SOURCE TEST REPORT
        ON MEASUREMENT OF EMISSIONS FROM
          OCCIDENTAL CHEMICAL COMPANY
            WHITE SPRINGS, FLORIDA
                      FOR
       THE ENVIRONMENTAL PROTECTION AGENCY
            UNITED STATES GOVERNMENT
             REPORT NO.  73-ROC-3
             <>ni iron iiii'ii f
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                                 SOURCE TEST  REPORT
                           ON MEASUREMENT OF EMISSIONS FROM
                             OCCIDENTAL CHEMICAL COMPANY
                               WHITE SPRINGS,  FLORIDA
                                         FOR
                          THE ENVIRQNMENTAL PROTECTION AGENCY
                              UNITED STATES GOVERNMENT
                                REPORT NO. 73-ROC-3
environmental science and engineering, inc.

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                        SOURCE TEST REPORT
REPORT NO:   73-ROC-3
PLANT TESTED:  OCCIDENTAL CHEMICAL COMPANY
               WHITE SPRINGS, FLORIDA
EMISSIONS FROM:  PHOSPHATE ROCK DRYING
           '      AND GRINDING PROCESSES
TESTOR:  ENVIRONMENTAL SCIENCE AND ENGINEERING, INC.
         P.O. BOX 13454
         UNIVERSITY STATION
         GAINESVILLE, FLORIDA  32604
CONTRACT NO:  68-02-0232, Task Order 12, Task Change No. 3

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                         TABLE OF CONTENTS
                                                                Page
INTRODUCTION                          .      •                      1
SUMMARY OF RESULTS                                                3
PROCESS DESCRIPTION                                              16
LOCATION OF SAMPLING POINTS                                      18
PROCESS OPERATION DURING TEST                                    26
SAMPLING AND ANALYTICAL PROCEDURES                               28

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                                              f
                           INTRODUCTION

Rock Drying
   ;        I
       Fluoride and participate emission tests were performed at the
phosphate rock drying operation located at the Occidental  Chemical
Company, White Springs, Florida.   Environmental Science and Engineer-
ing, Inc. of Gainesville, Florida performed the emission tests while
EPA personnel gathered plant process data.  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.
       All emission tests were performed simultaneously at the inlet
and outlet:of the Dorrco Cyclonic Wet Scrubber.  Fluoride emissions
           i.
were determined by a method currently being studied by the EPA, and
particulate emissions were determined by the EPA Method No. 5 (Federal
Register. Vol. 36, No. 59, August 17, 1971, Wash., D.C.).   Triplicate
tests were performed at all sampling sites.  The fluoride tests were
performed ;on December 19 and 20, 1972; and the particulate tests on
December 21, 1972 and January 9, 1973.
       Grab samples of the scrubbing liquids, the process reactants,
and the process products were analyzed for fluoride and P20s content
by the EPA.

Rock Grinding
       Particulate emission tests were performed at the phosphate rock
grinding operation located at the Occidental Chemical  Company, White
Springs, Florida.  Environmental Science and Engineering, Inc. performed
                               1

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the emission tests while EPA personnel gathered plant process data.
The purpose of the test was to obtain data for the use of both the
           i
Industrial Studies Branch and the Performance Standards Branch of the
EPA.                                                    .
       All particulate emission tests v/ere performed simultaneously
at the inlet and outlet of the Micro-Pulsaire Bag Collector on the
K.V.S. Ball Mill.  The test method used was EPA Method 5 (Federal
Register, Vol. 36, No. 59, August 17, 1971).  Triplicate tests were
performed at all sampling sites. . The tests were performed on January 11
and 12, 1973.
       Grab samples of the process reactants and process products
were analysed for trace metals, mercury, and fluoride content by the
EPA.

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                       SUMMARY OF RESULTS

Rock Drying
          Summarized results of the fluoride and particulate  emission
tests are shown in Tables 1  through 4.   Complete results  are  included
in Appendix A-l.
          During the preliminary investigation of stack gas velocity
profiles, an attempt was made to determine the magnitude  of tangential
flow in the outlet stack.  To do this,  a standard and S-type  pitot tube
were rotated 180ฐ at several points across the stack diameter to measure
the maximum velocity head reading.  No  appreciable difference could be
detected whether the pitot tube was parallel to the gas flow  or at some
angle to the flow.
          Based upon the difference in  inlet and outlet gas flow calcu-
lations, there possibly was some effect from tangential flow in the
outlet.  A comparison of the two average flow rates indicates that the
outlet was approximately 38 percent greater than the inlet.
          The velocity measurements for the inlet seemed fairly uniform;
therefore, the emission rates for the outlet were also calculated on
the basis of the flow rates calculated  from inlet measurements (see
Appendix A-l.
          Fluoride emission rates were  calculated by using the sample
recovered from the nozzle through the filter portion of the sampling
train.  The emissions were separated into insoluble and soluble fluoride
emissions.

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          Particulate emission rates were calculated by using the sample
recovered from the following portions of the sample train:  1) acetone
rinse of nozzle through front half of filter holder (Front Half); 2)
           i
in some cases, a water rinse of the front half; 3)  filter; 4) impinger
contents plus a water rinse of the back half of the filter holder through
the dry impinger that precedes the impinger with the silica gel  (Back
Half); 5) ether and chloroform extraction of organic matter contained in
No. 4 mentioned above; 6) acetone rinse of the back half after the water
rinse has been made.
          A water rinse of the front half was made, in some cases, after
the acetone rinse and brushing was performed.  The  reason for this was
to remove particulate matter that was visible after the acetone rinsing
and brushing.  This procedure was acceptable to the EPA test officer since
it followed the acetone rinse.
          Grab samples of the stack gases at each sampling site were
obtained by an Orsat analyzer, and the concentrations, of carbon dioxide,
          i
oxygen, and carbon monoxide were determined.  Analyses were made while
the dryer was on natural gas and while it was on fuel oil.
          Tables 5 and 6 contain the results of the laboratory analyses
performed ;on the grab samples from the process reactants and products,
and the scrubbing liquid"respectively.
          A complete set of the Appendices is available in the EPA
Emission Measurement Branch report files, listed under Report No.
73-ROC-3.,

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                                       . -_>!... .'I, .  '
                                                          jf"
                                                  -"•  ."       TABLE - 1   '

                                                  •   fifiJJSCE Cl'I2ฃZGil 2S5
TEST nUHRFR
PI. APT 11 A! IE
SOURCE TESTED
TYPE OF PLANT
73-ROC-3


OCCIDENTAL CHEMICAL CO.
DRYER SCRUBBER INLET
PHOSPHATE
ROCK DRYING

COIITROL EQUIPMENT- LIQUID SCRUBBER __
POLLUTAUT SAMPLED- FLUORIDES
rjflwr TWHBER
2)DATE
3)TIME BEGAN . . .
t iritiF END ' " '••.:'••
5 )T - UFT TIl'.E OF TEST, HIIWTFS
. 6)PP- BAROMETRIC PRESSURE, Itl IIG
DPS- STACK PRESSURE, It! KG
B)ฃ>H- GAS tlTR ORIFICE PRESS DROP, "820
9)TW -GAS HETER AVG TEMP, DEG F
• 10 )VC -TOTAL K20 COLLECTED. ML
iDvi'v-voL mo VAPOR COLT...CU FT.STP
12)VM -VOL DR? GAS SAMPLED ,CU FT ,HTR COtlD
13)VSTPD-VOL DRX GAS SAMPLED, CU FT.STP
IH)V(PCT)- STACK CAS MOISTURE ,PCT VOL
\S)TS- AVG STACK GAS TEMPERATURE, DEG F
16)C02-STACK GAS 002, PCT VOL
17) 02-STACK GAS 02 ," "
18) CO-STACK GAS CO, " ••
19) 112-STACK CAS 112 , ' ' ' •
20) FA-STACK GAS EXCESS AIR. PCT VOL
21)HD - STACK GAS MOLECULAR WEIGHT, DRZ •
22)MS - STACK GAS MOLECULAR VGHT ,STK COUD
23)GS - STACK GAS SPECIFIC GRAV ,REF AIR
2U) n - AVG SPUARE ROOT VEL HEAD," J120 '
2S)AVG SQUARE ROOT(STK TEMPxVEL HEAD)
26)CP - PITOT TUBE CORRECTION FACTOR
. -2.7) U - STACK GAS VELOCITY , FT/MIN
28) AS- STACK AREA, SQUARE FEET • .
29)AS'- EFFECTIVE STACK AREA, S(> FEET
3Q)QS - STK GAS FLOW RT ,CV FT/MIN.STK CUD
3DQSTPD-STK GAS FLOW RATE ,CU FT/tllll ,STP. ;•
32 )Dll - SAMPLING IIOZZLE DIAMETER, IN ••
331AI1 - SAHPLIllG IIOZZLE AREA, SQ FT
3H)PCT ISO-ISOKIfJETIC SAMPLING. PERCENT
35) FEED RATE, TONS/HOUR -
• 36) FLUORIDE EMISSIONS, WATER SOLUBLE
MILLIGRAMS
GRAINS/SCF
GRAINS/ ACF
LBS/HOUR1
LBS/TON OF FEED
37) FLOURIDE EMISSIONS, TOTAL
MILLIGRAMS
GRAINS/SCF
GRAINS/ACF
• LBS/HOUR
LBS/TON OF FEED
38) FLOURIDE EMISSIONS, % INSOLUBLE
39) P,0,, WATER SOLUBLE, KG
40) P,OJ?, TOTAL, MG
41) P,0c, % INSOLUBLE
T .
12/19/72
14:22
17:21
120
29. 9^
29.6
0.350
81.7
263
12.47,
41.160
40.277
23.6
169
2.00
17.4
.0.00
80.6
N.A.
29.0
26.4
0.911
0.834
20.9
0.830
3180
33.75
33.75
107,500
68,400
0.1)88
0.000192
80.4
285

14.4
O.OP552
0.00351
3.22
0.0113

34.3
0.0131
0.00837
7.6S
0.0269
58.0 • -
86.4
236.4
63.5
AND PgUg
12/20/72
09:53
12:13
120
29.9
29.6
0.480
74.3
553
26.22
49.640
49.263
34.7
173
2.00
17.4
0.00
80.6
N.A.
29.0
25.2
0.870
0';825 •
20.8
0.830
3230
33.75
33.75
109,300
59,000 .
0.188
0.000192
122
280

1.50
0.000547
0.000254
0.260
0.000929

40.4
0.0127
0.00684
6.43
0.0229
96.3
7.4.
347.4
97.9
: ...
- - 3 	
12/20/72
14:45
17:05
120
29.9
29.6
0.410
85.5
460
21.79
48.180
46.823
31.8
171
2.00
17.4
0.00
80.6
N.A.
29.0
25.5
0.880
0:817
20.5
0.830
3180
33; 75
33.75
107,350
61 ,000
0.188
0.000192
113
285

1.30
0.000428
0.000240
0.210
0.000737

36.1
0.0119
0.00674
6.20
0.0218
96.4
4.2
291.7
98.6
                                                                                                   120
                                                                                                   29.9
                                                                                                   29.6
                                                                                                   0.413
                                                                                                   80.5
                                                                                                   425
                                                                                                   20.2
                                                                                                   46.327
                                                                                                   45.454
                                                                                                   30.0
                                                                                                   171
                                                                                                   2.00
                                                                                                   17.4
                                                                                                   0.00
                                                                                                   80.6

                                                                                                   29.0
                                                                                                   25.7
                                                                                                   0.887
                                                                                                   0.825
                                                                                                   20.7
                                                                                                   0.830
                                                                                                   3200
                                                                                                   33.75
                                                                                                   33.75
                                                                                                   108,000
                                                                                                   62,800
                                                                                                   0.188
                                                                                                   0.000192'
                                                                                                   105
                                                                                                   283

                                                                                                   5.73
                                                                                                   0.00217
                                                                                                   0.00133
                                                                                                   1.23
                                                                                                   0.00432

                                                                                                   36.9
                                                                                                   0.0126
                                                                                                   0.00732
                                                                                                   6.77
                                                                                                   0.0239
                                                                                                   83.6
                                                                                                   32.7
                                                                                                   291.8
                                                                                                   86.7
*** S.T.P. - DRY, 70ฐF, 29.92 in Hg

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                                          TABLE - 2




                                 S.QU3.CS. C/JI22ZGE  ฃฃฃฃ
TEST NUMBER '-. 73-ROC-3 - J '
•'• PI.AVT NAME - OCCIDENTAL CHEMICAL CO. WHITE SPRINGS, FLA. .
SOURCE TESTED - ROCK DRYER SCRUBBER OUTLET (FLUORIDES)
rrpr OF PLANT - PHOSPHATE ROCK DRYING
CONTROL EQUIPMENT- LIQUID SCRUBBER .....
" 	 ' POLLUTAl.'T SAMPLED- FLUORIDES AND PgOg
1 )RUil I'UMRER
3)rr;.r BEGAN .
H)TIME END
5 )T - f!ET TIME OF TEST , MINUTES
6)PB- BAROMETRIC PRESSURE, IN RG
7)PS- STACK PRESSURE, IN P.G
*)LF.- GAS MTR ORIFICE PRESS DROP, ' 'R20
9)TW -GAS METER AVG TEMP, DEC, F
10 )VC -TOTAL !J20 COLLECTED, ML
11 )Vl.'7-VOL 1120 VAPOR COLL..CU FT,STP
. 12)VM -VCL DRY GAS SAi-lPLED ,CU FT , MTR COIID
13)VSTPV-VOL DRX GAS SAMPLED, CU FT ,STP
1>*)W (PCT) -STACK GAS MOISTURE , PCT VOL
1S)TS- AVG STACK GAS TEMPERATURE, DEC F
16)C02-S?ACK GAS C02 , PCT VOL
17) 02 -STACK GAS 02 , • • • '
18) CO-STACK GAS CO , " "
19) N2-STACK GAS //2 , ' ' • '
20) FA-STACK GAS EXCESS AIR, PCT VOL
21)//0 - STACK GAS MOLECULAR WEIGHT, DRY • ,
22)MS - STACK GAS MOLECULAR WGPT ,STK COIID
23)GS - STACK GAS SPECIFIC GRAV ,REF AIR
2U) H - AVG SPUARE ROOT VEL HEAD," H20
~ " 25)AVG SOUARE ROOT(STK TEMP*VEL HEAD)
26)CP - PITOT TUBE CORRECTION FACTOR
27) U - STACK GAS VELOCITY, FT/MIN
28) AS- STACK AREA, SQUARE FEET . •, . ;
29)A5'- EFFECTIVE STACK AREA, SO. FEET ' .'• ••
30 )P5 - STK GAS FLOW RT ,CU FT/MIN.STK CND
j 3DQSZPD-STK GAS FLOW RATE tCU FT/MIlltSTP
1 - 32 )DN - SAMPLING NOZZLE DIAMETER, III • v .•_
33)AN - SAMPLING NOZZLE AREA , SO. FT ' •
. 3ซ*)PCT ISO-ISOKINETIC SAMPLING, PERCENT
i ' ' ' ......
' 35) FEED RATE, TONS/HOUR
; 36) FLUORIDE EMISSIONS, WATER SOLUBLE
MILLIGRAMS
. . GRAINS/SCF
GRAINS/ACF
.. LBS/HOUR1
LBS/TON OF FEED
37) FLOURIDE EMISSIONS, TOTAL
' MILLIGRAMS
GRAINS/SCF
GRAINS/ACF
LBS/HOUR
1 LBS/TON OF FEED
38) FLOURIDE EMISSIONS, % INSOLUBLE
ซ ' 39) P,0,, WATER SOLUBLE, MG
? • 40) P,0^, TOTAL, MG
' 41) P,0ฃ, % INSOLUBLE
H .
12/19/72
14:20
. 17:18
132
29.9
29.9
0.620
77.6
423
20L05
59.486
58.693
25;i5
154.0
2.00
17.5
0.00
80.5
N.A.
29.02
26.21
0.904
0.507
12.567
0.830
1910
77.24
77.24
147,500
94800
Oi!250
0:000341
106.1

285

1.20
0.000315
0.000203
01260
0,000912

12.6
0.000331
0:000213
0.273
0,000958
4,76
2.4
2.46
2.44

2 	
12/20/72
09:30
12:18
132
29.9
29.9
0.490
76.8
393.5
18.65
51.449
50.813
26.8
154.4
2.00
17.5
0.00
80.5
N.A.
29.02
26.06
0.899
0.445
11.033
0.830
1680
77.24
77.24
129,800
81800
d;250
0-000341
106.5

280

0.50 ,
0.000152
0.0000958
0.106
0.000379

1.10
0.000334
0.000206
0.232
0.000829
54.5
2.3
2.6
11.5

	 y 	
12/20/72
14:40
17:13
132
29.9
29.9
0.560
82.9
424.9
20.14
56.373
55.069
26.8
154.7
2.00
17.5
0.00
80.5
N.A.
29.02
26.07
0.899
0.48
11.905
0.830
1810
77.24
77.24
140,000
88,400
0.250
0.000341
106.9 ';

285

0.40
0.000112
0.0000706
0.085
0.000298

0.80
0.000224
0.000141
0.170
0.000596
50.0
2.1
6.5
67.7

AVer age
N.A.
N.A.
N.A.
132
29.9
29.6
0.557
79.1
414
19.61
55.8
54.9
26.4
154.4
2.00
17.5
0.00
80.5
N.A.
29.02
26.1
0.900
0.477
11.8
0.830
1800
77.24
77.24
139,100
88300
0.250
0.000341
106.5

283

0.70
0.00019:
0.00012:
0.150
0.000531

4.83
0. 000291
o.ooois;
0.225
0.00079'
36.4
2.27
3.85
27.2
*** S.T.P.  -  DRY, 70ฐF, 29.92 in Hg

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                                               TABLE - 3
                    TEST  NUMBER
                    t>r,APT NAiir.
                    SOURCE TESTED
                    rypE  OF PLANT
                    CONTROL EQUIPMENT-
                    POLLUTAUT SAMPLED-
73-ROC-3                                :
OCCIDENTAL CHEMICAL CO.    WHITE SPRINGS  FLA.
DRYER SCRUBBER INLET (PARTICULATES)
PHOSPHATE ROCK DRYING
LIQUID SCRUBBER
PARTICULATES
nUvTl UUHBFR
2)DATE • . . .
3 )T IMF BEGAN
*)TinE END
5)T - NET TltfE OF TEST , MINUTES
G)Pfl- BAROMETRIC PRESSURE, Ill HG
7) PS- STACK PRESSURE, III EG
P)i//- GAS UTR ORIFICE PRESS DROP. "H20
<3)?n -CAS HETER AVG TEMP, DEC, F
10 )VC -TOTAL H20 CO LT.FCTED , ML
.\DVVV-VOL 1120 VAPOR COLL..CU FT.STP
12)V!1 -VOL DRY GAS SAMPLED ,CU FT ,UTR COND
13y.'STPD-VOT, DRY GAS SAMPLED, CU FT tSTP
lny./(PCT)-STACK CAS 110ISTVRE ,PCT VOL
15)75- AVG STACK CAS TCllPFRATURE , DEC P
16)C02-STACK GAS C02 , PCT VOL
17) 02 -STACK GAS 02 , •• ••
18) CO-STACK. GAS CO , ' ' • •
19) U2-STACK GAS 112 , " '•
20) r.A-STACK GAS EXCFSS f.IR , PCT VOL
21 )//D - STACK GAS HOLFCULAR HEIGHT, DRY •
22)113 - STACK GAS HOLECULAP VGfiT ,STK C011D
23)GS - STACK GAS SPECIFIC GRAV ,REF AIR
' 2U) U - AVG SMART. ROOT VF.L HF.AD," F120
2S)AVG SQUARE ROOT(STK TZHPxVFL HEAD)
26)CP - PITOT TUBE CORRFCTI011 FACTOR .:
27) V - STACK GAS VFLOCITy , FT/HIfl
• • 28) AS- STACK AREA, SGUARF FEFT
23)AS'- EFFECTIVE STACK AREA, SO FEET
• 30)Q5 - STK GAS FLOW RT ,CU FT/HIll.STK CUD
3DQSTPD-STK GAS FLOW RATE ,CU FT/HIIt *STP
•32)W/ - SAMPLING NOZZLE DIAMETER, IN
33 )All - SAMPLING NOZZLE AREA , SQ FT .
3"*)PC2- ISO-ISOKINETIC SAMPLING, PERCEUT
35) FEED RATE, TONS/HOUR
36) PARTICULATE EMISSIONS; PROBE, CYCLONE,
AND FILTER CATCH
MILLIGRAMS
GRAINS/SCF
GRAINS/ACF
LBS/HOUR
LBS/TON OF FEED
37) PARTICULATE EMISSIONS, TOTAL
MILLIGRAMS
i GRAINS/SCF
GRAINS/ACF
LBS/HOUR .
. . LBS/TON OF FEED
38) PARTICULATE EMISSIONS, % IMPINGER CATCH
1
12/22/72
9:25
11:58
120
29.9
29.6
0.300
73.6
429
20.33
40.180
39.911
33.8
172 -
2.00
17.4
0.00
80.6
N.A.
29.02
25.30
0.873
0.827
20.789
0.830
3230
33.75
33.75
109,000
59,900
0.188
0.000192
97.6
280


1278.9
0.494
0.271
253.89
0.907

1318.0 -
0.510
0.280
261.65
0.934
3.00
2
1/9/73
10:00
13:12
120
29.9
29.6
0.390
43.8
212
10.05
43.590
45.868
18.0
165 ..:-'
4.20
15.0
0.00
80.8
N.A.
29.27
27.25
0.940
0.826
20.648
0.830 ..
3090
33.75
33.75 .-.
104,400 :
71 ,800
0.188
0.000192
93.6
215


. 490.2 .
0.165
0.113
101.51
0.472

555.2
0.187
0.128
114.97
0.535
11.7
3
1/9/73
15:10
17:55
120
29.9
29.6
0.450
51 iO
408
19.34
46.500
48.246
28.6
168
4.20
15.0
0.00
80.8
N.A.
29.27
26.05 •
0.899
0.841
21.058
0.830
3230
33.75
33.75
108,900
64,900
0.188
0.000192
108
235


1337.7
0.428
0.255
238.09
1.013

• 1419.9
0.454
0.271
252.72
1.075
5.80
Average
N.A.
N.A.
N.A.
120
29.9
29.6
0.380
56.1
350
16.5
43.400
44.675
26.8
168
3.47
15.8
0.00
80.7
N.A.
29.19
26.20
0.904
0.831
20.8
0.830
3180
33.75
33.75
107,400.
65,500
0.188
0.000192
99.7
243


1035.6
0.362
0.213
197.83
0.797

1097.7
0.384
0.226
209.78
0.848
6.83
*** S.T.P. - DRY, 70ฐF, 29.92 in.  Hg

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                                                TABLE -  4
                                     SC4JSCE
rrsr IIUMBER - 73-ROC-3 .j '• . . -
PI.APT 11AIIF. - OCCIDENTAL CHEMICAL CO. WHITE SPRINGS, FLA.
SOVRCT TESTED - DRYER SCRUBBER OUTLET (PARTICULATES)
TYPE OF PLANT - PHOSPHATE ROCI<: DRYING
CONTROL EQUIPMENT- LIQUID SCRUBBER ' . .
POLLUTAKT SAMPLED- PARTICULATES
• 	 " ' - '' •
i)Hv~i HUMMER
2 )DATE
3)?IHr BEGAN
*)TIME EHD
5 )T - l!FT TIME OF TEST , MINUTES
G)PB- BAROMETRIC PRESS VRF , 111 RG
7) PS- STACK PRESSURE, III RG
S)i/.'- GAS MTR OK IF ICE PRESS PROP, "1120
3)7// -GAS METER AVG TEMP. DEC, F
iO)VC -TOTAL 1120 COLT.FCTED, ML
\\)\'nv-voL mo VAPOR COLL.,CU FT,STP
12)177 -VOL DRX GAS SAMPLED ,CU FT ,MTR COtlD
isy.'STPfl-vor, DRY GAS SAMPLED, cu FT.STP
\*Y.l (PCT) -STACK GAS MOISTURE tPCT VOL
15)?5- AVG STACK GAS TEMPERATURE , DEC F
\G)C02-STACK GAS C02 , PCT VOL
17) 02 -STACK GAS 02 , " • '
18) CO-STACK GAS CO, •' •• . .
19) N2-STACK GAS 112 , " "
: 20) FA-STACK GAS EXCESS AIR, PCT VOL
21)110 - STACK GAS MOLECULAR VEIGRT , DRY •
22)MS - STACK GAS MOLECULAR WGHT ,STK COHD
"• • 23X75 - STACK GAS SPECIFIC GRAV,REF AIR
2u) n - AVG SOUARE ROOT VEL HEAD," mo
. 2S)AVG SOUARE ROOT(STK TEMP*VEL HEAD)
. '26)C:P - PITOT TUBE CORRFCTIOIl FACTOR , (
! 27) U - STACK GAS VELOCITY. FT /Mill
28) AS- STACK AREA, SQUARE FEET
29)ytS'- EFFECTIVE STACK AREA, S(> FEET
: 30 )flS - STK GAS FLOW RT ,CU FT/llIH,STK CUD .
3DQSTPD-STK GAS FLOW RATE ,CU FT/MIll tSTP
32)Dll - SAMPLI11G HOZZLE DIAMETER, III
33)/U/ - SAMPLING 110ZZLE AREA, SQ FT
3*)PCT ISO-ISOKItlFTIC SAMPLING. PERCE11T
35) FEED RATE, TONS/HOUR
36) PARTICULATE EMISSIONS; PROBE, CYCLONE,
AND FILTER CATCH
MILLIGRAMS
GRAINS/SCF
GRAINS/ACF
LBS/HOUR
LBS/TON OF FEED
37)' PARTICULATE EMISSIONS, TOTAL
MILLIGRAMS
GRAINS/SCF
GRAINS/ACF
LBS/HOUR
LBS/TON OF FEED
38) PARTICULATE EMISSIONS, % IKPINGER CATCH

	 1 	
12/2S/72
9:30|
12:23
132
29.9
29.9
0.500
69.4
431
20.4'3
50.3|94
50.512
28.8
150
2.00!
17.5
0.00
80.5
N.A.
29.02
25. 9J
0.893
0.44'p
10.862
0.830
1660
77.24
77.24
. 128iOOO
79,2;00
0.250
0.000341
10914
280


220.6
0.06:74
0.0417
45.7,3
0.163

239]i 6 .
0.0732
0.0453
49.67
O.l!77
7.90

""' f 	
1/9/73
10:00
12:12
138
29.9
29.9
0.710
42.4
365.5
17.32
59.950
63.310
21.5
144
3.70
15.5
0.00
80.8
N.A.
29.21
. .26.8
0.924
0.527
12.964
,0.830
' 1950
77.24
. 77.24
150,500
103,600
0.250
0.000341
104.9
215


75.6
0.0185
0.0127
16.35
0.0760

129.1
0.0315
0.0217
27.92
. 0.130
41.4

	 3 	
1/9/73
15:10
17:22
132
29.9
29.9
0.520
47.4
353
16.73
48.710
50.908
24.7
149
3.70
15.5
0.00
80.8
N.A.
29.21
26.4
0.910
0.446
11.001
. 0.830
1660
77.24
77.24
128,600
84,200
0.250
0.000341
103.8
235


45.7
0.0139
0.00907
9.99
0.0425

*
*
*
*
*
*

Average
N.A.
N.A.
N.A.
134
29.9
29.9
0.577
53.1
383
18.16
53.000
54.900
25.0
148
3.13
16.2
0.00
80.6
N.A.
29.1
26.4
0.911
0.471
11.6
0.830
1760
77.24
77.24
135,700
89,000
0.250
0.000341
106.0
243


113.9
0.0333
0.0212
24.0
0.0938

*
*
*
*
*
*
    No data because sample bottle broke during  shipment.
*** S.T.P. - DRY,  70ฐF,  29.92  in. Hg               8

-------
                             TABLE 5
           i '
           FLUORIDE, TRACE METALS, AND MERCURY CONTENT
           IN  ROCK  DRYER PROCESS REACTANTS AND PRODUCTS
                              Fluoride Content
Run 1
Run 2
Run 3
1 • FEED IN
Insol Total
1 39.1 mg/gni 39.1 mg/gm
42.9 mg/gm 42.9 mg/gm
i '
42.2 mg/gm 42.2 mg/gm
PRODUCT OUT
Insol Total
42.5 42.5
44.7 44.7
39.9 39.9
                      COOLING POND ROCK
                     Insol           Total
                   192 mg/gm      192 mg/gm
NOTE:  EMB has not received Mercury and Trace Metals results
       at this time.

-------
                        TABLE 6

     FLUORIDE CONTENT IN ROCK DRYER SCRUBBING LIQUID



                          F'Total           P00r Total
Run 1      Inlet          0.4 mg/L          <0.01  mg/ml
          Outlet         0.4 mg/L          <0.15  mg/ml
Run 2     Inlet          0.4 mg/L          <0.01 mg/ml
          Outlet         2.9 mg/L           0.72 mg/ml
Run 3     Inlet          0.4 mg/L           0.00 mg/ml
          Outlet         1.5 mg/L           0.52 mg/ml
                           10

-------
Rock Grinding
       Summarized results of the particulate  emission  tests  are  shown
in Tables 7 and 8.   Complete results  are  included  in Appendix A-2.
       EPA Method No.  5 for particulate emission testing  was used  in
all tests except Run No.  3 of the inlet tests.  The particulate  loading
was so great that the filter was placed after the  impingers  instead of
in front of them.                                                 .
       Particulate emission rates were calculated  by using the  sample
recoveredjfrom the following portions of  the  sample train:   1)  acetone
rinse of nozzle through front half of filter  holder  (Front Half);
2) in some cases, a water rinse of the front  half; 3)  filter; 4) impin-
ger contents plus a water rinse of the back half of the filter  holder
through the dry impinger that precedes the impinger with the silica gel
(Back Half); 5) ether and chloroform extraction of organic matter con-
tained in No. 4 mentioned above; 6) acetone rinse  of  the back  half after
          I
the water rinse has been made.
       A water rinse of the front half was made,  in  some cases, after
the acetone rinse and brushing was performed.  The reason for this was
to remove particulate matter that was visible after  the acetone rinsing
and brushing. This procedure was acceptable to the EPA test  officer
since it  followed the acetone rinse.
       The lab results for Run No. 3 - Inlet were  corrected  for the re-
arrangement of the sample train. Values  obtained  from lab analyses for
Runs No.  1 and 2 were used to correct the values  obtained from Run No.  3.
                               11

-------
                                             TABLE - 7
i rrsr NUMBER - 73-ROC-3
i PI.AHT tlAltr - OCCIDENTAL CHEMICAL CO. WHITE SPRINGS, FLA. '.
SOURCE TESTED - K.V.S. BAG HOUSE INLET (PARTICIPATES)
TrPE OF PLANT - PHOSPHATE ROCK GRINDING .
CONTROL EQUIPMENT- BAG COLLECTOR
POLLUTANT SAMPLED- PARTICULATES
ilJJuTi IWMRER
2 )!>ATE • •
3 )TIllF BEGAN
H)TIME END
5)T - UF.T TIKE OF TEST, MINUTES
ti)PB- BAROMETRIC PRESS VRF . Ill HG
7) PS- STACK PRESS [IRE, Ill KG
i-)LIl- GAS t!TR ORIFICE PRESS DROP, "H20
D)r/J -GAS METER AVG TEMP, DEG F
loysc -TOTAL H20 COLLECTED, ML
\\)VUV-VOL 1120 VAPOR COLL..CU FT,STP
12 )i'// -VOL DRX GAS SAMPLED ,CU FT ,MTR COtlD
isyssTpp-voi, DRY GAS SAMPLED ,cu FT,STP
l*y.JlPCT)-STACK GAS MOISTURE ,PCT VOL
15)ฃS- AVG STACK GAS TEMPERATURE , DEG F
16)C02-STACK GAS C02 , PCT VOL
17) 02 -STACK GAS 02 , ' ' "
18) CO-STACK GAS CO , • ' "
19) 112-STACK GAS [12, " "
20) FA-STACK GAS EXCESS AIR, PCT VOL
2D//0 - STACK GAS MOLECULAR HEIGHT, DRY •
22 )//S - STACK GAS MOLECULAR UGnT ,STK COHD .
23)GS - STACK GAS SPECIFIC GRAV ,REF AIR
2ซป) n - AVG Sf>UARE-ROOT VEL HEAD," t!20
• 2S)AVG SQUARE ROOT(STK TZMP*VEL HEAD) .
26)CP - PITOT TUBE CORRECTION FACTOR.
27) U - STACK GAS VELOCITY, FT/HIH
28) AS- STACK AREA, SQUARE FEET
29)45'- EFFECTIVE STACK AREA, SO. FEET
30 )PS - STK GAS FLOV RT ,CU FT/III11,STK CUD
• 3DQSTPD-STK GAS FLOW RATE ,CU FT/MIll ,STP '.
32 )DN - SAMPLII1G NOZZLE DIAMETER, Itl
33)4/7 - SAMPLING NOZZLE AREA, SQ FT
3<*)PCir ISO-ISOKINFTIC SAMPLING, PERCENT
35) FEED RATE, TONS/HOUR
36) PARTICULATE EMISSIONS; PROBE, CYCLONE,
AND FILTER CATCH
MILLIGRAMS
GRAINS/SCF
GRAINS/ACF
LBS/HOUR
LBS/TOM OF FEED
37) PARTICULATE EMISSIONS, TOTAL
MILLIGRAMS
GRAINS/SCF
GRAINS/ACF
LBS/HOUR
LBS/TOH OF FEED
'38) PARTICULATE EMISSIONS, % IMPINGER CATCH
T
1/11/73
10:05
14:06
132
30.0
29.3
1.65
.59.8
65.0
3.08
89.510
91 .860
3.30
122
0.00
21.0
0.00
79.0
N.A.
28.84
28,49
0.983
0.598
14.409
0.830
2120
7.88
7.88
16,700.,
14,400
0.375
0.000767
49.5
121


272,944
45.847
39.562
5667.34
46.84

273,057.
45.866
39.578
5669.71
46.86
0.04

	 2" 	
1/11/73
16:35
20:23
132
30.0
29.3
1.81
62.6
78.0
3.70
104.200
106.399
3.40
123
0.00
21.0
0.00
79;0
N.A.
28.84
28.48.. .;
0.992
0.589
14.217
0.830
2090
7.88
7.88
1 6,500 :. .•••
14,200
0.375
0.000767
58.3
131


244,071
35.395
30.443
4306.47
32.87

244,121
35.402
30.449
4307.35 .
32.88
0.03

3
1/12/73
10:10
13:02
132
30.0
29.3
2.30
57.7
125
5.93
114.600
118.287
4.80
124
0.00
21.0
0.00
79.0
N.A.
28.84
. 28.32 ,
0.977
0.585
14.143
0.830
2090
7.88
7.88
16,500 .
. 14,000
0.375 '
0.000767
66.1
120


402,087.8
52.450
44.347
6260.65 .
. 52.17

. 402,154
52.458
44.381
6261.68
' 52.18
0.02

*Average
N.A.
N.A.
N.A.
132
30.0
29.3
1.73
61.2
71.5
3.39
96.855
99.130
3.35
123
0.00
21.0
0.00
79.0
N.A.
28.84
28.49
0.986
0.594
14.313
0.830
2105
7.88
7.88
16,600 ;
14,300
0.375
0.000767
53.9
126


258,507
40.701
35.071
4996.72
39.94

258,589
40.714
35.082
4998.34
39.95
0.035
  * Only Run No. 1 & 2 were used for Average Values.
 ** Run No. 3 are corrected values resulting from Sample Train Rearrangement.
*** S.T.P. DRY 70ฐF, 29.92 in. Hg
                                                  12

-------
                                            TABLE - 8
TEST NUMBER - 73-ROC-3
PL APT HAW. - OCCIDENTAL
SOURCE TESTED - K.V.S. BAG
TYPE OF PLANT - PHOSPHATE
CONTROL EQUIPMENT- BAG HOUSE

CHEMICAL CO.
HOUSE OUTLET
ROCK GRINDING

V -
WHITE SPRINGS,
(PARTICULATES)



'FLA.



POLLUTANT SAMPLED- PARTICULATES
1 yiWll VUURF.R
2) DATE
3 )TIME BEGAN
U )TII1E END
5 )T - NET TIKE OF TEST, MINUTES
ซ)P2?- BAROMETRIC PRESSURE, III KG ' .
DPS- STACK PRESSURE, 111 JIG
i- )/,//- GAS 1ITR ORIFICE PRESS DROP, ' '.H20
'3)ฑV/ -CAS METER AVG TEl-lP , DEC F
IO)KC -TOTAL 1120 COLLECTED, ML
11 )vvv-voL 1120 VAPOR COLL..CU FT,STP
12)17/ -VOL PR* GAS SAMPLED ,CU FT ,MTR COND
13)\'STPn-VOL DR\' GAS SAMPLED, CU FT ,STP
it)'..' (PCT) -STACK GAS MOISTURE ,PCT VOL
1S)TS_- AVG STACK GAS TEMPERATURE, DEC, F
16) "02 -STACK GAS C02 , PCT VOL
17) 02 -STACK GAS 02 , ' ' "
18) CO-STACK GAS CO, " "
19) 112-STACK GAS //2 , ' ' "
20) FA-STACK CAS EXCESS t.IR , PCT VOL
21)IID - STACK GAS MOLECULAR HEIGHT, DRY •
22)MS - STACK GAS MOLECULAR VGt!T,STK COND
23)GS - STACK GAS SPECIFIC GRAV ,REF AIR
' 2')) // - AVG SQUARE ROOT VEL HEAD,'' I!20
25 )/U'C SQUARE ROOT(STK TEMPxVEL HEAD)
26)CP - PITOT TUBE CORRECTION FACTOR
27) U - STACK GAS VELOCITY, FT/MIN
28) AS- STACK AREA, SQUARE FEET
29)/lS'- EFFECTIVE STACK AREA, SO. FEET
3Q)QS - STK GAS FLOV RT ,C.U FT/11IN,STK CUD
3DQSTPD-STK GAS FLO!/ RATE ,CU FT/MIV^STP
32)DN - 'SAMPLING NOZZLE DIAMETER, IN
33)AN - SAMPLING NOZZLE AREA, SQ FT
3
-------
The impinger contents plus the water washings, and the organic extrac-
tions were the two categories that were corrected.  The calculations
for these corrections are shown in Appendix A-2.
          Grab samples of the stack gases at each sampling site were
obtained by an Orsat analyzer, and the concentrations of carbon dioxide,
oxygen, and carbon monoxide were determined.
          Table 9 contains the results of the laboratory analyses
performed on the grab samples from the rock grinding process reactants
and products.
          A complete set of the Appendices is available in the EPA
Emission Measurement Branch report files, listed  under Report No. 73-ROC-3.
                                14

-------
                              TABLE 9

          FLUORIDE TRACE METALS, AND MERCURY CONTENT IN
          ROCK GRINDING PROCESS REACTANTS AND PRODUCTS
         FEED IN                        PRODUCT OUT
 Insol F         Total             Insol  F         Total  F

40.6 mg/gm     40.6 mg/gm         41.0 mg/gm      41.0 mg/gm
NOTE:  EMB has not received Hg and Trace Metals results at this time.
                               15

-------
                       PROCESS DESCRIPTION

Rock Drying
          Mined phosphate rock is separated from impurities by a flota-
tion process which yields concentrated phosphate rock containing about
15% water.  During storage the moisture is further reduced to as low as
10%.  Before shipping, the rock is dried to 1.5% to 3% moisture in a
fluidized-bed drier.
          Natural gas is burned except for about 30 days per year when
fuel oil  is fired because of gas curtailment.  The fuel oil used is a
.high-sulfur blend of #6 residual and #2 distillate.
          Combustion gases along with moisture from the drier flow into
a cyclone separator which removes the bulk of the participates and returns
them to the product belt conveyor.  The gases then flow to a cyclonic
scrubber  using once-through fresh water as the scrubbing medium.
          The EPA did not furnish any process schematic diagrams of the
rock drying operation for this report.

Rock Grinding
        Dried phosphate rock  is ground into a fine powder  in a ball mill.
Air is  used to convey the ground material out of the mill.  Exhaust air
containing  the mill output flows to a classifier which separates and re-
turns  the oversize  particles  to the mill.  The classifier  outlet is
ducted  to a cyclone separator which removes  sufficiently  ground rock
from the  air stream and routes  it to  the  storage bins.  In order to close
the air-flow circuit, conveying air is  returned to the mill except for
a  small  bleed  portion.  To prevent the  conveying air from becoming sat,-

                               16

-------
urated with moisture, this bleed air is vented and replaced with ambi-


ent air.  The vented stream flows to a bag collector before exiting a


stack to the atmosphere.
          i

          The EPA did not furnish any process schematic diagrams of


the rock grinding operation for this report.
                               17

-------
                   LOCATION OF SAMPLING  POINTS

Rock Drying
          Sampling points were selected  by using  the guidelines  stated
in Method No. 1  of the Federal Register  (Vol.  36, No.  59,  August 17,
1971, Wash., D.C.).  The points selected for the  control  inlet and
outlet are shown in Table 10.   Complete  field  data sheets  are  included
in Appendix B-l.
          The work area surrounding the  control  inlet sampling site
was satisfactory, and a minimal amount of difficulty was  incurred
while sampling.
          On the other hand, the work area surrounding the control
outlet sampling site was less desirable.  The  walkway around the stack
was only 41 inches wide, and the stack diameter was 119 inches.
Since an EPA sampling train was being used (rigid connection between
probe outlet and sample box), this situation necessitated the use of
two probes of different lengths during each test.
          Figures 1 and 2 are schematic  diagrams of the sampling sites
tested at the rock drying operation.
Rock Grinding
          Sampling points were selected  by using the guidelines  stated
in Method 1 of the Federal Register (Vol. 36,  No. 59, August 17, 1971,
Wash., D.C.).  The points selected for the control inlet and outlet
are shown in Table 11.  Complete field data sheets are included  in
Appendix B-2.
                              18

-------
          The work area surrounding the inlet sampling  site  was  such
that it was physically impractical, according to  the EPA Test Officer,
to sample from more than one sampling port.
          The work area surrounding the outlet sampling site was
adequate for a EPA sampling train, therefore the  required two sampling
ports were used during each test run.
          Figures 3 and 4 are schematic diagrams  of the sampling sites
tested at the rock grinding operation.
                               19

-------
                        TABLE  10



LOCATION OF SAMPLING POINTS USED  AT  ROCK  DRYER SITES
Traverse
Point No.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
Distance From
Inside Stack Wall , in.
Inlet
5 1/4
11 1/4
"17 1/4
23 1/4
29 1/4
35





A




•







Outlet
Too Close To Wall
3 13/16
6 9/16
9 3/8
12 1/2
15 11/16
19 5/32
23 3/32
27 3/8
32 3/8
38 7/16
47 3/8
71 5/8
80 9/16
86 5/8
91 5/8
95 7/8
99 13/16
103 5/16
106 1/2
109 5/8
112 7/16
115 3/16
Too Close To Wall
                         20

-------
















V
















"7"
*s.
•>x
s
s-
s*
^


^

4 Ports
_
*~







J I t /


- *s


V

@
X . /
; (



Fa


7^7
^
S*
"x
•*x.
^^
X.


7

2'=10'





n


1 / J /
















7-7





















2:



'
4'-
1


LH


""7




J'




-7" I

i

- '
\
1
I
T-i. .) ) )






























X
/ \

























•*>-

r


y

^ซ*-



/
/
/


^











x'




V







/








7






/
/



From dryer J
and product
separation cyclom
/
/

	 	 3'-4" (Inside)










(Front View)
•Ground
(Side View)
                  FIGURE 1:   INLET TO  SCRUBBER  FOR  ROCK  DRYER
                                     21

-------
   9'-ir I.D.I*
           .— n
0-
                     3'-n"
                                          2'-9'
                                          9'-4'
                                           30'
                                           17'
/ / /  rf ff///ffffrrr/ff///ff
   FIGURE 2:  OUTLET  FROM SCRUBBER FOR  ROCK DRYER
                                                      Ground
                   22

-------
                       TABLE  11



LOCATION OF SAMPLING POINTS USED  AT  ROCK GRINDING SITES
Traverse
Point No.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
Distance
Stack
Inlet
Too Close to Wall
1 1/4
2 1/8
3
4 •
5
6 1/8
7 3/8
8 3/4
10 3/8
12 1/4
15 1/8
22 7/8
25 3/4
27 5/8
29 1/4
30 5/8
31
33
34
35
35 7/8
36 3/4
Too Close to Wall
From Inside
Wall, in.
Outlet
Too Close to Wall
1 7/8
3 1/8
4 5/8
6 1/8
8
10
12 1/2
16 1/8
26 1/8
29 3/4
32 1/4
34 3/8
36 1/8
37 5/8
39 1/8
40 3/8
Too Close to Wall






                          23

-------
                                                  •  FIGURE 3

                                    INLET TO  BAGHOUSE  FOR K.V.S.  BALL  MILL
                                           Vent from unground rock
                                           storage silo  (15"I.D.)
                                             (closed during tests)
rv>
                                          vent from ground
                                          rock storage

-------
                FIGURE 4



OUTLET FROM BAGHOUSE FOR K.V.S. BALL MILL
                                                   Roof Top
                     25

-------
                   PROCESS OPERATION DURING  TEST

Rock Drying
          The first fluoride run was conducted on December 19,  1972,
from 2:30 to 5:25 p.m.   Process operation was normal  for the duration
of the run except that fuel oil was burned due to a natural  gas
curtailment.  Conversion of some of the sulfur in the fuel oil  to
sulfuric acid in the scrubber may explain the low scrubber water
outlet pH for this run.
          Run #2 was begun at 9:35 a.m. and  completed at 12:15  p.m.
on December 20.  Process operation was normal with no difficulties
encountered.  Natural gas was burned in place of fuel oil.  Production
rates were slightly lower than for Run #1 because of the high moisture
content of the rock feed.  Run #3 was conducted from 2:30 to 5:10 p.m.
with no difficulties.
          Due to inclement weather, particulate sampling was delayed
until December 22, 1973.  The first particulate run was conducted from
11:00 a.m. to 2:00 p.m. under normal operating conditions.  When
weather conditions worsened, it was decided to reschedule the remain-
ing two runs for the week of January 8, 1973.
          The second particulate run was conducted on January 9, 1973,
from 10:00 a.m. to 1:15 p.m.  Process operation was normal except that it
was discovered 60 minutes into the test that fuel oil was being burned
instead of natural gas; and the fan seemed to be performing below par
about half-way through the test.
          Particulate run #3 was begun at 3:10 p.m. and completed at
6:00 p.m. on January 9, 1973.  Process operation was normal except
for the burning of fuel oil and the use of a wetter than normal grade
of rock.                       26

-------
Rock Grinding
          Run No.  1  was conducted  on  January  11,  1973,  from  10:00 a.m.
to 2:18 p.m.   Excessive humidity resulted  in  moisture concentrations of
5-6 percent in the air to the  baghouse.   The  plant operator  indicated
that the moisture  content is usually  maintained around  two percent.
Except for the high moisture content  of the conveying air, process con-
ditions were  normal  for the duration  of the run.
          The remaining two runs were completed under normal process con-
ditions with  no difficulties.  Run No.  2 was  begun  at 4:35 p.m.  on
January 11, 1973,  and completed  at 8:24 p.m.  Run No. 3 was  conducted
from 10:10 a.m. to 1:00 p.m. on  January 12.  During Run No.  3  the weather
was wet and cold.
                               27

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                SAMPLING AND ANALYTICAL PROCEDURES

Rock Drying
       Preliminary stack parameter data such as the number and  location
of sampling points, stack gas velocities,  stack gas molecular weights,
and stack gas moisture contents were determined by the EPA Method Nos.  1,
2, 3, and 4, respectively (Federal Register, Vol.  36,  No.  59, August 17,
1971, Washington, D.C.).
       The stack gas velocity at the control outlet posed  a problem of
obtaining an accurate velocity head measurement because of the  tangential
flow within the stack.  A standard pitot tube was  used to  traverse the
stack, and it was rotated from side to side to try and locate the direc-
tion of flow.  No appreciable difference in velocity head  could be detected
during each rotation; therefore, sampling was conducted by traversing
the S-type pitot tube and sampling nozzle in a vertical position during
all fluoride and particulate emission tests.  After the velocity and gas
flow rates were calculated from the emission tests, it was evident that
there had been some influence of tangential at the control outlet because
of discrepancies in the gas flow rate entering and leaving the  control
device.  The outlet gas flow rates were approximately 38 percent greater
than the inlet gas flow rates.
       Since there was no evidence of diffusion air being  injected into
the system following the scrubber, the difference  in the inlet  and outlet
flows was probably attributable to the tangential  flow.
                                28

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       Grab samples of the stack gases were collected in  plastic  bags,
and then analyzed for carbon dioxide, oxygen,  and carbon  monoxide con-
tent by an Orsat analyzer.  All  sampling sites were analyzed while the
dryer was burning both natural gas and fuel oil.
       On the day prior to performing the first emission  tests,  the pre-
liminary moisture test at the control inlet was made while  the dryer
was burning natural gas.   After the first emission tests  had been com-
pleted, it was learned that the dryer was operating on fuel  oil.   This
resulted in a greater moisture content than  had been estimated,  which
made the isokinetic sampling rate deviate considerably.
       Fluoride emissions were determined by a method specified  by the
EPA project test officer.  This method is currently being evaluated by
the EPA, and has been temporarily designated as a proposed  EPA Method
No. 13, "Determination of Total  Fluoride Emissions From Stationary
Sources."
       A schematic diagram of the fluoride sampling train is shown in
Figure 5.
       A sample train leak check was inadvertently excluded for  Run
No. 3 of the outlet tests.
       The analysis for the one sample taken as the water blank  con-
tained a sizeable amount of fluorides.  Based upon fluoride analyses
of the same water by Environmental Science and Engineering, Inc., the
only explanation for the high fluoride contenrt of the blank must be that
it was contaminated after it was taken from the water supply at  the
test site.
                                29

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co
o
                                      18
 1.  Stainless steel nozzle
 2.  Heated glass-lined probe with
       stainless steel sheath
 3.  Ice bath
 4.  Impinger, modified tip,  100 ml H-O
 5.  Impinger, standard tip,  100 ml H.O
 6.  Impinger, modified tip,  dry
 7.  Impinger, modified tip,  200 gms silica gel
 8.  Glass filter holder with Whatman No. 1 filter
 9.  Thermometer
10.  Flexible sample line
11.  Vacuum Gauge
12.  Main valve
13.  By-pass valve
14.  Air-tight vacuum pump
15.  Dry test meter
16;  Calibrated orifice
17.  Inclined manometer
18.  S-type pitot  tube
                                                                 L4_
                                                                 FIGURE  5
                                               PROPOSED  EPA METHOD 13 FLUORIDE SAMPLING TRAIN
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       During each fluoride emission test,  grab samples  of the  process
reactants and products, and inlet and outlet scrubbing liquid were
taken.  The pH and temperature of each scrubbing liquid  grab  sample  was
recorded at the test site.   Also, several  samples of the cooling  pond
water and rock were collected during the tests.
       Particulate emissions were determined by the EPA  Method  No. 5,
described in the Federal  Register (Vol. 36, No. 59, August 17,  1971,
Washington, D.C.).
       Figure 6 is a schematic diagram of the particulate sampling train
used.
       Inadvertently, the sample train leak check was excluded  for Run
No. 3 - Inlet, and Run No.  2 - Outlet.  The sample train vacuum gauge
reading for these two tests were about the  same as the other  tests for
which leak checks were made.
       A water rinse of the particulate train "front half" was  made
after the acetone rinse,  because the EPA project test officer deemed it
necessary to remove the water soluble particulate material from the
nozzle, probe, and cyclone.  This was performed for each run  with the
exception of Run No. 2 - Inlet and Run No.  3 - Outlet.  Only  acetone was
used on the front half following these two runs.
       All samples collected were analyzed by the EPA.  Laboratory
results for fluorides, particulates, and ?2ฎ5 are included in Appendix
D-l.  Results of the trace metals and mercury data can be found in  the
EPA's Emission Measurement Branch report file No. 73-ROC-3.
       Complete sampling procedures are included in Appendix  C-l.
                                31

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CO
ro
                                   20
 1.   Nozzle
 2.   Probo   (heated, glass-lined)
 3.   Cyclone and flask    (inlet only)
 4.   Filter
 5.   iicatcd compartment
 G.   Ice bath
 7.   Impinger with 100 ml distilled water
 8.   Inipingcr with 100 ml distilled water
 9.   Impingcr, dry
10.   Impingcr with silica gel
11.   Thermometer
12.   Flexible sample line
13.   Vacuum gauge
14.   Main control valve
15.   Air tight vacuum pump
10.   By-pass control valve
17.   Dry test meter
18.   Calibrated orifice
19.   Inclined manometer
20.   "S" type pitot tube
                                                            . EPA PARTICULATE SAMPLING TRAIN

                                                                        FIGURE  6

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Rock Grinding
       Preliminary stack .parameter data such  as  the  number  and  location
of sampling points, stack gas velocities,  stack  gas  molecular weights,
and stack gas moisture contents were determined  by the  EPA  Method  Nos. 1,
2, 3, and 4, respectively (Federal  Register,  Vol.  36, No. 59, August  17,
1971, Washington, D.C.).
       Grab samples of the stack gases were collected in  plastic bags
and then analyzed for carbon dioxide, oxygen, and  carbon  monoxide  content
by an Orsat analyzer.  All sampling sites  were analyzed prior to any
emission tests.
       Particulate emissions were determined by  the  EPA Method  No.  5,
described in the Federal Register (Vol. 36, No.  59,  August  17,  1971,
Washington, D.C.).
       Figure 6 is a schematic diagram of the sampling  train used  for
all tests except Run No. 3 at the inlet sampling site.
       Because of the high particulate load at the inlet  sampling  site,
the nozzle and probe were continually plugging up.  As  a  result, the
sample train had to be shut down many times during the  first two test
runs.  At the beginning of Run No. 1, the plugging of the nozzle was  so
severe that the EPA test officer suggested that  we switch to a  3/8-inch
nozzle to try and eliminate the problem.  As a result of  this switch,
the isokinetic sampling rate could not be maintained.
       Since simultaneous sampling was being conducted  at the inlet and
outlet, each time the inlet train shut down* the outlet train was  also
                                33

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shut down.  As a result of much confusion during the first test run,  the
outlet train was inadvertently excluded from the leak check for Run No. 2.
The sample train vacuum readings for the Run No. 2 - Outlet tests  were
about the same as the previous tests, which indicates no gross  leakage.
       Also as a result of the confusion created by the frequent stopping
and starting of the sample train for Run No. 1  - Outlet, the isokinetic
sampling rate was not maintained.
       The sample recovery procedure for Run No. 1 - Inlet was  altered
somewhat from the EPA Method No. 5.  The front half was rinsed  with water,
following the acetone rinse.  The water removed some of the water soluble
particulate matter.
       The configuration of the sampling train was changed for  Run No.  3-
Inlet at the request of the EPA test officer.   This change resulted in
the filter holder being placed just ahead of the last impinger, which
contained silica gel.  The plugging up of the filter from the excessive
particulate emissions was essentially eliminated.
       Since the configuration of the sampling train used for Run No. 3-
Inlet was changed from the normal  EPA Method No. 5 train, the laboratory
data had to be corrected for the change.  Basically, the laboratory
data from the first two'tests were used to determine corrected  values
for the third test.  The complete procedure used for calculating the
corrected values is included in Appendix A-2.
       Grab samples of the rock entering the grinder, and the final  rock
product leaving the grinder were taken periodically during each test.
                                34

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       All  samples collected were analyzed by tie EPA.   Laboratory
results for fluorides  and particulates are included in Appendix D-2.
Results of the trace metals and mercury data calh be found in the EPA's
Emission Measurement .Branch report file No. 73-ROC-3.
       Complete sampling procedures are included in Appendix C-2.
                                35

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