73-FRT-7
                               (REPORT NUMBER)
AIR  POLLUTION  EMISSION  TEST
                         U.S.S. AGRI-CHEMICALS
                             (PLANT NAME;
                         NASHVILLE,  TENNESSEE
                           (PLANT ADDRESS)
           U. S. ENVIRONMENTAL PROTECTION AGENCY
                 Office of Air and Water Programs
             Office of Air Quality Planning and Standards
             Emission Standards and Engineering Division
                  Emission Measurement Branch
               Research Triangle Park, N. C.  27711

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  EPA REPORT NUMBER 73-FRT-7

     U.S.S.  Agri-Chemicals

     NASHVILLE, TENNESSEE
         Submitted to
Environmental Protection Agency
    Office of Air Programs
    Contract No. 68-02-0225

          Task No. 15


         Submitted by
   Engineering-Science, Inc.
      7903 Westpark Drive
    McLean, Virginia  22101
        November  1974

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I  TABLE OF CONTENTS









Section                   Title                                          Page




   II            INTRODUCTION                                              1




  III            SUMMARY AND DISCUSSION OF RESULTS                         2




   IV            PROCESS OPERATION                                        12




    V            LOCATION OF SAMPLING PORTS                               15




   VI            SAMPLING AND ANALYTICAL PROCEDURES                       22

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                               LIST OF TABLES
Table                               Title                                 Page
III-l         Corresponding Changes of Ammonia Concentrations in
              Exhaust Gas and Scrubber Liquor                               7
III-2         Kiln Dryer/Cooler Baghouse Emission Summary                   8
III-3         Ammoniator Scrubber Emission Summary                          9
III-4         Kiln Dryer/Cooler Baghouse Flow Data                         10
III-5         Ammoniator Scrubber Flow Data                                11
                               LIST OF FIGURES
Number                              Title                                 Page
IV-1          Schematic Diagram of Process, U.S.S. Agrichemicals,
              Nashville, Tennessee                                         14
V-l           Kiln Inlet to Baghouse                                       16
V-2           Kiln Baghouse Stack                                          17
V-3           Location of Sampling Ports:  Ammoniator Scrubber Inlet
              and Outlet                                                   20
V-4           Traverse Point Locations                                     21

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II   INTRODUCTION







     Source emission tests were conducted at the U.S.S. Agri-Chemical phosphate




fertilizer plant, Nashville, Tennessee, during the week of May 21, 1973.  The




purpose of the tests was to gather data upon which the U. S. Environmental Pro-




tection Agency can establish emission standards for new sources in the phosphate




fertilizer industry under Section 111 of the Clean Air Act of 1970.




     This report describes the methods used and results obtained in the test




series.  In total,twelve (12) samples were obtained for each of the following




emissions; particulates, ammonia and total fluorides.  Samples were obtained from




two process operations, the dryer kiln/cooler baghouse and the ammoniator




scrubber.  Simultaneous sampling of both the inlet and outlet gas streams of




each control device was conducted.  Thus three samples were collected for




each of the pollutants at each of the following locations:  kiln baghouse




inlet, kiln baghouse exit, ammoniator scrubber inlet and ammoniator scrubber




exit.  The sampling locations are shown in Figure IV-1. In addition to these




gas stream samples, grab samples of scrubber liquid, phosphate rock and granu-




lated fertilizer product were periodically taken for analysis by EPA.  Analyses




of the fluoride and ammonia samples were done by EPA chemists.  An analysis  of




the particulate samples was done by ES.




     Section III of this report contains a discussion and summary of the




results of the tests.  Subsequent sections describe the location of the sampling




ports and the sampling and analytical procedures.  The Appendices contain all




the raw data collected on-site as well as the complete analysis of this data.




     Mr. Robert M. Martin and Mr. J.E. McCarley, of the Office of Air Quality




Planning and Standards, Environmental Protection Agency, coordinated the tests




and arranged for the test facilities.




                                      1

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 Ill  SUMMARY AND DISCUSSION OF RESULTS




     The data obtained during the test was reduced to computer format for




analysis.  The concentrations of particulate, fluoride, and ammonia in the




exhaust gases along with their respective emission rates were calculated.




Complete particulate results, along with a sample calculation, appear in




Appendix A, and complete results for fluoride and ammonia appear in Appendix




B.  All results are expressed both in English and metric units.  In accordance




with EPA's letter of June 20, 1973, included in Appendix J, emission rates are




reported in Ib/hr and Ib/ton feed.  Summaries of the data appear in Table III-l




through III-5, and are discussed in more detail later in this section.




     When the fertilizer plant changes production to a different type of




fertilizer, input feed rates must also change.  While ES was testing, two




types of fertilizers were produced:  10-10-10 and 6-12-12, the numbers




standing for proportionate amounts of constituents.  Feed rates for each type




of product, as reported by EPA in their letter of December 10, 1973, are




as follows:



                                 NH- Feed Rates




                             10-10-10      1.20 tons/hr




                              6-12-12      2.45 tons/hr








                                 P-0  Feed Rates
                             10-10-10      0.465 tons/hr




                              6-12-12      2.90 tons/hr




                                 TOTAL FEED RATE




                                   25 tons/hr

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Fertilizer 10-10-10 was produced from tests number 1 through 6 and 6-12-12




was produced during the remainder of the tests.




     As described in Section V, the scrubber inlet (horizontal stack, see




Figure V-3) had three inches of water flowing in the lower quarter.  For




flow rate calculations, an effective cross-sectional area was derived by sub-




tracting the area occupied by the water.  An effective stack diameter was




then calculated from this derived area.  The real diameter, 18 inches, was




reduced to 15.4 inches.




     When reviewing the values for flow rate at the kiln and ammoniator,




discrepancies on the order of 25-35% between inlet and outlet were noticed.




EPA methods and standards were stringently adhered to and all calculations were




carried out properly.  No evidence is available to formulate an explanation




for these discrepancies at the kiln.  However, at the scrubber, system leakage




could have allowed dilution air to enter the gas stream.




     When reviewing isokinetic values, a few are noted that are greater than




10% from isokinetic.  For most cases where the isokinetic value was greater




than 110%, the average orifice pressure drop is approximately 0.40 in. H_0.




At this rate, the meter AH0 is about 1.7 instead of the value of 1.85 which




was used to set up the nomograph.






A.  Particulate Analysis



     Test No. 11-1, at the scrubber inlet, must be disregarded because a




quantity of mud and water, which was later found to be flowing in the stack,




had been inadvertently sampled.  Test No. 11-0, at the scrubber stack must




be disregarded due to upset conditions at the scrubber which occurred suddenly




during the test allowing a large amount of particulate matter to be caught




by the sample train before the train could be shut down.

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     The particulate emissions do not appear to be influenced by the type of




fertilizer being produced.  Controlled filterable particulate emissions at the




baghouse stack range from  .65 to 1.38 Ibs/hr.  Controlled total emissions range




from 3 to 14 Ibs/hr.  Controlled emissions as a function of feed rate range




from 0.13 to 0.56 Ibs/ton  feed.  Comparing inlet and outlet emission data at




the baghouse it is noted that filterable particulates are reduced greater than




99.9% in the baghouse; total particulates are reduced 99.7%.  At the inlet




to the baghouse only 0.43% of the total particulate catch is found in the




impingers.  At the outlet  86% of the total catch passes through the filter




and is caught by the impingers.




     At the scrubber stack controlled filterable particulate emissions range




from 2.73 to 3.24 Ibs./hr.  Controlled total emissions range from 4.25 to 7.73




Ibs/hr.  Controlled emissions from the baghouse as a function of feed rate




range from 0.17 to 0.31 Ibs/ton feed.  The scrubber is 97% efficient in re-




moving filterable particulates and 95% efficient in removing the total particu-




late load.  At the scrubber inlet only 2% of the particulate catch is found in




the impingers, but at the outlet 47% of the catch passes through the filters




and is caught by the impingers.




B.  Fluoride Analysis




     Test No. 4-1 at the kiln baghouse inlet was voided because the sample




was spilled during analysis.



     Controlled emission rates at the baghouse stack show a relationship to the




type of fertilizer being produced.  Production of 10-10-10 fertilizer with a




P90_ feed rate of 0.465 ton/hr yields a controlled fluoride emission rate of




about 2.7 Ib/hr, while 6-12-12 production, with a larger P^ feed rate of




2.90 tons/hr yields smaller controlled fluoride emissions of 0.57 to 0.78




Ibs/hr.   Controlled emission'rates as a function of feed show this same rela-




tionship with 5.8 Ibs/ton P205 feed being emitted during 10-10-10 production





                                    4

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and 0.20 to 0.27 Ibs/ton ?205 feed being emitted during 6-12-12 production.




     Controlled fluoride emission rates from the scrubber stack during 6-12-12




production range from 0.02 to 0.25 Ibs/hr, or 0.006 to 0.087 Ibs/ton P20_ feed.




No tests were conducted at the scrubber stack during 10-10-10 production,




therefore, no comparison can be made.




     Checking inlet and outlet data, it is observed that the baghouse is




96% efficient in removing fluoride; at the scrubber, 46% of the fluoride




load is removed.




C.   Ammonia Analysis




     Ammonia samples were drawn non-isokinetically and no attempt was made to




measure stack velocity or flow rate.  To calculate ammonia concentrations and




emission rates, the flow rates calculated from parallel tests were used.  If




no parallel tests were made at the same time, then figures from tests conducted




on the same day were used.  If no tests were conducted on the same day at that




particular test location, then an average value for flow rate was used.




     During 6-12-12 production, controlled ammonia emission rates are higher




than during 10-10-10 production.  At the baghouse stack, controlled ammonia




emissions are about 2.1 Ib/hr or 1.8 Ib/ton NH_ feed with an NH^ feed rate




of 1.20 tons/hr during 10-10-10 production, and 10 to 19 Ibs/hr or 4 to 8




Ibs/ton NH- feed with a higher feed rate of 2.45 tons/hr during 6-12-12




production.  At the scrubber stack, controlled ammonia emissions during




10-10-10 production are 116 to 142 Ibs/hr or 97 to 118 Ibs/ton NH3 feed,




while during 6-12-12 production, controlled emissions are about 177 Ibs/hr




or 72 Ibs/ton NH3 feed.



     Comparing the inlet and outlet data, it is noted that the baghouse reduces




ammonia emission by 88%.  Negative efficiencies were noted at the scrubber.

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Engineering-Science, Inc. had followed the EPA test methodology for sampling




ammonia in exhaust gas streams.  The results presented in this study indicate




that more gaseous ammonia was liberated from the ammoniator scrubber than was




measured in the inlet gas stream.  In other words, by our calculations the




ammoniator scrubber seemed to add ammonia to the gas stream instead of re-




ducing or minimizing these emissions.  ES has reviewed the data thoroughly and



are convinced that errors in transcribing, calculations, laboratory reporting,




and final writing did not result in the negative efficiencies projected.



     The most probable cause for the results obtained for ammonia emissions




is  the scrubber operation since gaseous ammonia can be absorbed in water or




some acidic solution.  Changes in the inlet concentration may change the




equilibrium of the  scrubber solution and  thus may cause ammonia to be liber-




ated.  The net effect of this situation — the liberation of ammonia from




the scrubber water  under certain conditions — could have occurred during




the three tests for ammonia made on the ammoniator scrubber.  As shown in




Table III-l, the change in ammonia concentration in the exhaust gas corres-




ponded to the change in ammonia concentration of the scrubber liquor.  When




the concentration of ammonia in the exhaust gas decreased from inlet to




outlet, the ammonia concentration in the  scrubber liquor increased.  When




the concentration in the exhaust gas increased, the concentration in the




scrubber liquor decreased.  The scrubber  was probably operating at near




NH_ saturation level.  It must be noted that the scrubber was primarily




designed to remove particulates, not ammonia.

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                  TABLE  III-l
CORRESPONDING CHANGES OF AMMONIA CONCENTRATIONS
      IN EXHAUST GAS AND SCRUBBER LIQUOR
Test No.
2
6
9
Liquor HN3 Gas NH3
Concentration Concentration
(mg/1) (gr/scfd)
In Out In Out
48.7 49.4 2.14 1.99
39.9 52.1 3.22 2.57
116.8 108.7 1.71 3.22

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                                                                       TABLE III-2

                                                      KILN DRYER/COOLER BAGHOUSE EMISSION SUMMARY
Run No.
1
5
AVGa
7
4
8
10
AVGa
3
12
13
AVG
Pollutant
PT
PT
PT
PT
FL
FL
FL
FL
NH3
NH3
KH3

Product
10-10-10
10-10-10
10-10-10
6-12-12
10-10-10
6-12-12
6-12-12
6-12-12
10-1 • 10
6-12-12
6-12-12
6-12-12
FRONT HALF
In
gr/scfd
19.85
9.59
14.72
11.76








Out
gr/scfd
.008
.005
.007
.004








In
Ib/hr
4532
2096
3314
2817








Out
Ib/hr
1.376
.814
1.095
.649








In
Ib/ton
181.3
83.8
132.6
112.7








Out
Ib/ton
.055
.033
.044
.026








Eff
99.9
99.9
99.9
99.9








TOTAL
In
gr/scfd
19.91
9.65
14.78
11.79
*
.122
.045
.084
.052
.426
.697
.562
Out
gr/scfd
.079
.021
.050
.050
.015
.004
.003
.004
. .011
.112
.060
.086
In
Ib/hr
4547
2109
3328
2825
*
27.7
10.3
19.0
12.17
101.3
164.2
132.8
Out
Ib/hr
13.95
3.36
8.66
8.92
2.71
.778
.572
.675
2.11
18.86
10.45
14.66
In
Ib/ton
181.9
84.4
133.2
113.0
*
9.54
3.57
6.56
10.14
41.36
67.02
54.19
Oat
Ib/tor.
.558
.134
.346
.357
5.83
.268
.197
.233
1.76
7.70
4.27
5.99
Eff
99.7
99.8
99.8
99.7
*
97.2
94.4
95.8
82.7
81.4
93.6
87.5
do
         *Sadple spilled during analysis.
              -  Average for specified product.

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                                                              TABLE III-3
                                                 AMMONIATOR SCRUBBER EMISSION SUMMARY
Run No.
11
14
15
AVG
16
17
18
AVG
2
6
AVG
9
Pollutant
PT
PT
PT
PT
FL
FL
FL
FL
NH3
NH3
NH3

Product
6-12-12
6-12-12
6-12-12
6-12-12
6-12-12
6-12-12
6^12-12
6-12-12
10-10-10
10-10-10
10-10-10
6-12-12
FRONT HALF
In
gr/scfd
__«._..
2.95
3.18
3.07








Out
gr/scfd
.__-»___—
.068
.053
.061








In
Ib/hr
_«___
95.0
133.4
114.2








Out
Ib/hr
_____..
3%.24
2.73
2.99








In
Ib/ton
—TEST
3.80
5.34
4.57








Out
Ib/ton
VOIDED
.130
.109
.120








Eff
.«.»_...
96.6
98.0
97.3








TOTAL
In
gr/scfd
— r. — . — -•.•-
3.07
3.20
3.14
.005
.005
.005
.005
2.15
3.23
2.69
1.72
Out
gr/scfd
_.._««-*»..
.162
.083
.123
.001
.004
.001
.002
2.04
2.65
2.35
3.2?
In
Ib/hr
•-••••.
98.9
134.2
116.6
.21:
.18;
.19!
.19?
84.0 •
113.0
98.5
66.0
Out
Ib/hr


7.73
4.25
5.99
.03!
.25'
.01;
.10:
115.9
142.0
129.0
177.5
In
Ib/ton


3.96
5.37
4.67
.073
.064
.069
.069
70.0
102,5
86.3
26.9
Out
Ib/ton


.31
.17
.24
.013
.087
.006
.035
96.6
118.3
107.5
72.4
Eff
X


92.2
96.8
94.5
82.0
-36. 8b"
91.5
45.6
-38.0
-25.7
-31.9
-169.
Although negative efficiency, the value was included in average.

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             TABLE III-4
KILN DRYER/COOLER BAGHOUSE FLOW DATA
Test
No.
1-1
1-0
4-1
4-0
5-1
5-0
7-1
7-0
8-1
8-0
10-1
10-0
AVG-I
AVG-0
Flow Rate
(acfm)
38,949
29,576
38,931
29,628
37,949
27,334
40,002
29,094
39,629
28,915
38,193
28,752
38,942
28,883
Flow Rate
(scfm)
26,650
20,604
26,822
21,040
25,510
18,834
27,961
20,646
26,417
20,518
26,641
20,353
26,667
20,333
Moisture
C%)
8.71
9.85
8.95
8.85
10.63
10.43
7.47
8.44
11.68
9.16
7.36
10.31


Stack
Temp.(°F)
224
210
214
202
218
210
216
205
219
203
221
196


Isokinetic
(%)
105.7
101.1
116.4
96.7
114.2
102.5
110.4
101.0
118.0
101.6
111.3
99.2


Impinger
Catch (%)
.33
90.13
—
—
.65
75.76
.30
92.70
—
—
—
—
0.43
86.2
                   10

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         TABLE 111-5
AMMQNIATOR SCRUBBER FLOW DATA
Test
No.
11-1
11-0
14-1
14-0
15-1
15-0
16-1
16-0
17-1
17-0
18-1
18-0
AVG-I
AVG-0
Flow Rate
(acfm)
5,066
7,579
5,348
7,753
6,148
8,115
6,056
7,965
6,003
8,795
5,577
8,073
5,700
8,046
Flow Rate
Cscfm)
4,036
5,567
3,755
5,558
4,899
6,004
4,687
5,744
4,785
6,808
4,391
6,132
4,426
5,969
Moisture
C%)
12.21
13.34
22.64
16.02
12.21
12.94
12.85
15.02
9.54
10.91
10.53
13.16


Stack
Temp. (°F)
110
143
110
138
110
141
123
142
129
130
130
126


Isokinetic
(%)
	 | 	
—
99.8
113.5
104.7
107.0
105.1
105.9
107.7
102.8
107.8
95.7


Impinger
Catch (%)
^«i
—
3.90
58.1
0.55
35.8
—
—
—
—
—
—
2.22
47.0
                11

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IV   PROCESS OPERATION







     This plant produces different grades of fertilizer with ammonium sulfate as




the source of ammonia.  The sulfate is shipped from Gary, Indiana, where it is




produced as a by-product of coke oven operation.  Anhydrous ammonia and nitro-




gen solutions are also used as nitrogen sources to react with the phosphoric




acid.  Since the phosphoric acid might not react with all the ammonia, sulfuric




acid is added to pick up excess ammonia.




     The mixing of these materials  (plus some others) is carried out  in the




ammoniator which is basically a reaction vessel.  Ammonia not absorbed in  the




mixture escapes into  the air causing air pollution.  Other  emissions  from  the




ammoniator are flourides and particulates.




     The granules produced in the ammoniator are dried in a rotary dryer.




Cooling air is introduced into the rotary cooler to cool the hot material.   The




cooler gases charged with particulates are drawn by a fan located downstream of




a cyclone which serves to remove the coarse material.   The gases drawn by this




fan are discharged into the plenum of the dryer.




     The dryer is operated by natural gas and has its own blower for supplying




air to the burner.  Gases and particulates are withdrawn by an induced fan via




a baghouse and discharged into the atmosphere.  The fan is centrifugal, driven




by a 100 HP, 1725 RPM Reliance Motor.  The pulley ratio is 1:2, resulting in




about 3000 RPM on the fan shaft.  The ID of the stack is 32.5 inches.




     The granules are sized in two closed (not hooded) screens.  The first,




called the hot screen, classifies the granules leaving the dryer.  The fine




material is introduced into the cooler and coarse material into a crusher  for




reduction in size and returned for screening to the same hot screen.
                                     12

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     From the cooler, the granules are discharged over a fine screen.  Those




not passing through this screen represent the product.  The fines going




through are recycled to the ammoniator.  Raw material is fed to the ammoniator




at 25 TPH.  The recycle-to-feed ratio varies between 0.5:1 to 1.5:1.  That




means that total material handled in the ammoniator, recycle plus feed, ranges




between 40 and 60 TPH for a production rate of 25 TPH.




     A schematic diagram of the process appears in Figure IV-1.  This and




the process description were provided by EPA.
                                     13

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                     SCHEMATIC DIAGRAM OF PROCESS, USS AGRICHEMICALS NASHVILLE, TENNESSEE
                       Test Locations
                                             Test Locations
      Phosphoric Acid
             Ammonia
     Ammonium Sulfate
               H2S04
tr>
c/i
C5
Product
                                  Ai r —i
                                      ___  product Screen
                                                                             Hot Screen^
                                       Fines
                                                                                            Recycle
                                                                                                   CD
                                                                                                   73

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V   LOCATION OF SAMPLING PORTS









     Four different sampling locations were used during the tests;  therefore,




each will be discussed individually.






A.  Granulating Kiln Baghouse Inlet




     Two 2-1/2 inch diameter sampling ports were located in the granulating




kiln effluent duct.  The ports were located 90° apart and approximately 16 feet




downstream from the kiln discharge point.  Figure  V-l is a line sketch showing




the location and configuration of the sampling ports.




     The kiln effluent duct to the baghouse is constructed of 1/8 inch steel




plate, 37 inches inside diameter.  A small access platform was erected to




support the sample train during the horizontal traverse.  The vertical port




was traversed by suspending the sample box on ropes and pulleys from the




overhead roof supports.  During the vertical traverse, the sample box was




modified so that the probe extended downward vertically.  Referring to




Method 1  (Federal Register; Vol. 36; n.  247; December 23, 1971), a total of




12  sampling points  (6 on each axis) were selected.






B.  Granulating Kiln Baghouse Exit




     Two 2-1/2 inch diameter sampling ports were located in the baghouse




effluent stack, 90° apart approximately  30 feet above ground.  Figure  V-2 is




a line sketch of the baghouse, showing the location and configuration of the




sampling ports.




     The baghouse effluent stack is constructed of 1/8  inch steel plate,




32-1/2 inches inside diameter.  A3' x 8' platform extension  from the upper




baghouse platform was constructed specifically for the  project.  Access  to




the platform was provided by a vertical  ladder to  the  ground.
                                   15

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                                                             FIGURE V-l.
                   KILN  INLET TO BAGHOUSE
 Sampli ng
   Port
2 1/2" Dia.
                              16
                                               ENGINEERING-SCIENCE, INC.

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                                                                  FIGURE V-2
                        KILN BAGHOUSE STACK
                          09
Motor
                          in
                          CM
                                32-1/2
                                      r
 Sampl1ng
   Port
2 1/2" Dia.
                                                      Baghouse
                                  17
                                                    ENGINEERING-SCIENCE, INC.

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     The ports were located approximately 25 feet downstream from the baghouse



induced draft fan and 8 feet upstream from the effluent exit point.   According



to Method 1, a total of 12 sampling points (6 on each axis)  were selected.









C.  Ammpniator Scrubber Inlet



     Two 2-1/2 inch diameter sampling ports were located in the horizontal



section of the scrubber inlet duct about 25 feet above ground.   Figure  V-3



is a line sketch of the venturi scrubber, separation tank, fan and stack



showing the location and configuration of the sampling ports.  The horizontal



orientation of the duct necessitated vertical sampling in one of the ports.



A system of ropes and pulleys was used to support a standard EPA sample train



box which had been modified for this purpose.



     The scrubber inlet duct is constructed of 1/4 inch fiberglass, 18 inches



inside diameter.  A 4' x 4' working platform was constructed specifically for



the project.  Platform access was provided by a vertical ladder down to a



previously existing platform on the kiln baghouse structure.  Access to this



platform was by a vertical ladder to ground level.



     The ports were located 4 feet upstream from a 90° elbow and 10 feet
                              I


downstream from the nearest turn.  According to Method 1, a total of 12 sampling



points (6 on each axis) were selected,  Later, this was reduced to only the



6 points on the horizontal access due to the extremely large quantity of water



found to be flowing down the lower quarter diameter of the duct.  The water was



found upon inspection to be at least three inches deep in the bottom of the duct,



thus negating the possibility of sampling the lower 3 points on the vertical



axis.  Testing continued after the EPA project officer approved the plan to



utilize only the six horizontal axis points.  Figure V-4  shows  all  traverse



point locations for all stack ports.  In all cases, the points  are  numbered



consecutively, from 1 to 6 with the first point nearest the  sampling port.



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D.  Ammoniator Scrubber Outlet




     Two 2-1/2 inch diameter sampling ports were located in the ammoniator




scrubber stack, 90° apart and approximately 30 feet above ground.  The loca-




tion and configuration of the sampling ports are also shown in the line sketch,




Figure  V-3.  The ammoniator scrubber stack is constructed of 1/4 inch fiber-




glass, 24 inches inside diameter.  A 61 x 61 working platform at the building




roof line already existed before the test and no modifications or additions




were required to the structure.  Access to the platform was provided by




vertical ladders to a lower roof top and then to the ground.




     The ports were located 27 feet downstream from a forced draft fan and




 15  feet upstream from the effluent exit point.  According to Method 1, a




 total  of 12  sampling points  (6 on each axis) were selected.
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                                                              FIGURE V-3
                    LOCATION  OF SAMPLING PORTS
              •AHHONIATOR SCRUBBER INLET AND OUTLET
                                                       1/2" Dia
Induced Draft Fan
                                  20
ENGINEERING-SCIENCE, INC.

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                                                  FIGURE V-4
       TRAVERSE POINT LOCATIONS
 KILN OUTLET
 to Baghouse
  KILN STApK
from Baghouse
                                  SCRUBBER INLET
                                   SCRUBBER STACK
                  21
                                     ENGINEERING-SCIENCE, INC.

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VI   SAMPLING AND ANALYTICAL PROCEDURES




     The sample and velocity traverse points were selected as described in




Section  V.  All participate and fluoride tests, with the exception of the




ammoniator scrubber inlet, included a traverse of both axes in the stack with




ten-minute sampling times at each point.  Sampling data, however, was reported




every five minutes, twice for each sample point.  As described in Section V,




the excessive quantity of water flowing down the ammoniator scrubber inlet




duct necessitated sampling on only the horizontal axis.  Sampling times and




sequences were suggested or approved by the EPA field officer.




     Heavy particulate loading was experienced at times, expecially on the




scrubber inlet and scrubber stack, necessitating a test shutdown, change of




filter, and a test restart.  This is noted in the test log in Appendix G.






A.   Particulate Sampling




     The isokinetic sampling of particulate matter was performed using an EPA




approved sampling train.  The probe tip in test 11-1 was changed to a smaller




size in the middle of the test to keep the test isokinetic.  The probe size




used in calculations was a weighted average.  Water was used instead of  acetone




for the front half wash after each particulate  test.   Since fertilizer is




more soluble in water than acetone, a water wash would lead to  a more  efficient




recovery of particulate from the sample train.  Particulate  sample catch was




determined by Method 5, Standards of Performance  for  New Stationary Sources.






 B.   Fluoride Sampling




     The sampling of fluorides was conducted  isokinetically with a modified




 sampling train.  An unheated filter holder was  placed between the third and




 fourth  impingers and contained'a Whatman  No.  1  paper filter.   The rest of the
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train remained the same as a standard particulate train.  Sampling times were




two hours with data points recorded every 5 minutes.  AH fluoride catch was




emptied into one bottle.  Analysis consisted first of fusing insoluble fluoride




with sodium hydroxide and distilling the samples from sulfuric acid to remove




interferences, then a portion of the distillate was reacted with SPADNS




reagent.  The fluoride was determined spectrophotometrically by its bleaching




effect upon the reagent dye.  This procedure is described further in Appendix E.





C.   Ammonia Sampling




     Ammonia sampling was carried out non-isokinetically with the probe in-




serted halfway into the stack port.  Sampling  times were 60 minutes with  data




recorded every 15 minutes.  A modified sampling train was used in which the




ammonia was absorbed with dilute sulfuric acid in the first two sample




train impingers.  The rest of the train remained the same as a standard




particulate train.  A modified Kjeldahl distillation procedure recovers  the




ammonia as ammonium borate, and subsequent titration with standard sulfuric




acid solution yields the acid equivalent to isolated ammonia.  This procedure




 is described further in Appendix E.
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