  The water  insoluble particulate collected on.  the  filter
        is  rinsed throughly to be sure that  all  water soluble fluoride is
        rinsed through.  The  water  soluble fraction  is  distilled from sul-
        furic acid to a maximum -temperature  of '180 C.    If chloride  is suspected
        in  the sample Ag So .  is  added to the still.  SPADNS  solution is added
        to  an aliquot of the  distillate  and  the  absorbance is read at 570  nm.
        The concentration of  the sample  is determined from a calibration curve
        prepared from standard fluoride  solutions.   It  is very important that
        the temperature of the samples be the same as that of the standards
        when absorbances are  recorded.

           • The water insoluble fraction of the sample is evaporated to dry-
        ness in the presence  o±  a slurry or  CAU,  and then lustd  will* IJACII.  TIi£
        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, QAEHL
        cc:.  R. E. Lee

-------
                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.         «•             •
                                     •    .                 <>
     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

-------
    APPENDIX   D
Project Participants

-------
                       PROJECT PARTICIPANTS
                  Environmental  Engineering, Inc.
Name                                        Title
John R.  Dollar, E.I.T., M.S.E.              Project Manager
George Allen                                Environmental  Specialist
Marvin Hamlin                               Environmental  Specialist

                  Environmental  Protection Agency
Name
Roy Neulicht
Lee Beck
Andrew Tremholm

-------