TEST NUMBER 73-ROC-2

INTERNATIONAL MINERALS AND
     CHEMICAL CORP.
    NORALYN,  FLORIDA
        PEDCo ENVIRONMENTAL

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          TEST NUMBER 73-ROC-2

       INTERNATIONAL MINERALS AND
             CHEMICAL CORP.

            NORALYN, FLORIDA
             Prepared by
        Normal Kulujian, P.E.
       Richard W. Gerstle, P.E,
       Contract No. 68-02-0237
             Task No. 19
PEDCo-Environmental Specialists, Inc.
           Cincinnati, Ohio
              June 1973

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                 I..  TABLE OF CONTENTS

                                                  Page

  II.  INTRODUCTION                                 1

 III.  SUMMARY OF RESULTS                           3

  IV.  PROCESS DESCRIPTION                          7

   V.  PROCESS OPERATION                           10

  VI.  LOCATION OF SAMPLING POINTS                 11

 VII.  SAMPLING AND ANALYTICAL PROCEDURES          14

       Set Up Procedure                            14
       Preliminary Traverse and Moisture           14
       Gas Velocity and Temperature                15
       Molecular Weight and Gas Analysis           15
       Particulate Sampling                        15
       Sample Storage                              17

VIII.  APPENDIX

       A.  COMPLETE PARTICULATE RESULTS WITH EXAMPLE
           CALCULATIONS

       B.  PROCESS .OPERATIONAL LOG

       C.  FIELD DATA

       D.  SAMPLING PROCEDURES

       E.  LABORATORY REPORT

       F.  SAMPLE NUMBER LOG

       G.  TEST LOG

       H.  SAMPLE HANDLING LOG

       I.  PROJECT PARTICIPANTS AND TITLES

       J.  PRESURVEY REPORT
                           11

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II, INTRODUCTION



     Under the Clean Air Act of 1970, as amended, the Environ-



mental Protection Agency is charged with the establishment



of performance standards for stationary sources which may



contribute significantly to air pollution.  A performance



standard is based on the best emission reduction systems



which have been shown to be technically and economically



feasible.                              .  '





     In order to set realistic performance standards, accurate



data on pollutant emissions must be gathered from the stationary



source category under consideration.





     Atmospheric emissions of particulate and fluorides from



the International Minerals and Chemical Corporation (IMC)  rock



grinding operation in Noralyn, Florida were sampled to establish



a guide for New Source Performance Standards as authorized by



the Clean Air Act of 1970.  Triplicate tests were made to



determine particulate concentrations at the inlet and outlet of



the rock grinder..  The three tests Were made February, 1973.






     Stored rock is transferred to a mill by a conveyor belt.



Different ducts are used for the ground product and exhaust gases

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from the mill.  The exhaust gases are cleaned in a baghouse.



The cleaned exhaust is pulled up through the stack by an induced



draft fan.  The material caught in the baghouse is recycled



back to the milling operation.

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III.  SUMMARY OF RESULTS



     Table 3.1 presents the overall test summary of the three




particulate tests in U.S. and metric units.  Results from the



three tests were averaged to obtain values in Table 3.1.



Results from each individual test are summarized in Table 3.2.






     The rock grinding operation is enclosed in a building, so



both inlet and outlet sampling sites were under cover.  A clean



up area was not available, so the samples from the test trains



were transferred to containers in a mobile van.






     The reagent in the Orsat apparatus produced questionable



exhaust gas analyses, so values of ambient air were assumed for



calculations.  Since the air entering the milling operation



experiences no change (i.e. combustion), the assumption of



atmospheric properties is valid.






     The inlet site consistently had a higher flow rate than



the outlet site; values for the three tests ranged between 16 and



18 percent greater.  A leak through the ducting, control device,



or dampers may have accounted for the loss.






     The high isokinetic value for the Run No. 8 inlet test



resulted because the improper nozzle size was used.  A comparison



of the inlet and outlet catch reveals that while the maximum

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dust from the three tests was caught at the outlet site



(Table 3.2), the inlet sample was the smallest of the three



catches.  Therefore the data from the second test (Run No. 8)



was not averaged in Table 3.1 values.






     A minor process upset also occurred during Run No. 8,




when a large wooden object jammed the mill.  The wood was



removed and the mill was back in operation within ten minutes.






     The various types of feed are discussed in Section  V.



Raw materials and product samples were taken during the tests.



It was impossible to get a baghouse catch sample because there



was no access opening.

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                         Table 3.1  OVERALL SUMMARY OF RESULTS FROM PHOSPHATE ROCK GRINDER
Pollutant
Measurement
System
Volume of Gas Sampled
Percent Moisture by Volume
Average Stack Temperature
Dry Stack Volumetric Flow Rate
Actual Stack Volumetric Flow Rate
Percent Isokinetic
Feed Rate
., Partial Catcha
Weight
Concentration/Dry Volume
Concentration/Actual Volume
Concentration/Time
Lb/ton, Feed Concentration/
Input Feed Rate
Total Catch
Weight
Concentration/Dry Volume
Concentration/Actual Volume
Concentration/Time
Lb/ton, Feed Concentration/
Input Feed Rate
Percent Impinger Catch
Units
U. S.
DSCF
%
oF
DSCFM0"
ACFMd
%
Ton/hr
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton

mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton
%
Metric
DNm3e
%
°C
DNm /sec
M3/secq
%
Mton/hr
mg
mg/DNm3
mg/m3
kg/hr
kg/Mton

mg
mg/DNm3
mg/m^
kg/hr
kg/Mton
%
Particulate
. U. S.
' Inlet"
61.564
5.98
202
2996
3931
104.2
34.5
12915
3.246
2.473
83.03
2.399

12949
3.255
2.480
83.25
2.405
0.25
Outlet
114.743
5.97
161
2708
3312
98.4
35.0
48.0
0.00647
0.00529
0.150
0.0042

100.6
0.01358
0.01110
0.314
0.0089
50.6
u Metric
Inlet"
1.7433
5.98
94.2
1.414
1.855
104 . 2
31.3
12915
7427
5658
37.66
1.199

12949
7446
5673
37.76
1.203
0.25
Outlet
3.2492
5.97
71.5
1.278
1.563
98.4
31.7
48.0
14.8 '
12.1
0.0679
0.0021

100.6
31.08
25.40
0.142
0.0044
50.6
a) Partial catch includes probe, cyclone and filter.
b) Dry standard cubic feet at 70°F, 29.92 in. Hg.
c) Dry standard cubic feet per minute at 70°F, 29.92 in. Hg.
d) Actual cubic feet per minute.
e) Dry normal cubic meters at 21.1°C, 760 mm Hg.
f) Dry normal cubic meters per second at 21.1°C,
    760 mm Hg.
g) Actual cubic meters per second.
h) Second inlet test  (Run No. 8) not included in
    averages.

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                            Table 3.2  PARTICULATE EMISSION DATA SUMMARY

                        IMC Corp., Noralyn, Florida - Rock Grinder Operation

Run
Date
Volume of Gas Sampled-DSCFa
Percent Moisture by Volume
Average Stack Tempera ture-°F
Stack Volumetric Flow Rate-
DSCFMb
Stack Volumetric Flow Rate-
ACFMC
Percent Isokinetic
Feed Rate-ton/hr
Particulates-probe, cyclone,
 and filter catch
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
Particulates , total catch
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
Percent impinger catch
Inlet
7
2-16-73
60.401
6.07
203
2916

3835

105.0
36.0


14513
3.708
2.820
92.686
2.574

14556
3.719
2.828
92.961
2.582
0.3
8
2-16-73
59.022
5.91
205
2903

3822

213.8
36.0


10303
2.694
2.048
67.027
1.861

10332
2.702
2.052
67.216
1.867
0.3
9
2-16-73
62.728
5.89
200
3075

4026

103.4
33.0


11316
. 2.784
2.126
73.373
2.223

11342
2.790
2.131
73.542
2.228
0.2
Outlet
7
2-16-73
114.965
5.32
161
2720

3295

98.2
36.0


63.3
0.00849
0.00698
0.198
0,0055

111.0
0.01490
0.01224
0.347
0.0096
43.0
8
2-16-73
112.393
6.05
161
2654

3256

98.3
36.0


47.8
0.00656
0.00535
0.149
0.0041

130.0
0.01784
0.01455
0.406
0.0113
63.2
9
2-16-73
. 116.870
6.53
160
2751

3386

98.7
33.0


33.0
0.00435
0.00354
0.102
0.0031

60.7
0.00801
0.00651
0.188
0.0057
45.6
a)  Dry standard cubic feet at 70°F, 29.92 in. Hg.
b)  Dry standard cubic feet per minute at 70°F, 29.92 in. Hg.
c)  Actual cubic feet per minute.

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IV.  PROCESS DESCRIPTION



     A phosphate rock plant flow diagram, shown in Figure 4.1,



illustrates the steps of the process in relation to the grinding



operation.  After the phosphate rock is mined and dried, it is



ready to be ground.






     The Noralyn, Florida IMC plant uses the swept air principle



of grinding the phosphate rock.  A picture of the grinding



operation is shown in Figure 4.2.  Each of three mills can



process approximately 35 tons of rock per hour.  The velocity



of the air through the Raymond Mills governs the particle size



of the ground rock.  The ground product is fed to a rail car



where it is shipped to fertilizer or elemental phosphorus



plants.  Exhaust gases pass through a baghouse and an induced



draft fan before being emitted to the atmosphere.  The baghouse



collection hopper is ducted back to mills, recycling the caught



particles.






     Two different milling configurations were present at the



Noralyn plant.  These are discussed extensively in Appendix C.

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cc
       HIGH PRESSURE
               WATER
         DRAGLIf!E
RECOVERY PLANT
          OVERBURDEN  .:-
            •; BEDROCK  :.-.>XN'-'* <\V-^ '
                                        I    I
                      DRY ROCK STORAGE
                                                   J
                                                     DRY
                                                     ROCK
                                                     SHIPPING
                          GROUND  ROCK
                          SHIPPING
                                                                                WET  ROCK  STORAGE
                                                                                  AND  RECOVERY
                               'igure 4.1  Phosphf.te rock flow sheet.

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  PRODUCT
      RAYMOND
       MILL
                                   CONTROL
                                   DAMPER
                                               BAGHOUSE
    C)    CONVEYOR
                                    STACK HAD COVER
                                    NO VISIBLE EMISSIONS
                                    G. RILEY SAW SOME  BEFORE  TEST STARTED

                                      ROOF
Fiaure 4.2   Diagram of phosphate  rock  grinder  at  IMC  plant,  Noralyn,  Florida

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V.  PROCESS OPERATION*




     During the testing, process operations of the Noralyn



rock grinding mill No. 4 were monitored by Mr. J. Peoples of



EPA.  Mr. Peoples collected process data and communicated



to the testing crew any upsets or abnormalities during the



testing periods.






     Feed and grinding rates are based on estimates obtained



from IMC plant personnel and observed loading rates of railroad



cars (Appendix C contains detailed comments recorded during



the testing periods).






     Particulate tests were conducted on February 16, 1973 at



the No. 4 rock grinder unit.  The sampling began at 11:25 A.M.



The material processed during the first and second run was a



65-200 grind (65% through a 200 mesh screen).  A 90-100 grind



was produced during the third run.  The testing was completed



at 7:45 P.M.  Raw materials and product samples were obtained



during all of these tests.  No process upsets occurred during



Runs 1 and 3.  However during Run 2 testing had to be delayed



twice due to operational difficulties.  The opacity of the



grinder stack was less than 10% opacity during the testing



periods.
*Written and supplied by EPA.
                          10

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VI.  LOCATION OF SAMPLING POINTS




     A section 24 inches upstream from the entrance to the



baghouse was the best inlet sampling site.  The 11.75 inch



diameter duct had a 45 degree bend approximately 42 inches up-



stream of the sampling site.  A diagram of the rock grinding



inlet and sampling points is shown in Figure 6.1.






     Since the inlet sampling location was only about 3.6



diameters downstream of the duct bend, 28 traverse points were



chosen.  The project officer approved the number of sampling



points and a test duration of 84 minutes  (3 minutes per point).






     Two sample ports were installed on the west side and



bottom of the horizontal duct.  The sample  box was placed



on a variable set of jacks when sampling the vertical traverse



points.





      Two  possible  outlet  sampling  sites were  considered,



 one  inside  the building and one  on the  roof.   The  inside



 site was  chosen  so both inlet and  outlet  sampling  team



 could coordinate the  tests.   The chosen sampling site was



 less than one foot from the roof and  approximately four feet



 below the top of the  stack  as shown in  Figure  6.2.   Sampling



 ports were  cut from the narrow side of  the  12  in.  x  14 in.



 rectangular stack.  Six sample points were  chosen  on four



 traverse  locations; the 24  points  were  sampled  for five



 minutes each, or 120  minutes  per test.  The draft  fan was the



 nearest upstream obstruction,  64 inches from  the sampling site,





                          11

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               11 .75" ID
                 ii

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                      ALL  DIMENSIONS
                      IN FEET ARE .
                      APPROXIMATE
WALKWAY —
   LOOKING NORTH
                   LOOKING WEST
   -0.10"
       SECTION AA
POINT
1
2
3
4
5
6
7
8
9
10
11
12
13
14
TRAVERSE
DISTANCE,
INCHES
1 .0
1 .0
1 .0
1 .7
2.4
3.2
4.3
7.5
8.6
9.4
10.0
10.7
10.7
10.7
Figure  6.1   Diagram of rock grinder  inlet  and  sampling points
                            12

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IMPLING
'CTION- r"1
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12.25 !
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11°
8.75 ' j!
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SECTION AA
PLATFORM
/-AND BUILDUP
/ FOR SAMPLE BOX



TRAVERSE
DISTANCE,
POINT INCHES
1 1.0
2 3.0
3 5.0
4 7.0
5 9.0
6 11.0
\

                  EXISTING STRUCTURE
ALL DIMENSIONS
IN  FEET ARE
APPROXIMATE
Figure 6.2  Diagram of rock  grinder  outlet  and  sampling  points.
                             13

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VI.  SAMPLING AND ANALYTICAL PROCEDURES




     All particulate sampling procedures were similar to



Method 5 as defined in the Federal Register.  The contractor



performed all testing and sample recovery operations; collected



samples were analyzed by EPA personnel.  The inlet and outlet



sampling crew consisted of two man teams which included a



probe and meter technician.






Set Up Procedure



     The inlet and outlet trains were set up in a routine



fashion.  In both cases the sample box and meter box were



within 15 feet of each other.






Preliminary Traverse and Moisture



     A preliminary velocity traverse at the inlet and outlet



location determined approximate nozzle sizes and isokinetic



sampling conditions.  A 0.180-inch I.D. nozzle was used for



inlet testing while the outlet was sampled with a 0.277 inch



I.D. nozzle.  The wrong nozzle (0.125 I.D.) was inadvertently



placed on the probe for the second inlet test (Run 8).   This



resulted in a high isokinetic sampling rate.






     The inlet stack gas moisture was determined by a train



similar to Figure 4.2, Federal Register/ Volume 36, No. 247,



page 24887.  A wet and dry bulb thermometer was used to calculate



outlet flue gas moisture.
                           14

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Gas Velocity and Temperature




     Velocities were measured at each sampling point across



the stack diameter to determine an average value according to



procedures described in the Federal Register.  Gas flow




temperatures were measured by long stem dial thermometers.






Molecular Weight and Gas Analysis



     The flue gas was assumed to have a composition and molecular



weight similar to atmospheric air.  The values were used to



determine isokinetic sampling rates.






Particulate Sampling



     Particulate matter was isokinetically sampled from the



drying operation with a train shown in Figure 7.1.  The train



consisted of a stainless steel nozzle, a heated glass probe,




a heated glass fiber filter, and four impingers connected in



series with glass ball joint fittings.  The first two impingers



contained 100 ml of water each, the third impinger was left



empty and approximately 200 grams of preweighed silica gel were



placed in the fourth impinger.






     In all cases sampling was conducted under isokinetic




conditions by continually monitoring the velocity with a pitot



tube and adjusting the sampling rate accordingly.
                           15

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                                           FILIER HOLDER
                 STACK V/ALl
                                                                           THERMC.V.E fER
REVERSE-TYPE
PHOT IU3E
                                         DRY TEST METER      VACUUM PUMP
                      Figure  7.1.   Particulate  sampling train.

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     Inlet concentrations were so heavy that several filter



changes were needed during each test to pull the proper amount




of air through the train.  During the last inlet test (Run 9),



an impinger connector was broken while transferring the train




between sampling ports.  Contents from the broken inipinger were




included in the acetone wash.





     The train cleanup procedure  consisted  of measuring  the



water collected and weighing  the  silica gel to  determine




moisture content.  The water  was  then  poured into  a glass



jar.  The filter was removed  and  placed in  a marked container.



The probe and front half  of  the  filter holder were then  rinsed



with analytical reagent grade acetone  and the washings placed in



a glass container.  The rear  half of  the  train  consisting of



filter holder, impingers, and connectors was rinsed with



distilled water and this  water added  to the impinger contents.



The rear half of the train was then rinsed  with  acetone  and



placed in a third sample  jar.  A portion of the  acetone  and



distilled water used in the sample recovery were set aside and



used as blanks for analysis.





Sample Storage



     All samples were placed in 1000 ml glass and polyethylene



containers and marked with EPA identification tags  (see Appendix



F).  The bottles were then put in wooden boxes  with styrofoam



separators and hand delivered to EPA, North Carolina, after all



tests were completed.






                           17

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