United States
           Environmental Protection
           Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
EMB Report 78-NHF-4
April 1979
           Air
&EPA     Urea Manufacture
           Emission Test Report
           Agrico Chemical
           Company
           Blytheville, Arkansas

-------
                                            REPORT-ON "A" GRANULATOR SCRUBBER TESTS
                                        FOR UREA, AMMONIA AND FORMALDEHYDE EMISSIONS
                                              AND REMOVAL EFFICIENCIES,  OPACITY AND
                                          PARTICLE SIZE AND SYNTHESIS TOWER SOLUTION
                                        VENT TESTS FOR UREA AND AMMONIA EMISSIONS AT
                                                        THE AGRICO CHEMICAL  COMPANY
                                                           UREA FERTILIZER PLANT IN
                                                              BLYTHEVILLE, ARKANSAS
        THE  RESEARCH  CORPORATION
                                                     OF NEW ENGLAND
                                            ENVIRONMENTAL  CONSULTANTS
WILLARD A.  WADE  III, P.E.
PROJECT MANAGER

REED W. CASS
PROJECT ENGINEER

TRC PROJECT NO.  0998-E80-00
OCTOBER 30, 1979
EPA CONTRACT #68-02-2820
      WORK ASSIGNMENT #6
          THOMAS M. BIBB
     EPA PROJECT OFFICER
          CLYDE E. RILEY
   EPA TECHNICAL MANAGER
                                                            125 Silas Deane Highway
                                                                        Wethersfield
                                                                  Connecticut O61O9
                                                                     C2O3) 563-1^31

-------
                                TABLE OF CONTENTS -

 SECTION                                                                 PAGE
  1.0  '         INTRODUCTION	     1
  2.0           SUMMARY AND DISCUSSION OF RESULTS	    15
  3.0           PROCESS DESCRIPTION AND OPERATION  	    45
  4.0           LOCATION OF SAMPLING PORTS 	   106
  5.0           SAMPLING AND ANALYSIS METHODOLOGIES  	   115
  **  APPENDICES NOT AVAILABLE WITH THIS REPORT **
APPENDIX
   A            COMPLETE TEST RESULTS WITH SAMPLE EQUATIONS AND EXAMPLE
                CALCULATIONS
   B            PARTICLE SIZE TESTS
   C            VISIBLE EMISSIONS RESULTS
   D            EPA METHOD 1, 2, 3, 4, UREA AND AMMONIA FIELD DATA SHEETS
                FOR "A"
   E            FORMALDEHYDE DATA
   F            MISCELLANEOUS SAMPLES AND OPERATIONS FIELD DATA
   G            SYNTHESIS TOWER SAMPLING DATA
   H            SAMPLING TRAIN CALIBRATION DATA
   I            SAMPLING LOGS
   J            PROCESS OPERATION DATA
   K            TRC LABORATORY ANALYTICAL DATA
   L            ANALYTICAL DATA SHEETS AS RECEIVED FROM AGRICO CHEMICAL
                BLYTHEVILLE, ARKANSAS
   M            SAMPLING AND ANALYTICAL RESULTS
   N            CLEANUP EVALUATION RESULTS
   0            EPA AUDIT SAMPLES
   p.            PROJECT PARTICIPANTS

-------
                                LIST OF TABLES
TABLE                                                                         PAGE

 1        Daily Summary Log for "A" Granulator Sampling on October 10, 1978
            At Agrico Chemical Company in Blytheville, Arkansas .......   5

 2        Daily Summary Log for "A" Granulator Sampling on October 11, 1978
            At Agrico Chemical Company in Blytheville, Arkansas .......   ?'
          Daily Summary Log for "A" Granulator Sampling on October 12, 1978
            At Agrico Chemical Company in Blytheville, Arkansas
 4        Daily Summary Log for "A" Granulator Sampling on October 13, 1978
            At Agrico Chemical Company in Blytheville, Arkansas .......  12

 5        Daily Summary Log for Synthesis Tower Vent Sampling on October 13,
            1978 at Agrico Chemical Company in Blytheville, Arkansas  ....  13

 6        Summary of Results of Urea and Ammonia Tests on October 10 and 11,
            1978 of Gases Entering and Exiting the "A" Granulator Scrubber at
            Agrico Chemical Company in Blytheville, Arkansas  ........  1?

 7        Summary of Results of Formaldehyde, Urea, and Ammonia Tests on
            October 11, 1978 of Gases Entering and Exiting "A" Granulator
            Scrubber at Agrico Chemical Company in Blythville, Arkansas ...  18

 8        Summary of Results of Urea and Ammonia Tests on October 10 and 11,
            1978 of Gases Sampled at the "A" Granulator Scrubber Inlet (TP-1)
            At Agrico Chemical Company in Blytheville, Arkansas .......  20

 9        Summary of Results of Formaldehyde, Urea, and Ammonia Tests on
            October 11, 1978 of Gases Sampled at the "A" Granulator Scrubber
            Inlet (TP-1) At Agrico Chemical Company in Blytheville,
            Arkansas . ............ ..... .............  21

10        Summary of Results of Urea and Ammonia Tests on October 10 and 11,
            1978 of Gases Sampled at the "A" Granulator Scrubber Outlet (TP-2)
            At Agrico Chemical Company in Blytheville, Arkansas .......  22

11        Summary of Results of Formaldehyde, Urea, and Ammonia Tests on
            October 11, 1978 of Gases Sampled at the "A" Granulator Scrubber
            Outlet (TP-2) at Agrico Chemical Company in Blytheville,
            Arkansas  ............................

12        Six Minute Arithmetic Averages of October 10, 1978 Opacity Readings
            on "A" Granulator Scrubber Stack at Agrico Chemical Company in
            Blytheville, Arkansas ......................  ™

13        Six Minute Arithmetic Averages of October 11, 1978 Opacity Readings
            on "A" Granulator Scrubber Stack at Agrico Chemical Company in
            Blytheville, Arkansas ......................

-------
                            LIST OF TABLES (CONT'D)
TABLE   .           .    .   .                                                    PAGE

14        Six Minute Arithmetic Averages of October 12, 1978 Opacity Readings
            on "A" Granulator Scrubber Stack at Agrico Chemical Company in
            Blytheville, Arkansas 	  32
15        Summary of Inlet and Outlet Particle Sizing Test Results on "A"
            Granulator Scrubber at Agrico Chemical in Blytheville, Arkansas    34

16        Summary of October 10, 11, 12, 13, 1978 "A" Granulator Scrubber
            Pressure Drop Measurements at Agrico Chemical Company in
            Blytheville, Arkansas ......................  37

17        Summary of October 10 and 11, 1978 Urea, Ammonia and Formaldehyde
            Measurements on the Scrubbing Liquid Entering and Exiting "A"
            Granulator Scrubber at Agrico Chemical Company in Blytheville,
            Arkansas ...... ........... ..... ....... .......... .........  39

18        Summary of October 10 and 11, 1978 pH and Temperature Measurements
            on Individual Samples of Scrubbing Liquid Entering and Exiting "A"
            Granulator Scrubber at Agrico Chemical Company in Blytheville,
            Arkansas  ............ . ...............  ^0

19        Summary of October 11, 1978 Urea, Ammonia and Formaldehyde Measure-
            ments on the "A" Granulator Urea Melt, Product Before Screen and
            Product After Screen at Agrico Chemical Company in Blytheville,
            Arkansas  ............................  ^2

20        Summary of Results of Urea and Ammonia Tests on October 13, 1978
            of Gases in the Synthesis Tower Vent at Agrico Chemical Company,
            Blytheville, Arkansas ......................  ^3
21        Parameters Monitored During Testing At Agrico Chemical Company
            in Blytheville, Arkansas  ....................  50

22        Summary of Testing At Agrico Chemical Company in Blytheville,
            Arkansas   ............................  5(>

23        Parameter Deviations During Testing At Agrico Chemical Company
            in Blytheville, Arkansas  ....................  58

24        Parameter Deviations Between Tests At Agrico Chemical Company
            in Blytheville, Arkansas  ....................  94

25        Production Rates During Testing At Agrico Chemical Company
            in Blytheville, Arkansas  .................... 101
                                      iii

-------
                                LIST OF FIGURES
FIGURE .         ....                                                    PAGE

 1        Overhead View Showing Locations of Solution Vent and Granulators
            A, B, and C Exhaust Ducting, Scrubbers and Sampling Points at
            Agrico Chemical Company in Blytkeville, Arkansas 	      3

 2        Six Minute Arithmetic Averages of October 10, 11 and 13, 1978
            Opacity Readings on "A" Granulator Scrubber Stack at Agrico
            Chemical Company's Blytheville, Arkansas Facility  	     29

 3        Cumulative Size Distributions of Particulate in the Granulator
            A Scrubber Stack at Agrico Chemical Company in Blytheville,
            Arkansas	     35

 4        Urea Manufacturing Agrico Chemical Co. in Blytheville, Arkansas.     47

 5        Locations of "A" Granulator Scrubber Inlet Test Ports and Points
            at Agrico Chemical Company in Blytheville, Arkansas   	    107

 6        Locations of "A" Granulator Scrubber Outlet Test Ports and Points
            at Agrico Chemical Company in Blytheville, Arkansas	    109

 7        Locations of Smoke Observer for October 10-12, 1978 Opacity
            Readings on "A" Granulator Scrubber Stack at Agrico Chemical
            Chemical Company in Blytheville, Arkansas	    HI

 8        Locations of Scrubber Liquid Collection Taps for October 10 and
            11, 1978 Tests on "A" Granulator at Agrico Chemical Company in
            Blytheville, Arkansas	

 9        Location of Synthesis Tower Solation Vent Sampling Port at Agrico
            Chemical Company in Blytheville, Arkansas  	

10        Modified EPA Particulate Sampling Train August 18, 1977, Federal
            Register 	

11        Modified EPA Particulate Sampling Train August 18, 19.77, Federal
            Register	     12°

12        Modified EPA Particulate Sampling Train August 18, 1977, Federal
            Register	
                                        IV

-------
                                PREFACE






     The work reported herein vras conducted by personnel from TRC - The Research




Corporation of New England (TRC), The GCA/Technology Division (GCA),  The Agrico




Chemical Company, Blytheville, Arkansas, and the U.S. Environmental Protection




Agency (EPA).




     The scope of work issued under EPA Contract No. 68-02-2820,  Work Assignment




No. 6 was under the supervision of the TRC Project Manager,  Mr. Willard A.  Wade,




III.  Mr. Reed W. Cass of TRC served as Project Engineer and was  responsible




for summarizing the test and analytical data in this report.  Analysis of the




samples was performed at the TRC labs located in Wethersfield, Connecticut  under




the direction of Ms. Joanne J. Marchese and at the Agrico Chemical, Blytheville,




Arkansas labs under the direction of Mr. Jesse Boggan.




     Mr. Stephen V. Capone and Mr. Stephen K. Harvey of GCA were  responsible




for monitoring the process operations during the testing program.  GCA person-




nel were also responsible for writing the Process Description and Operations




Section along with Appendix J of this report.




     Members of Agrico Chemical, Blytheville, Arkansas whose assistance and




guidance contributed greatly to the accomplishment of the test program, include




Mr. Jesse Boggan, Environmental Coordinator, Mr. James Kilpatrick, Chief Chem-




ist, and Mr. Deryl Beiard, Chemist.




     Mr. Eric A. Noble, Office of Air Quality Planning and Standards, Industrial




Studies Branch, EPA, served as Test Process Project Engineer and  was responsible




for coordinating the process operations monitoring.




     Mr. Clyde E. Riley, Office of Air Quality Planning and Standards, Emission




Measurement Branch, EPA, served as Technical Manager and was responsible for




coordinating the emission test program.

-------
October 30, 1979
                                         TRC - The Research Corporation of
                                                   New England
                                              Willard A. Wade, III, P.E.
                                                  Project Manager
                                                    Reed W. Cass
                                                  Project Engineer

-------
NOTE:
     Mention of trade names or commercial products in this publication does not




constitute endorsement or recommendation for use by the Environmental Protection




Agency.
                                   vii

-------
                               SECTION 1




                             INTRODUCTION






   . Section 111 of .the Clean Air Act of 1970 charges the Administrator of




the U.S. Environmental Protection Agency (EPA) with the responsibility of




establishing Federal standards of performance for new stationary sources




which may significantly contribute to air pollution.  When promulgated,




these standards of performance for new stationary sources (SPNSS) are to




reflect the degree of emission limitation achievable through application of




the best demonstrated emission control technology.  To assemble this back-




ground information, EPA utilizes emission data obtained from controlled sources




involved in the particular industry under consideration.




    Based on the above criteria, EPA's Office of Air Quality Planning and




Standards (OAQPS) selected the Agrico Chemical Company's urea manufacturing




plant at Blytheville, Arkansas as a site for an emission test program.  The




test program was designed to provide a portion of the emission data base re-




quired for SPNSS for the processes associated with the production of urea.




    The Agrico Chemical Company's urea manufacturing plant at Blytheville,




Arkansas produces granulated urea for industrial and fertilizer usage.  The urea



                                     ®
is manufactured by three Spherodizers  or granulators which operate continuous-




ly, 24 hours a day and 7 days a week as production demands.  Emissions sampling




was conducted on the "A" granulator exhaust emissions while its urea production




rate was approximately 400 ton/day.




    Each granulator has its own impingement type water scrubber.  The granula-




tor exhaust is ducted through a scrubber and fan prior to being discharged from




a stack.  Air flow through the granulator is controlled with a dilution damper




which varies the ratio of dilution air to exhaust gas flowing to the constant
                                 -1-

-------
flow scrubber.  A schematic of the granulators'.exhaust gas ducting and control

systems .are presented as Figure 1.  Emission sampling was also conducted on the

main exhaust vent atop the urea synthesis tower (see Figure 1).   This vent

combines the various solution synthesis process gases into one common stack

before exhausting them to the atmosphere.

    EPA engaged TRC to measure urea, ammonia and formaldehyde concentrations

and mass flow rates, particle size distributions,  and plume opacities.  All

measurements made at this facility were performed during times of normal

operation of the urea production process as described in Section III, "Process

Description and Operations".

    The testing of the solids formation process was designed to characterize

and quantify uncontrolled and controlled drum granulator emissions as well as

determine the control equipment efficiency.

    The synthesis process testing was designed to characterize and quantify

emissions from one of the two newest processes expected to be installed for

future urea solution capacity expansion in the industry.

    The measurement program which was conducted at the Agrico Chemical Company

facility in Blytheville, Arkansas during the week of October 9 through October

13, 1978 consisted of the following:


"A" Granulator Scrubber Measurements
    1.  Urea and Ammonia in Gas Streams:  Three repetitions of concurrent
        inlet and outlet test runs were performed.  The tests were conducted
        in accordance with the prescribed EPA method for urea and ammonia
        and provided velocity, moisture, ammonia and urea emission data.

    2.  Formaldehyde in Gas Streams:  Three repetitions of concurrent inlet
        and outlet test runs were conducted.  The tests were conducted in
        accordance with the prescribed EPA method for determination of formal-
        dehyde and provided velocity, moisture, ammonia, urea particulate,
        and formaldehyde emissions data.

-------
                       FAN
               OUTLET
              SAMPLING
                PORTS
SAMPLING
  PORT
 SOLUTION
   VENT
TOWER FRAME
                                                 WET
                                               SCRUBBER
                                              DILUTION
                                                AIR
                     STACK

                        INLET
                      SAMPLING
                        PORTS
                                            s
                                               WET
                                             SCRUBBER
                                             DILUTION
                                         f     AIR
                                                WET
                                             SCRUBBER
                                              DILUTION
                                          f     AIR
                         STACK
                                                             GRANULATOR 'A"
WALL
                                                              GRANULATOR "B"
                                                       H    GRANULATOR
       FIGURE 1:    .- PLAN VIEW SHOWING LOCATIONS  OF SOLUTION VENT AND
                   GRANULATORS A, B AND C EXHAUST DUCTING, SCRUBBERS AND
                        SAMPLING POINTS AT AGRICO CHEMICAL COMPANY
                                 IN BLYTHEVILLE,  ARKANSAS
                                       -3-

-------
    3.  Particle Size Distributions in Gas Streams:  Three repetitions of
        inlet and outlet test runs were conducted.  The tests were per-
        formed using the prescribed procedures as instructed by the manu-
        facturer which are applicable to cascade impactors.

    4.  Visible Emissions from Stack:  Approximately eight hours of visible
        observations were recorded on the stack discharge.  Observations
        were performed in accordance with EPA Method 9 guidelines.

    5.  Gas Pressure Drop Across Scrubber:  Pressure drop measurements were
        recorded approximately every 15 minutes during the testing periods.

    6.  pH, Temperature and Urea, Ammonia and Formaldehyde Content of
        Scrubber Liquor;  Samples of inlet and outlet scrubber aqueous solu-
        tions were collected approximately every 30 minutes during the urea
        and ammonia testing.  The pH and temperature of each sample was
        recorded.  The samples were composited into 3 inlet and 3 outlet
        samples which were analyzed for urea, ammonia and formaldehyde.

    7.  Urea, Ammonia and Formaldehyde Content of Product;   Single grab
        samples of the urea melt, formaldehyde additive,  and the granulator
        product (unscreened and screened) were collected  during the urea,
        ammonia, and formaldehyde tests.  The formaldehyde additive sample
        was retained for future analysis.  In addition the product samples
        were analyzed for moisture content.
Urea Synthesis Tower Vent Measurements

    1.  Urea and Ammonia in Gas Stream:  Three repetitious test runs were
        performed according to procedures prescribed in EPA methods for
        urea and ammonia and for sampling streams with high moisture content.


    TRC personnel were responsible for collecting and measuring the above emis-

sion parameters.  Simultaneously, GCA was responsible for monitoring and record-

ing necessary process and control equipment operating parameters.

    Most of the test runs were discontinuous due to excessive loading at the

granulator inlet sampling location.  These interruptions which also delayed the

simultaneous outlet sampling were encountered throughout the test  program as

indicated in Tables 1 through 5 (Daily Summary Logs).

    The following sections of this report cover the summary of results, process

description and operation, location of sampling points,  and sampling and analy-

tical procedures.  In addition, Appendix N contains the summary of results of
                                  -4-

-------
                      TABLE  1.   DAILY SUMMARY LOG FOR "A"  GRANULATOR SAMPLING ON OCTOBER 10,  1978

                                  AT AGRICO CHEMICAL COMPANY IN BLYTHEVILLE, ARKANSAS
I
Ul
I
Clock
Time
1115
1130

1131.
1135



1139
11.45
1150
1157
1200
1215
1230
1231
1235




1240
1245
1250
1300
1310
1315
1328
1330

1.14 5
1353
1400
1415
1455
1500
1510
1515
1525
1530 •
1531
1538
1540
J545
1-)50

Production
Rate'
(tons/day)

399°





























i

394°
















































394




399

397
1

1








39.3




I





Urea b
I'artlculatc
Inlet

Started
Run 1 (Test 2)
\
Stopped
Changed
Probe
TlpB
Continued






i
Stopped
Switched
Ports
1
1
Nozzle
Plugged
Continued
1
1
f
Stopped
Nozzle
Plugp.ed

Continued
f
Completed
Run 1 (Test 2)
Started
Run 2 (Test 3)
1

1
f
Stopped
Probe
Tip
Plugged
Continued
Outlet



Started
Run 1 (Test 2)
























Stopped
Switched
Ports

Cont Lnued














Completed
Run 1 (Test 2)










Started
Run 2 (Test 3)








Stack
Visible
Emissions
Started










Stopped


































Scrubber Liquid
Inlet
pH




9.9







9.9
9.9





9.9





9.8


9.9





10. 1

10.1

10. 1



10.1



Temperature,
°C




40







40
40





40





40


40





40

36

38



38



Outlet
pll




~§7
-------
                                                                    TABLE  1  (Continued)
 i
ON
 I
Clock
Time
1600


1612
1615
1620
1630
1631


1637
1650
1700

1737

Production
Rate3
(tons/day)























C
3i>7














d
393

Urea b
Pnrtlculate
Inlet
Stopped
Switched
Ports
Continued
















Completed
Run 2 (Test 3)


Outlet














Stopped
Switched
Ports
Continued
1
1
t
Completed
Run 2 (Test 3)
Stack
Visible
Emissions
















Scrubber Liquid
Inlet .
PH
10.1




10.1





10.1




Tempernture,
°C
38




37





38




Outlet
pH
8.9




8.9





8.9




Temperature ,
°C
29




28





29




Pressure
Drop,
In 1120
16.25 '•



16.25

16.25





16.25



                                  Average production rate  value for  each test run.
                                  Urea participate samples analyzed for  ammonia  content.
                                  Inlet test runs production  rates.   Supplied by CCA.
                                  Outlet test runs production rates.  Supplied by CCA.  x

-------
TABLE 2.
DAILY SUMMARY LOG FOR "A" GRANULATOR SAMPLING ON OCTOBER 11, 1978
   AT AGRICO CHEMICAL COMPANY IN BLYTHEVILLE, ARKANSAS
Clock
Time
0918


0920


0924
0938
0947
0948

0956

0958
1004
1020
1028

1035
1040


1044
1050
1115
1120


1127
1129


1140
Production
Rate3
(tons/day)
399e


















f
399






















399


399





405





i




402






Urea h
Partlculates'
Inlet
































Outlet
































Stack
Visible
Emissions






Started
Stopped
ContM











1












Stopped





Co nt 'd








Scrubber Liquid
Inlet
PH
































Temp,
°C
































Outlet
ph
































Temp ,
°C
































Formaldehyde
Inlet



Started
Run 1
(Test 4)










Stopped
Switched
Ports
Con



t'd



Completed
Run 1
(Test 4)



Started
Run 2
(Test 5)










Outlet
Started
Run 1
(Test 4)






Stopped
Switched
Ports

Cont'd
1
Completed
Run I











Started
Run 2
(Teot 5)
t
Pressure
Drop
In, 1120














15.50


15.50




15.50
15.50
15.00




15.00


Process Material Samples
"Alr Grannlator
Melt
































Unscreened
































Screened

































-------
                                                   TABLE 2 (Continued)
i
00
I
Clock
Time

1156
1159
1200
1203
J206
1207
1209

1220
1235
1237
1239

1242
1243

1335
1340

1343
1348
1355

1111
1418
1420
1425
1428
1429


1430
1440
1445

1446
1455
1.5.10
1512
1515
1516
1518

Production
Rate3
( tonsA ay)















e










£









402


405


421

























419




































419
421


Urea b
Particulars
Inlet


















Outlet


















I











i






(






•
i
i
i




Stack
Visible
Kralsaions






























Stopped




Cont'd



































Stopped




Scrubber Liquid
Inlet
PH












































Temp,
°C












































Outlet
Ph












































Temp,
°C












































Formaldehyde
Inlet
t
Stopped
Switched
Ports
Cont'd
Stopped
Nozzl*
plugged
Cont'd










Completed
Run 2
(Test 5)
Started
Run 3
(Test 6)








Stopped
Switched
Ports
Cont'd
1

1
t
Stopped
Process
Delay
Cont'd










Completed
Run 3
(Test 6)
Outlet
1
f
Slopped
Switched
Ports

Cont'd




Completed
Run 2
(Test 5)







Started
Run 3
(Tent 6)
t
Stopped
Switched
Torts
Cont'd
Stopped
Process
Delay




Cont'd
1
i
f
Completed
Run 3
(Test 6)

Pressure
Drop
In, H20



15.00





14.60
14.60







14.00



14.00



14.00






14.00



14.00





14.20
Process Material Samples
"A" Granulator
Melt





































Grab
Snmpl c
Collected




Unscreened












































Screened













































-------
                                                   TABLE 2 (Continued)
i
VD
I
Clock
Time
1608
1610
1615

1616
1620

1626
1630


1631


1636
1639
1640
1641

1644

1645
1657
1650

1652

1707
1710

1717
1720
1723

1731


1732
1735
1740
1800
Production
Rate3
(tons/day)



e f
352 352











































































































Urea b
Particulars
Inlet








Started
Run
3
(Test 7)








Stopped
Nozzle
Plugged
Cont
'd
Stopped
Nozzle


Plugged
Cont


'd
I
1
Stopped
Nozzle
Plugged
Cont

.'d

Stopped
Switched
Ports
Cont

'd
1
Stopped
Nozzle


Plugged










Outlet




Started
llun 3
(Test 7)
Stopped
Awaiting
. Inlet to
Correct
Problems





Cont'd
































Stopped
Switched
I'orts
Cont'd






Stack
Visible
Emissions

Cont'd













































































Scrubber Liquid
Inlet
PH
9.9




10.0










10.0






9.8




9.9


10.0







10.0
9.9
Temp,
°C
40




40










38






38




38


38







39
38
Outlet
ph
8.6




8.5










8.6






8.6




8.7


8.7







8.6
8.6
Temp,
°C
29




29










29






29




29


29







29
28
Formaldehyde
Inlet









































Outlet









































Pressure
Drop
in, H20


15.00





15.50












14.50
















14.00

14.00
Process Material Samples
"A" Cranulator
Melt









































Unscreened









































Screened










































-------
                                                                        TABLE 2  (Continued)


Clock
Ti me
J302
1810
1B25
1826
1832


1850
1950

Production
Rate3
(tons/day)


1
T e f
352 352





Urea b
ParticulaLep
Inlet Outlet
Cnnt'd

1 ,
t 1




Completed Completed
Run 3 Run 3
(Test 7) (Test 7)



Stack
Visible
l-jni sslons
1
1
1
Stopped





Scrubber Liquid
Inlet
P»


10.0
JO.O






Temp ,
T.

38
39






Outlet
Pl>


8.6
8.6






Temp ,
°C

28
28








Formaldehyde
Inlet Outlet





— _




Pressure
Drop
In, H?0









(1
Process Material Samples
"A" Granulator
Melt









Unscreened

Compos! te





Composite
Composite
Screened

. Composite





• Composite
Composite
o
'Average production rate value for each test run.
 Urea particulate samples  analyzed for ammonia content.
 Formaldehyde samples also analyzed for urea and ammonia content.
 Process samples analyzed for urea, ammonia, and formaldehyde content.
 Inlet test runs production rates.  Supplied by GCA.
 Outlet test runs production rates.  Supplied by OCA.       '

-------
TABLE 3.  DAILY SUMMARY LOG FOR "A" GRANULATOR SAMPLING ON
          OCTOBER 12, 1978 AT AGRICO CHEMICAL COMPANY IN
          BLYTKEVILLE,  ARKANSAS
Mean
Time
0919

0920

0930
1100
1109

1110
1130
1200
1230
1300
1330
1420
1445
1509
1530
1629

1830
1900
1930
2000
2029

2030
Production
Ratea
(tons /day)

396b




410°







i









410

397



1



i

397


Particle Size
Inlet
Started
Run 1
Completed
Run 1























Outlet












Started
Run







'
1








Completed
Run 1


Started
Run




2


,

Completed
Run

2

Stack
Visible
Emissions















Started
t
Stopped









Pressure
Drop
in, H20




16.75
16.75


16.50
15.75
15.25
15.75
15.75
15.00
14.75





15.25
15.25
15.50
15.00


15.00
 Average production rate for each test run.
 Inlet test runs  production rates.   Supplied by GCA/Technology.
"Outlet test runs production rates.   Supplied by GCA/Technology.
                               -11-

-------
TABLE 4.
DAILY SUMMARY LOG FOR "A" GRANULATOR SAMPLING ON
OCTOBER 13, 1978 AT AGRICO CHEMICAL COMPANY IN
BLYTHEVILLE, ARKANSAS
Mean
Time
0820
0855

0900
0915
0930
1000
1030
1100
1130
1140
1200
1230
1255

1300
1316


1317

1330
1400
1430
1500
1508

1509

Production
Rate3
(tons/day)

359°









l












359



"k
350°








371b

Particle Size
Inlet
















Started

Run 2
Completed
Run 2




Started
Run 3
Completed
Run 3
Outlet

Started
Run 3








i











Completed
Run 3














Pressure
Drop
in, H20
16.00


16.50
15.50
16.00
15.50
15.50
15.50
16.00
16.00
16.50
16.25


16.50





17.00
16.50
18.00
16.50




     Average production rate value  for each  test run.

     Inlet  test runs production rates.  Supplied by GCA/Technology.
     •»
     "Outlet test runs production rates.  Supplied by GCA/Technology.
                              -12-

-------
TABLE 5.  DAILY SUMMARY LOG FOR SYNTHESIS TOWER VENT SAMPLING ON
          OCTOBER 13, 1978 AT AGRICO CHEMICAL COMPANY IN BLYTHEVILLE,  ARKANSAS
Clock
Time
0930

0945
1030

1046

1130
1145
a
Production
Rate
(tons/day)

1100


1100


1100

Ureab
Particulates
Started Run 1

Completed Run 1
Started Run 2

Completed Run 2

Started Run 3
Completed Run 3
Process Sample
Formaldehyde
Additive






i
Grab Sample
Collected

   Production rate, tons/day of 99.5 percent urea solution based on
  feed rate of ammonia to synthesis process.

   Two trial runs were conducted on October 12, 1978, however, they
  were not analyzed for urea and ammonia content.
                                 -13-

-------
cleanup evaluations performed on the sample collectors used for the test




program.  The Quality Assurance Audit samples analysis results supplied by




the EPA are included in Appendix 0.  Detailed descriptions of methods and




procedures, field and laboratory data, and calculations are presented in




various appendices, as noted.
                                  -14-

-------
                               SECTION 2

                   SUMMARY AND DISCUSSION OF RESULTS



INTRODUCTION

     This section presents the results of a testing program conducted during the

week of October 9 through 13, 1978 at the Agrico Chemical Company Facility in

Blytheville, Arkansas.  Testing was performed on gas and water streams entering

and exiting the "A" Granulator Scrubber and on the gas stream venting from the

Synthesis Tower.

     The inlet gas sampling location for the "A" Granulator Scrubber (designated

TP-1) was in a 30-foot straight section of horizontal duct.  The integrated gas

samples for the urea, ammonia and formaldehyde tests were collected isoki-

netically from 24 traverse points which were determined in accordance with EPA

Reference Method I.1  The gas samples for the particle sizing tests were col-

lected from a single point located at the centroid of the duct's cross sectional

area.

     The outlet gas sampling locations for the "A" Granulator Scrubber (desig-

nated TP-2) was in the 85-foot vertical stack.  The integrated gas samples for

the urea, ammonia and formaldehyde teats were collected isokinetically from 12

traverse points which were also determined from EPA Reference Method 1.  The gas

samples for the particle sizing tests were collected from the centroid of the

duct's cross sectional area.

     The gas sampling location for the Solution Tower Vent was in the 45-foot

straight section of vertical duct.  "The-samples were extracted from a single

point located at the centroid of the duct's cross sectional area.
 Standards of Performance for New Stationary Sources, Appendix A.  Federal
Register, Vol. 42, No. 160-Thursday, August 18, 1977, pp. 41756-41758.


                                  -15-

-------
     The following sections present summary tables of results and narrative on




the testing.  The Appendices contain all the pertinent data and information on




the testing.  Appendix N contains the results of the analyses of samples of the




pretest cleanup of the sampling train and the deionized distilled water blank.









UREA AND AMMONIA TESTS ON "A" GRANULATOR SCRUBBER




     The summaries of the urea and ammonia results at the "A" Granulator inlet




(TP-1) and outlet (TP-2) are contained in Tables 6 and 7.  It should be noted




that the Run Numbers and TRC Test Numbers do not coincide.  This is because




there were two types of tests performed on the gases entering and leaving "A"




Granulator.  One type of test was primarily for urea and ammonia and the other




type was primarily for formaldehyde.  The Run Numbers signify the position of




the tests in the sequence for each type of test.  The TRC Test Numbers signify




the position of the tests in the sequence of all the urea and ammonia and for-




maldehyde testing on "A" Granulator.  TRC Test Number 1 was performed as a




preliminary test to determine the moisture content  of the gas streams.




     The calculated urea removal efficiency of the "A" Granulator Scrubber




(Tables 6 and 7) averaged 99.9%.  The calculated ammonia removal efficiency of




the "A" Granulator Scrubber (Tables 6 and 7) was always less than zero.  A check




of the ammonia concentration of the water solution entering and leaving the




scrubber (Table 13) shows the water entering the scrubber to have a higher




ammonia concentration than that leaving and thus indicates that some of the am-




monia was stripped from the scrubber water,  thus increasing its concentration




in the air stream.
                                  -16-

-------
                 TABLE  6.  SUMMARY OF  RESULTS OF UREA AND  AMMONIA TESTS ON OCTOBER  10 AND 11,  1978
                             OF GASES ENTERING AND EXITING THE "A" GRANULATOR SCRUBBER AT  AGRICO
                             CHEMICAL COMPANY  IN BLYTHEVILLE,  ARKANSAS
Run Number (TKC Test Number)
Loca t ion
Date
Time
Volume of Gas Sampled — DSCF3
Percent Moisture by volume
Average Stack Temperature — °F
Stack Volumetric Flow Rate — DSCFM°
Stack Volumetric Flow Rate-AGFM'
Pressure Drop Across Scrubber — in. 11^0
Scrubber Liquid — pll
Percent Isokinetic
Percent Opacity Average
Production Rate — Tons/ Day
Net Sampling Time — Minutes
Urea Concentrations and Mass Flow Rates
(Ana lysis Procedures-Co lorimetric)
1 gr/DSCFd
— ' /»fre
^j gr/ACr

Ib/ton
Collection F.fficiency, Percent
Run 1 (Test 2)
Inlet
10-10-78
11:30-14:15
88.09
1.6
1.61
4H.970
58,700

9.9
96.7

397
120


64,280
11.26
9.394
4,726
286.1
99.
Outlet
10-10-78
11:31-13:36
107.8
4.3
100
52,020
57,410
17.9
8.9
97.9
5.0
392
120


39.52
0.005659
0.005127
2.523
0.1544
9
Run
Inlet
10-10-78
15:00-17
71.05
2.1
163
50,020
60.480

10
95.4

387
96


60,090
13.05
10.79
5,594
347.2

2 (Test 3)
Outlet
10-10-78
:20 15:31-17:37
109.90
4.1
98
53,090
58,260
16.3
8.9
97.8
No Readings
391



73.94
0.01038
0.009458
4.723
0.2898
99.9
Run 3 (Test 7)
Inlet
10-11-78
16:16-18;
56.68
2.8
161
50,670
61,940

10
100.2

350
72


40,200
10.94
8.952
4,753
325.7

Outlet
10-11-78
:32 16:16-18:32
1.1.5.0
3.4
103
55,420
61.,. 3 70
14.6
8.6
98
1.1
350
120


62.03
0.008324
0.007516
3.953
0.271
99.9
Average
Inlet

_
71.94
2.2
162
49,890
60,370

10
97.4

378



54,860
11.75
9.712
5,024
3.1.9 . 7
99.
Outlet

_
1 10.9
3.9
100
53,500
59,020
16.267
8.8
97.2
3.1
378



>8.50
0.008121
0.007367
3.733
Q.23C4
9
Ammonia Concentrations  and Mass
  Flow Rates
(Analysis Procedure-Direct
  Nesslerizatiou)
mg
gr/DSCF
gr/ACF

Ib/ton
Collection Efficiency, Percent
533.0 1,352 416.4 2,572 298.4 2,1.02 415.9 2,008
0.09337 0.1936 0.0942 0.361 0.08123 0.2821 0.08960 0.2728
0.07789 0.1754 0.07478 0.329 0.06644 0.2547 o 0730 0 >591
39.19 86.31 38.77 164.3 35.28 134 37.75 128.20
2.372 5.282 2.406 10.08 2.418 9.182 2.399 8 181
'0' <0 <0 <0
    'Dry standard cubic feet at 68°F,  29.92 in Hg.

     Dry standard cubic feet per minute at 68°F,  29.92 in Hg.

     Actual cubic feet per minute.

     Grains per dry standard cubic foot at 68°F,  29.92 in llg.
    £
     Grains per actual cubic foot.

     Ammonia collection efficiency <0  because ammonia was stripped from scrubber water which enriched  the ammonia
     concentration In the scrubber outlet air.

-------
           TABLE 7.   SUMMARY OF RESULTS OF  FORMALDEHYDE, UREA,  AND AMMONIA TESTS  ON OCTOBER  11,  1978
                        OF  GASES ENTERING  AND  EXITING "A"  GRANULATOR  SCRUBBER AT AGRICO  CHEMICAL COMPANY
                        IN  BLYTHEVILLE, ARKANSAS
oo
Run Number (TRC Test Number)
Location
Time
Date
Volume of Cas Sampled — USCFa
Perr.unt Moisture by Volume
Average Duct Temperature — °F .
Duct Volumetric Flow Rate — DSCFH
Duct Volumetric Flow Rate — ACFM°
Pressure Drop Across Scrubber — in
Percent Isoklnetlc
Net Sciinpl Ing Time — Minutes
I'ercent Opacity Average
Production Rate — Tons/Day
Formaldehyde Concentrations and
Mass Flow Kates
(Analysis Procedure-Co lorlme trie)
"'8 8 d
(;r/ACFd
(•r/DSCF
Ib/hr
Ib/ton
Collection Efficiency, Percent

Run 1 (Test 4)
Inlet Outlet
0920-1040 0918-1028
10-11-78 10-U-78
58.86 59.04
1.6 5.4
157 99
52,4.10 55,350
62,760 61'960
"8 15.50
•100.6 100.8
72 60
5.0
397 397



1.240
0.0002714
0.000325 h
0.146
0.008828

Rates

42,000
9.194
11.01 I,
4,946
299





357
0.07814
0.09358 h
42.04
2.541

	 . 	
(tun 2
Inlet
1120-1242
10-11-78
58.06
2.4
162
50,270
61,290
14.9
103.5.
72

400



0.304
0.00006626
0.00008079
0.035
0.002091



40,420
8.811
10.74
4,629
278
99.




231
0.05035
0.06139
26.45
1.589


(Test 5)
Outlet
1129-1239
10-11-78
57.56
4.1
102
54,380
60.560

100
60
3.7
400



0.47
0.0001131
0.0001260
0.05873
0.003525
0


46.9
0.01129
0.01257
5.86
0.3518
9




500
0.1204
0.1340
62.48
3.75
<0j>

Run
Inlet
1335-1516
10-11-78
58.2
2.7
168
50,550
62,480
14.1
103.2
72

419



1.610
0.0003452
0.0004267
0.1849
0.01059



38,111
8.172
10.10
4,376
250.8





243.3
0.05217
0.06449
27.94
1.601


3 (Test 6)
Outlet
1348-1515
10-11-78
55.9
4.3
105
53,550
60,060

98.6
60
3.7
417



0.259
0.00006374
0.00007150
0.03282
0.001887



12.4
0.003052
0.003423
1.571
0.09035
100




607.9
0.1496
0.1678
77.02
4.429
<0

Average
Inlet Outlet


58.38 57 ..5
2.3 4.6
162 1Q2
51,080 54,430
62,180 60,860
14.83
102.4 99.8
72 60
4.1.
405 405



1.05 0.365
0.0002275 0.0000884
0.0002775 0.00009875
0.122 0.04578
0.007170 0.002706



40,180 29.65
8.726 0.00717
10.62 0.00800
4,650 3.72
275.9 0.2211
99.9




277.1 554
0.06022 0.135
0.07315 0.1509
32.14 69.75
1.910 4.090
<0

              aDry standard cubic  feet  at 68°F, 29.92 in Hg.
              ^cy standard cubic  feet  pur minute at 68°F, 29.92 in Hg.
               Actual cubic fcut per minute.
Grains per actual cubic foot.

Grains per dry standard cubic foot.
Ammonia results should be  1 ess for these runs because  (00% capture
was not achieved (No  IN ll?SOi, in Train)-
Ammonia col lection effIcienry <0 because ammonIn was strIpped from
scrubber water whi cb  onr It-hud the ammonia concent rat ion iu the scrubber
outlet air.
                    of ^^^ lo;;^

-------
UREA RESULTS AT "A" GRANULATOR SCRUBBER.INLET (IP-1)





    A summary of the urea results of the urea and ammonia tests of gases sam-




pled at the "A" Granulator Scrubber Inlet (TP-1) is presented in Table 8.




The urea results are presented based on two methods of analysis.  The colori-




metric analysis was performed at the TRC Laboratory in Wethersfield, Connecticut




by TRC chemists and the Kjeldahl analysis was performed at Agrico in Blytheville,




Arkansas by Agrico chemists.  Comparison of averages (Table 8) of the urea




results shows the colorimetric results to be 8% higher than the Kjeldahl results.




The average urea mass flow rates at TP-1 as determined by the colorimetric and




Kjeldahl analyses were 5,024 and 4,853 pounds per hour, respectively.




    A summary of the urea results of the formaldehyde tests at TP-1 is presented




in Table 9.  The average urea mass flow rates at TP-1 was 4,650 pounds per hour.




The approximately 350 lb per hour difference between the urea mass flow rates




measured during the urea and ammonia tests and the formaldehyde tests is most




difficult to explain.  The urea production rate averaged 380 tons/day for the




urea and ammonia tests versus 408 tons/day for the formaldehyde tests.  This




would indicate that a higher urea mass flow rate should be present during the




formaldehyde tests.  The inlet sampling trains were modified for the formaldehyde




tests by removing the t^SO, impingers.  However, the maximum percent of the




total urea mass collected in the I^SC^ impingers was only 0.002% for the urea




and ammonia tests, making their contribution insignificant.









UREA RESULTS AT "A" GRANULATOR SCRUBBER OUTLET (TP-2)





    A summary of the urea results for the urea and ammonia tests at the "A"




Granulator Scrubber Outlet (TP-2) is presented in Table 10.  The outlet urea




results are also presented on the colorimetric analysis and the Kjeldahl analysis.




Comparison of the averages (Table 10) of the urea results shows the Kjeldahl
                                 -19-

-------
                TABLE 8.   SUMMARY  OF RESULTS  OF UREA  AND AMMONIA TESTS  ON OCTOBER 10  AND  11,  1978
                            OF  GASES SAMPLED AT THE "A" GRANULATOR SCRUBBER INLET  (TP-1) AT AGRICO
                            CHEMICAL COMPANY IN BLYTHEVILLE,  ARKANSAS
















1
NJ
O
1








Run Number (TRC Test Number)
Date
Volume of Gas Sampled — DSCFa
Percent Moisture of Volume
Average Stack Temperature — °F
Stack Volumetric Flow Rate-DSCFM
Stack Volumetric Flow Rate-ACFML
Percent Isokinetic
Net Sampling Time — Minutes
Production Rate — Tons/Day
Urea Concentrations and Mass
Flow Rates .
(Analysis Procedure)
mg
gr/DSCF
Rr/ACFf
Ib/br
Ib/ton

Ammonia Concentrations and
Mass Flow Rates
(Analysis Procedure)6
mg
gr/DSCF
gr/ACFf
Ib/br
Ib/ton
Run 1 (Test 2)
Run 2 (Test 3)
10-10-78
88.09
1.6
161






48,970
58,700
96.7
120.
397


Colorlmetric
64,280
11.26
9.394
4,726
286.1


Direct
Nesslerization
533
0.09337
0.07789
39.19
2.372






Kjeldnhl
62,984
11.11
9.27
4,664
282.4


Distillation
Titriroetric
387
0.06784
0.0566
28.47
1.723






10-10-78
71.05
2.1
163
50,020
60,480
95.4
96
387


Colorlmetric Kjcldalil
60,090
13.05
10.79
5,594
347.2


Direct
58,241
12.57
10.40
5,390
334.6


Distillation
Nesslerization Titrimetric
416.4
0.0942
0.07478
38.77
2.406
h
-
-
-
—
Run 3 (Test 7)











10-11-78
56.68
2.8
161
50,670
61,940
100.2
72.
350


Colorimetric Kjeldahl
40,200
10.94
8.952
4,753
325.7


Direct
37,638
10.24
8.384
4,451
305


Distillation
Nesslerization Titrimetric
298.4
o.osm
0.06644
35.28
2.418
h
-
-
-
"











Average

71.94
2.2
162
49.H90
60,370
97.4
96.0
378


Colorlmetric Kjcldalil
54.H60
11.75
9.712
5,024
319.7


Direct
Nessle
415.9
0.0896
0.0730
37.75
2.399
52,954
11.35
9.39
4,853
308.8


Distillation
rization Titrimetric
h
-
-
-•
"
'Dry  standard cubic feet at 68°F,  29.92 in. Hg.
 Dry  standard cubic feet per minute at 68°F,  29.92 in. Hg.
(•
 Actual cubic feet per minute.
 Colorimetric analysis conducted by TRC personnel; Kjeldali] analysis conducted by Agrico personnel.
efirains per dry standard cubic foot, 68°F,  29.92 in.  Hg.
 Grains per actual cubic foot.
8Direct Nesslerization analysis conducted by  TRC personnel; distillation followed by titrimetrlc determination
 conducted by Agrico personnel.
Negative values  (see Table l.-l for additional information).

-------
                      TABLE  9.   SUMMARY OF RESULTS OF  FORMALDEHYDE,  UREA,  AND AMMONIA  TESTS  ON OCTOBER  11,  1978

                                 OF  GASES  SAMPLED AT THE "A"  GRANULATOR SCRUBBER  INLET  (TP-1)  AT AGRICO  CHEMICAL

                                 COMPANY IN BLYTHEVILLE, ARKANSAS
i
to
Run Number (TRC Test Number)
Date
Volume of Gas Sampled — DSCF3
Percent Moisture by Volume
Average Duct Temperature — "f
Duct Volumetric FJow Rate — DSC KM
Duct Volumetric Flow Kate — ACFMC
Pressure Drop Across Scrubber — In. HgO
Percent Isokinetic
Net Sampling Time — Minutes
Production Rate — Tons/Day
Forma Idebyde Concentrations and Mass Flow Rates
(Analysis Procedure-Colo rime trie)
'"« d
gr/OSCF
gr/ACFe
Ih/lir
Ib/ton
Urea Concentrations and Mass Flow Rates
(Analysis Procedure-Co lorine trie)
rag d
gr/DSCF
gr/ACF
Ib/hr
Ib/ton
Ammonia Concentrations and Mass Flow Rates
(Analysis Procedure-Direct Nesslerization)
mg .
gr/DSCF
gr/ACFe
Lb/hr
Ib/ton
Run 1 (Test 4)
10-11-78
58.86
1.6
157
52,410
62.760
15.5
100.6
72
397


1 . 240
0.00032!;
0.0002714
0.146
0.00882R


42,000
1.1.01
9.194
4,946
299


357
0.09358
0.07814
42.04
2.541
Run 2 (Test 5)
10-11-78
58.06
2.4
162
50=270
6,1290
14.9
103.5
72
400


0.304
0.00008079
0.00006626
0.035
0.002091


40,420
10.74
8.811
4,629
278


231
0.06139
0.05035
26.45
1.589
Run 3 (Test 6)
10-11-78
58.21
2.7
168
50,550
62,480
14.1
103.2
72
419


1.610
0.0004267
0.0003452
0.1849
0.01059 •


38,111
10.1
8.172
4,376
250.8


243.3
0.06449
0.05217
27.94
1 . 601
Average

58.38
2.3
162.33
51,080
62,180
14.83
102 . 4
72
405


1.05
0.0002775
0.0002270
0.1220
0.007170


40,180
10.62
8.726
4,650
275.9


277.1
0.07315
0.06022
32.14
1.910
         Dry standard cubic  feet @ 68°F,  29.92 in. Hg.


         Dry standard cubic  feet per minute @ 68°F, 29.92 in.  Hg.

        Q
         Actual cubic feet per minute.


         Grains per dry standard cubic foot.

        f>
         Grains per actual cubic foot.


         Ammonia results should he le.'.s for these runs  because 100% capture was not achieved (No IN lljSOi, in Train).

-------
            TABLE  10.  SUMMARY OF RESULTS OF  UREA  AND AMMONIA TESTS ON OCTOBER 10 AND 11,  1978
                         OF GASES SAMPLED  AT THE "A" GRANULATOR SCRUBBER OUTLET  (TP-2)  AT  AGRICO
                         CHEMICAL COMPANY  IN BLYTHEVILLE,  ARKANSAS















1
M
M
1






Run Number (TRC Test Number)
Date
Volume of Gas Sampled — DSCF
Percent Moisture by Volume '
Average Duct Temperature — °F
Duct Volumetric Flow Rate-DSCFM5
Duct Volumetric Flow Rate-ACFM°
Pressure Drop Across Scrubber-
in. , I120
Percent Isokinetic
Net Sampling Time — Minutes
Percent Opacity Average
Production Rate — Tons/Day
Urea Concentrations and
Mass Flow Rates .
(Analysis Procedure)
mg
gr/DSCF '
gr/ACFf
Ib/hr
Ib/ton
Ammonia Concentrations and
Mass Flow Rates
(Analysis Procedure)*'
Run 1 (Test 2)














10-10-78
107.8
4.3
inn.
52,020
57,410

17.9
97.9
120.
5.0
392


Colorimetric Kjeldahl
39.52
0.005659
0.005127
2.523
0.1544


Direct
53.1
0.00786
0.0072
3.521
0.215


Distillation
Nesslerization Tit rime trie





mg
gr/DSCF
gr/ACF
lh/hr
ib/ton
1,352
0.1936
0.1754
86.31
5.282
1,791
0.232
0.256
114.17
6.987
Run
2 (Test 3)
Run 3 (Test 7)
10-10-78









No



Colorimetric
73.94
0.01038
0.009458
4.723
0.2898


Direct
109.90
4.1
98.
53,090
58,260

16.3
97. b
120.
Readings
391


Kjeldahl
128.0
0.02384
0.01634
8.158
0.5006


Distillation
Nesslerization Titriraetric
2,572
0.361
0.329
164.3
10.08
3,261
0.4571
0.4166
208.1
12.76













10-11-78
115.0
3.4
103.
55,420
61,370

14.6
98.0
120.
1.1
.350


Colorimetric Kjeldahl
62.03
0.008324
0.007516
3.953
0.271


Direct
75.5
0.0093
0.0103
4.861
.333


Distillation
Nesslerization Titrimetric
2,102
0.2821
0.2547
134
9.182
2,045
0 . 249
0.276
131.3
8.997














Average

110.07
• 3.93
100.3
535.0
52,020

16.3
97.2
120.
3.1
37b


Colorimetric KjeJdulil
58.5
0.008993
0.007637
3.733
0.2384


Direct
85.5
0.0137
0. 01128
5.513
.3495


Distillation
Nesslerization Titrimetric:
2,008
0.2789
0.2530
128.2
8.181
2,366
0.3127
0.3162
151.2
9.581
 Dry standard cubic feet at 68°F, 29.92  in llg.
 Dry standard cubic feet per minute at 68°F, 29.92 in llg.
 Actual cubic feet per minute.
 Colorimetric analysis conducted by TRC  personnel; Kjeldahl analysis conducted by Agrico personnel.
eCrains per dry standard cubic  foot at 68"F, 29.92 in Hg.
 Grains per actual cubic foot.
^Direct nesslerization analysis conducted by TRC personnel; distillation followed by tltrimetric determination
 conducted by Agrico personnei.

-------
results  to be 48% higher than the color line trie results.


    The  average urea mass flow rates at TP-2  (Table 10) as determined by the


colprimetric and Kjeldahl analyses were 3.733 and 5.513 pounds per hour,


respectively.


    A summary of the urea results of the formaldehyde tests at TP-2 is pre-


sented in Table 11.  The average urea mass flow rate at TP-2 was 3.715 pounds


per hour.


    The  results show large differences in the urea mass flow rates measured at


TP-2 for both the urea and ammonia tests (2.523 to 4.723 Ib/hr) and the formal-


dehyde tests (1.571 to 5.860 Ib/hr).  These differences are believed to have


been the result of the build up and periodic dislodgement of urea on the fan,


breeching and stack walls.  Water sprays were used twice a day to remove urea


from the fan to prevent vibration.   Testing was delayed for fan wash down.




AMMONIA  RESULTS AT "A" GRANULATOR SCRUBBER INLET (TP-1)


    A summary of the ammonia results of the urea and ammonia tests of gas sam-


pled at  the "A" Granulator Scrubber Inlet (TP-1) is presented in Table 8.  The


ammonia  results are presented based on two methods of analysis.  The analysis


by direct Nesslerization was performed at the TRC Laboratory in Wethersfield,


Connecticut by TRC chemists and the distillation/titrimetric analysis was per-


formed at Agrico in Blytheville, Arkansas by Agrico chemists.  The distillation/


titrimetric method was done in addition to the direct Nesslerization because


of interferences in the direct Nesslerization method.  However,  it is documented


in the literature that during preliminary distillation analysis approximately 7

                                           1
percent of the urea is converted to ammonia  .   Since there was  such a high con-


centration of urea (11.75 gr/dscf)  compared  to ammonia (0.0896  gr/dscf-by direct


Nesslerization),  a small deviation  from the  7  percent conversion factor would mean a
Standard Methods, 14th Edition,  1975,  p.  408


                                  -23-

-------
                    TABLE  11.   SUMMARY OF  RESULTS  OF FORMALDEHYDE, UREA,  AND  AMMONIA TESTS  ON OCTOBER 11,  1978
                                OF  GASES SAMPLED AT THE "A" GRANULATOR  SCRUBBER OUTLET (TP-2)  AT AGRICO  CHEMICAL
                                COMPANY IN  BLYTHEVILLE, ARKANSAS
-P-
I
Run Number (TRC Test Number)
Date
Volume of Cas Sampled — DSCFa
1'ercent Moisture by Volume
Average Duct Temperature — °F
Duct Volumetric Flow Rate — DSCFM
Duct Volumetric Flow Rate — ACFMC
Pressure Drop Across Scrubber — in l^O
Percent Isokinctic
Net Sampling Time — minutes
Percent Opacity Average
Production Rate — Tons/Day
Formaldehyde Concentrations and Mass Flow Rates
(Analysis Procedure)
">g .
gr/DSCF
gr/ACFG
Ib/hr
1 1)/ ton
Urea Concentrations and Mass Flow Rates
(Analysis Procedure)
mg
gr/DSCF
fir/ACF
Ib/hr
Ib/ton
Ammonia Concentrations and Mass Flow Rates
(Analysis Procedure)
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton
Run 1 (Test 4)
10-11-78
59.04
5.4
99
55,350
61.960
15.5
100.8
60
5.0
397





f





f







f

Run 2 (Test 5)
10-11-78
57.56
4.1
102
54,380
60,560
U.9
100
60
3.7
400


0.47
0.0001260
0.0001131
0.05873
0.003525


46.9
0.01257
0.01129
5.86
0.3518


500
0.1340
0.1204
62.48
3.75
Run 3 (Test
10-11-78
55.9
4.3
105
53,550
60,060
14.1
98.6
60
3.7
417


0.259
0.00007150
0.00006374
0.03282
0.001887


12.4
0.003423
0.003052
1.571
0.09035


607.9
0.1678
0.1496
77.02
4.429
6) Average

57.5
4.6
102
54.430
60.H60
14.83
99.8
60
4.1
405


.365
0.00009875
0.0000884
0.04578
0.002706


29.65
0.00800
0.00717
3.72
0.2211


554
0.1509
0.135
69.75
4.090
         3Dry standard cubic feet at 68°F, 29.92 in.  Hg.
         ''Dry standard cubic feet per minute nt 68°F,  29.92 in. llg.
         'Actual cubic feet per minute.
         Grains per dry standard cubic feet.
         Grains per actual cubic feet.
         Results vii i dec! -  portion of sample hist.

-------
considerable change in the amount of ammonia in the sample.  When the values




measured for ammonia by the distillation/titrimetric method were corrected




for the 7 percent conversion of urea, the net ammonia concentrations were




negative.  Appendix L has additional information concerning conversion of




urea to ammonia and the impact on the ammonia results.




     The average ammonia mass flow rate at TP-1 as determined by direct Nes-




slerization was 37.75 Ib per hour.




     A summary of the ammonia results of the formaldehyde tests as TP-1 is




presented in Table 9.  The average ammonia mass flow rate was 32.14 Ib per




hour.  It was expected that the ammonia which was collected by the formalde-




hyde tests would be less than that during the urea and ammonia tests because




IN I^SO^ was not used in the formaldehyde train.  However, two water impingers




(.100 ml distilled/deionized H20 each) were used in the formaldehyde train




while only one water impinger (100 ml distilled/deionized 1^0) was used in




the urea and ammonia tests.  The differences in ammonia emissions as measured




by both, methods is not significant.









AMMONIA RESULTS AT "A" GRANULATOR OUTLET (TP-2)




     A summary of the ammonia results of the urea and ammonia tests at the




"A" Granulator Scrubber Outlet (TP-2) is presented in Table 10.  The samples




were analyzed by the direct Nesslerization and distillation/titrimetric




methods as explained in the two previous sections.  Since the urea in the




sample was low (58.5 mg) compared to the ammonia (2009 mg), the correction




for the 7 percent converstion to urea to ammonia during distillation was small




compared to the amount of ammonia measured and, therefore, did not alter the




results.  The average ammonia mass flow rates determined by the direct
                                     -25-

-------
 Nesslerization and  distillation/titrimetric methods were  128.2  and  151.2  Ib




 per hour,  respectively.




      A summary of the ammonia results  of  the  formaldehyde tests at  TP-2  is




 presented  in Table  11.   The average ammonia mass  flow rate at TP-2  was 69.75




 Ib/hr.   Again, as described in the previous section,  it was expected  that the




 ammonia measured by the  formaldehyde train would  be less  than that  collected




 in the urea and ammonia  train because  the formaldehyde train did not  have the




 IN t^SO^ in the impingers.   These outlet  ammonia  values are effected  substantially




 by the sampling method as  anticipated.









 SAMPLING AND ANALYSIS PROBLEMS WITH UREA  AND  AMMONIA  TESTS




      The main sampling problem occurred at the  scrubber inlet (TP-1)  and  was




due to the  high concentration and large size of  the urea particles.  This  caused




 plugging of both the pitot tubes and the  sample probe and nozzle.   The problem




 of plugging of the  pitot tube was alleviated  by pumping air through the pitot




 tube side  facing upstream.   This purge line was removed and the pitot recon-




 nected  to  the manometer  for velocity readings.  The problem of  the  nozzle




 plugging was never  eliminated and the  system  had  to be frequently shut down




 and the nozzle cleaned.  The plugging was minimized by inserting the  probe




 into the duet with  the nozzle facing downstream.   The probe was rotated 180




 into the flow stream immediately before the initiation of  sampling.   The  probe




 was removed from the duct  in the reverse order. To reduce further the risk .of




 plugging,  we used the largest nozzle for which  we could still maintain an




 isokinetic flow rate.  This large nozzle  increased sample  velocities  through




 the probe  thus reducing  agglomeration at  the  various  fittings in the  probe




 assembly.
                                      -26-

-------
     The four major problems which, were enountered during analysis were inter-




ferences, sensitivity of analytical instrumentation, conversion of urea to




ammonia and contamination of either glassware and/or sampling and wash water.




The interferences showed up on the blank wash up of the clean glassware in that




the ammonia samples had high absorbance.values but had a green instead of a




yellow color which is expected for the ammonia.  During analysis, each sample




was checked to assure that sample color was consistent with that expected




Csee Appendix K).  Analysis of the water blank found evidence of ammonia con-




tamination at the level of 0.14 mg/1.   This was insignificant compared to




sample ammonia concentrations.  Some of the measurements were made just above




the limit of sensitivity of the spectrophotometer and, therefore, the error




involved could be substantial.  Conversion of urea to ammonia occurs when a




sample containing a large amount of urea and a small amount of ammonia




(.in comparison to the urea) is distilled.   It has been documented that




approximately 7% of the urea is converted to ammonia.  A correction for




urea conversion to ammonia was applied to the results of the Agrico analysis




by distillation and many of the results were calculated to be negative.









FORMALDEHYDE RESULTS AT GRANULATOR "A" SCRUBBER INLET (TP-1)




     A summary of the formaldehyde results of gas sampled at the "A" Granulator




Scrubber Inlet TP-1 is presented in Table 9.  The average formaldehyde mass flow




rate was 0.122 Ib/hr.  Examination of the formaldehyde mass flow rates for each




of the three tests reveals that Run #2 had a much lower formaldehyde mass flow




rate than either Run #1 or #3 while the Scrubber Outlet (TP-2) mass flow rates




for Run #2 and #3 were similar with Run #2 having the highest formaldehyde




mass flow rate.  However, Run #1 for formaldehyde was voided due to a portion




being lost.
                                  -27-

-------
FORMALDEHYDE RESULTS AT GRANULATOR "A" SCRUBBER OUTLET




     A summary of the formaldehyde results of gas sampled at the "A" Granulator




Scrubber Outlet TP-2 is presented in Table 11.  The average formaldehyde mass




flow rate was 0.046 lb/hr.  The results of the formaldehyde tests are somewhat




questionable because the results of the analysis of the clean impinger samples,




done prior to testing,  indicate contamination of the same magnitude as the




concentrations measured during some of the tests.   This problem is dealt




with more thoroughly in Appendix N.









SAMPLING AND ANALYSIS PROBLEMS WITH FORMALDEHYDE BESIGNATED TESTS




     The only sampling problem encountered was plugging at the scrubber inlet




(TP-1) which has already been discussed in the previous subsection




An analysis problem did occur in that the analysis of a sample of the prewash




of the sampling train glassware indicated contamination of the glassware of




approximately the same magnitude as the amounts of formaldehyde measured at




the scrubber outlet.  There was also some formaldehyde in the blank ^0 sample.




The blank value was subtracted from the samples in accordance with the volume




of water used during sampling and wash up.
VISIBLE EMISSIONS FROM "A" GRANULATOR SCRUBBER STACK




     The opacity of the plume from "A" Granulator Scrubber stack ranged from 0




to 5 percent.  The six minute arithmetic averages are represented graphically in




Figure 2 and are summarized in Tables 12-14.  Most of the observations were made




from the synthesis tower with the trees as background because the plume was




white and the sky cloudy or completely overcast.   Some readings were made on




October 10, 1978 when the sun was shining and these were made using the






                                   -28-

-------
I
N3
    Q.
    O
     CD
     
-------
TABLE 12.  SIX MINUTE ARITHMETIC AVERAGES OF" OCTOBER 10, 1978
          OPACITY READINGS ON "A" GRANULATOR SCRUBBER STACK AT
          AGRICO CHEMICAL COMPANY IN BLYTHEVILLE, ARKANSAS
                                      Average Opacity
                  Time	for 6 Minutes

               11:15-11:20                   5
               11:21-11:26                   5
               11:27-11:32                   5
               11:33-11:38                   5
               11:39-11:44                   5
               11:45-11:50                   5
               11:51-11:56                   5
                              -30-

-------
TABLE 13.  SIX MINUTE ARITHMETIC AVERAGES OF-OCTOBER 11, 1978
           OPACITY READINGS ON "A" GRANULATOR SCRUBBER STACK AT
           AGRICO CHEMICAL COMPANY IN BLYTHEVILLE, ARKANSAS
Time
09:24-09:29
09:30-09:35
09:36-09:38*
09:47-09:52
09:53-09:58
09:59-10:04
10:05-10:10
10:11-10:16
10:17-10:22
10:23-10:28
10:29-10:34
10:35-10:40
10:41-10:44*

11:27-11:32
11:33-11:38
11:39-11:44
11:45-11:50
11:51-11:56
11:57-12:02
12:03-12:08
12:09-12:14
12:15-12:20
12:21-12:26
12:27-12:32
12:33-12:38
12:39-12:43*
13:43-13:48
13:49-13:54
13:55-14:00
14:01-14:06
14:07-14:12
14:13-14:18
Average Opacity
for 6 Minutes
5
5
5
5
5
5
5
5
5
5
3.3
0
0

3.7
3.9
2.9
4
2.5
3.3
1.8
3.4
4.2
4.7
4.3
4.8
5
5
5
4.2
5
3.9
4.5
Time
14:19-14:24
14:25-14:30
14:31-14:36
14:37-14:42
14:43-14:48
14:49-14:54
14:55-15:00
15:01-15.06
15:07-15:12
16:10-16:15
16:16-16:21
16:22-16:27
16:28-16:33
16:34-16:39
16:40-16:45
16:46-16:51
16:52-16:57
16:58-17:03
17:04-17:09
17:10-17:15
17:16-17:21
17:22-17:27
17:28-17:33
17:34-17:39
16:40-17:45
17:46-17:51
17:52-17:57
17:58-18.03
18:04-18:09
18:10-18:15
18:16-18:21
18:22-18:25*

Average Opacity
for 6 Minutes
5
5
4.5
2.5
3.2
0.8
0.9
3.2
4
5
4.6
5
1.8
3.7
1.1
.5
.3
0
0
0
0
0
.6
.5
0
.3
1.5
.7
.5
1.3
0.8
0.7

     *Averaging time less than 6 minutes.
                              -31-

-------
TABLE 14.  SIX MINUTE ARITHMETIC AVERAGES OF - OCTOBER 12, 1978
           OPACITY READINGS ON "A" GRANULATOR SCRUBBER STACK AT
           AGRICO CHEMICAL COMPANY IN BLYTHEVILLE, ARKANSAS
                                           Average Opacity
                  Time                      for 6 Minutes
14:45-14:50
14:51-14:56
14:57-15:02
15:03-15:08
15:09-15:14
15:15-15:20
15:21-15:26
15:27-15:30*
1.9
1.3
0.6
2
0
1.4
0
1.4
                    *Averaging time less than 6 minutes.
                              -32-

-------
synthesis tower as a dark background.  The detailed information on the visible


emission measurements can be found in Appendix C.





PARTICLE SIZING TESTS ON "A" GRANULATOR SCRUBBER


     Particle size distribution tests were conducted on the "A" Granulator


Scrubber Inlet (TP-1) and Outlet (TP-2).   Summaries of the results from the


inlet and outlet tests are presented in Table 15.    In a cascade impactor


the stage which the gas stream enters first has a  lower impaction velocity


then the subsequent stage.  As the impactor velocity increases, the size


cutoff of the particulate which will be collected  decreases.   The aerodynamic


size range is determined by the size cutoffs of stages n and  n+1 and cor-


responds to the mass of particulate collected on stage n+1.  In other words,


stage n collects particles greater than a particular size, stage n+1


collects particles greater than a second  particular size.   Therefore,


particles collected on stage n+1 are _ the size cutoff for stage n+1 and


the range of sizes of the particulate collected on stage n+1  is defined.


The size of the particulates entering the "A" Granulator Scrubber was 100%


>2.2 ym in that essentially all the particulate was collected in the


cyclone precollector.  Most of the particulate leaving the scrubber was


also collected in the cyclone precollector (average 77% of total mass


collected). The cumulation size distribution curves for outlet Runs 2 and


3 are depicted in Figure 3.  The curve in Figure 3 correspond to the per-

                                         <
centage of total mass collected which is  - a particular particle size


expressed in terms of aerodynamic diameter.  A straight line  on the log


probability graph paper would indicate a  normal distribution  of particulate.
                                  -33-

-------
             TABLE 15.   SUMMARY OF INLET AND OUTLET PARTICLE SIZING TEST RESULTS ON "A",
                        GRANULATOR SCRUBBER AT AGRICO CHEMICAL IN BLYTHEVILLE,  ARKANSAS2
TRC
Test
No.
1

2





3





4





5

6

Sampling
Location
Scrubber
Inlet
Scrubber
Outlet




Scrubber
Outlet




Scrubber
Outlet




Scrubber
Inlet
Scrubber
Inlet
Particulate
Test Test Concentration, Aerodynamic *
Date Time grains/dscf Size Range, urn
10/12/78 0919-0920 12.10 >2.2

10/12/78 1109-1509 0.0033 >3.7
2.7-3.7
1.7-2.7
1.0-1.7
0.56-1.0
<0.56
10/12/78 1629-2029 0.0044 >3%7
2.7-3.7
1.7-2.7
1.0-1.7
'0.56-1.0
<0.56
10/13/78 0855-1255 0.014 >3.Q
2.8-3.8
1.7-2.8
1.1-1.7
0.56-1.1
<0.56
10/13/78 1316-1317 32.67 >2.3

10/13/78 1508-1509 16.94 >2.4

Mass in
Size Range, %
100

98.7
0.00
0.14
0.21
0.39
0.39
89.35
0.00
7.32
1.31
1.05
0.97
65.34
0.00
4.54
0.67
23.89
5.56
100

100

The complete results can be found in Appendix B.

As unit density spheres

-------
100
 1Q
                   •
                   I
                                ^^

                                I
A— -
                                  «MRUN 2 (TRC TEST 3)
                              A— -ARUN 3 (TRC TEST 4)
LEGEND

 10/12/78, 1629 - 2029
 10/13/78, 0855 - 1255
  iL
                             I
                  10      20    30   40
                      PERCENTAGE OF MASS
                   50   60   70    80
                   CORRESPONDING SIZE
          90
98
          FIGURE 3:   CUMULATIVE SIZE DISTRIBUTIONS OF PARTICULATE IN THE "A"
                       GRANULATOR SCRUBBER STACK AT AGRICO CHEMICAL COMPANY
                       IN  BLYTHEVILLE, ARKANSAS
                                    -35-

-------
 It was not possible to plot cumulative size distribution curves for inlet




 Runs 1-3 (TRC Tests 1, 5, & 6) or outlet Run 1 (TRC Test 2) because more




 than 98% of the total mass was collected in the cyclone for these tests.




      It was necessary to run the impactors on the inlet at a sampling rate




 of approximately one cubic foot per minute to maintain Isokinetic sampling




 through the 3/16" nozzle.  A smaller nozzle was not used because of pro-




 blems of nozzle clogging during the urea and ammonia tests.  This high flow




 rate resulted in a smaller size cutoff for the cyclone than desired.   The




 high concentration of particulate at the scrubber inlet required a one minjute




 sampling duration.  The short sampling duration necessitated presetting the




 impactor flow.  Each inlet test was begun by turning the impactor nozzle into




 the flow stream and starting the pump.  Only minor adjustments were then




 required to maintain isokinetic flow.
PRESSURE DROP MEASUREMENTS ACROSS "A" GRANULATOR SCRUBBER




     The pressure drop measurements across the "A" Granulator Scrubber were made




with a vertical U tube water manometer which was connected to pressure taps at




the scrubber inlet and outlet.  The inlet pressure tap consisted of a stainless




steel tube inserted into the middle of the duct through the dilution air damper.




The tubing was fixed in place so that the open end was perpendicular to the




flow stream.  The outlet pressure tap consisted of a hole drilled through the




section of ducting between the scrubber outlet and the inlet to the fan.  The




pressure drop across the scrubber was recorded at approximately 15 minute in-




tervals during the tests for urea, ammonia and formaldehyde.  The pressure drop




was recorded at approximately 30 minute intervals for the particle sizing tests.




     The pressure drops across the "A" Granulator Scrubber ranged from 14.0 to




20.5 inches of vertical water column and are presented in Table 16.

-------
           TABLE 16.
    SUMMARY OF OCTOBER 10,  11,  12, 13, 1978 "A" GRANULATOR
    SCRUBBER PRESSURE DROP  MEASUREMENTS AT AGRICO CHEMICAL
    COMPANY IN BLYTHEVILLE, ARKANSAS
   Date
10/10/78
 10/10/78
 10/11/78
 10/11/78
 10/11/78
 10/11/78
Clqck
Time

1130
1145
1200
1215
1230
1245
1300
1315
1330
1345
1400
1415

1500
1515
1530
1545
1600
1615
1630
1700

1020
1035
1050
1115

1120
1140
1200
1220
1235

1340
1355
1420
1440
1455
1518
1615
1630
1645
1735
1800
AP, "H20

  18.25
  17.75
  17.25
  17.25
  17.25
  17.25
  17.25
  18.00
  18.75
  20.50
  18.00
  17.00

  16.25
  16.25
  16.25
  16.25
  16.25
  16.25
  16.25
  16.25

  15.50
  15.50
  15.50
  15.50

  15.00
  15.00
  15.00
  14.60
  14.60

  14.00
  14.00
  14.00
  14.00
  14.40
  14.20
  15.00
  15.50
  14.50
  14.00
  14.00

Date
10/12/78




Dilution









10/13/78















Clock
Time
0930
1100
1110
1130
1200
Damper Closed Down
1230
1300
1330
1420
1830
1900
1930
2000
2030
0820
0900
0915
0930
1000
1030
1100
1130
1140
1200
1230
1300
1330
1400
1430
1500

AP, "H?(
16.75
16.75
16.50
15.75
15.25
1 Notch
15.75
15.75
15.00
14.75
15.25
15.25
15.50
15.00
15.00
16.00
16.50
15.50
16.00
15.50
15.50
15.50
16.00
16.00
16.50
16.25
16.50
17.00
16.50
18.00
16.50
                                        -37-

-------
 UREA,  AMMONIA AND FORMALDEHYDE IN SCRUBBING LIQUOR ENTERING AND EXISTING "A"
 GRANULATOR SCRUBBER

     Samples(500 ml)  of the scrubbing liquor streams entering and leaving

 (after the pump) the "A" Granulator Scrubber were collected at approximately

 15 minute intervals during the urea and ammonia tests.   The solution temperature

 was measured  immediately after each sample was collected.   The pH of each sample

 was also measured.  The  individual  samples  were composited  into one inlet  and one

 outlet sample and the pH was measured.   The composited  samples were analyzed

 for urea, ammonia and formaldehyde.  Table 17 presents  a summary of the measured

 urea,  ammonia and formaldehyde concentrations in the scrubber liquor.   Table

 18 contains the pH and  temperature readings of each of  the individual  samples.

     The urea concentration for the inlet  ranged from 21,680 to 49,360 mg/£

 and averaged  36,590 mg/£.   The concentration for the outlet ranged from 506,

 200 to 1,012,000 mg/X, and averaged 689,400 mg/fc.

     The ammonia concentration for the inlet ranged from 7,420 to 22,780 mg/£.  .

 and averaged  13,900 mg/£.   The concentration for the outlet ranged from 1,350

 to 2,550 mg/Jl and averaged 1,800 mg/&.

     The formaldehyde concentration for the inlet ranged from 1.52 to  36.8

 mg/& and averaged 21.2  mg/£.   The concentration for the outlet averaged

 0.0275 mg/£.

     Assuming that the scrubber liquid flows into and out of the scrubber are

equal,  the results of the analysis of the scrubber liquids shows the average

urea concentration of the outlet solution to be 18.8 times the inlet solution

which would be expected because the urea is being scrubbed out of the gas stream

entering the scrubber.  The average ammonia concentration of the outlet solution
                                 -38-

-------
       TABLE 17.   SUMMARY  OF  OCTOBER 10 AND  11,  1978 UREA, AMMONIA AND FORMALDEHYDE MEASUREMENTS  ON THE
                      SCRUBBING LIQUOR ENTERING  AND  EXITING  "A"  GRANULATOR SCRUBBER AT AGRICO  CHEMICAL
                      COMPANY  IN  BLYTHEVILLE,  ARKANSAS
 1
                 Run Number (TRC Tost (lumber)          Run 1 (Teal 2)        Run 2 (Teat 3)          Run 3  (Test 7)           Average
                 Location                          Inlet     Outlet       Inlet.     Outlet       Inlet     Outlet     Inlet    Outlet
                 Date                            10/10/78    10/10/78    10/10/78   10/10/78     10/11/78    10/11/78
                 Urea Concentration, mii/l"           21.680     506,200     38,720    1,012,000    49,360     550,000    .U.,590    689,400
                 Ammonia Conccnl.r.it LUII. mg/1          7,420       1,350     22,780        2,550    11,510       1,500    13,900      1,800
                 Formaldehyde Concentration, mg/1     25.2         NDd       36.8         (ID       1.52       0.0275    2.1.2      0..0275
                 pllb                              9.90        8.90       10.1         8.90      9.95        0.6      NAe       NA
                 Temperature0, °c                    40          32       38          29        39         29       39        30
Co               Solids, ms/1                        -                               -                             Nl)f       NDf
                      inj illgriiuis p*T 1 Iter
                      pll ol compos I IK samp) e
                      average samp It* temperature's measured irotiit-d lately nf tPi. col] ret Ion
                      not detocto.l
                     °not nppl ir.-H.h-
                      from s.'tinpli's  roUcr.l.p
-------
   TABLE 18.  SUMMARY OF OCTOBER 10 AND 11, 19.78 pH AND
              TEMPERATURE MEASUREMENTS ON INDIVIDUAL SAMPLES
              OF SCRUBBING LIQUID ENTERING AND EXITING "A"
              GRANULATOR SCRUBBER AT AGRICO CHEMICAL COMPANY
              IN BLYTHEVILLE, ARKANSAS
Run No. Sampling
(TRC Test No.) Date Time
1 (2) 10/10/78 1135
1200
1215
1235
1310
1330
2 (3) 10/10/78 1455
1510
1525
1540
1600
1620
1650
3 (7) 10/11/78 1608
1620
1640
1650
1710
1720
1740
1800
1810
1825
Scrubber Inlet
Sample
pH °C
9.85
9.91
9.90
9.88
9.79a
9.92
10.05
10.10
10.10
10.10
10.10
10.08a
10.08
9.90
9.95
9.95
9.80
9.85
9.98
9.95
9.94
9.95
9.95
40
40
40
40
40
40
40
36
38
38
38
37
38
40
40
38
38
38
38
39
38
38
39
Scrubber Outlet
Sample
pH °C
8.90
8.90
8.91
8.90
8.84
8.95
8.90
8.90
8.95
8.85a
8.90
8.91
8.92
8.60
8.50
8.55
8.55
8.65
8.65
8.603
8.61
8.62
8.60
32
30
31
32
33
33
30
29
29
29
29
28
29
29
29
29
29
29
29
29
28
28
28
pH drifting.
                               -40-

-------
was 0.13 times the inlet solution which indicates that the ammonia is




being stripped from the scrubber liquor (the measurements on the inlet and




outlet gas streams indicated this — See Table 6).   The average formaldehyde




concentration of the outlet solution was 0.0013 times the inlet solution




which indicates that the formaldehyde was reacting with the urea since there




was no evidence of formaldehyde stripping by the measurements on the inlet




and outlet gas streams (see Table 7).   The lower pH measured in the scrubber




outlet solution is consistent with the lower ammonia concentration and the




lower temperature of the outlet solution is indicative of the dissolution




of urea into the scrubbing media, which is an endothermic reaction.









"A" GRANULATOR PROCESS SAMPLES UREA, AMMONIA, AND FORMALDEHYDE COMPOSITION




     Process samples were taken of the urea melt, the urea product before




screening, the urea product after screening and the formaldehyde additive.




The urea melt, product before screening and product after screening was




analyzed for urea, ammonia and formaldehyde.  The formaldehyde additive




sample is being retained for possible future analysis.  The results of the




analysis of the process samples are summarized in Table 19.









UREA AND AMMONIA TESTS ON SYNTHESIS TOWER MAIN VENT




     A summary of the urea and ammonia test results on the Synthesis Tower




Main Vent (TP-1) are presented in Table 20.  The average urea and ammonia




mass flow rates were 0.0713 and 1283.5 pounds per hour, respectively.
                                  -41-

-------
TABLE 19.  SUMMARY OF OCTOBER 11, 1978 UREA, AMMONIA AND
           FORMALDEHYDE MEASUREMENTS ON THE "A" GRANULATOR
           UREA MELT, PRODUCT BEFORE SCREEN AND PRODUCT AFTER
           SCREEN AT AGRICO CHEMICAL COMPANY IN BLYTHEVILLE,
           ARKANSAS

Date
Sampling Time
Urea Percent by Weight
Ammonia Percent by Weight
Formaldehyde Percent by Weight
Urea
Melt
10/11/78
1510
98.77
0.00
0.15
Urea Product
Before Screen
10/11/78
1850
93.98
0.00
0.50
Urea Product
After Screen
10/11/78
1850
100.0
0.00
0.23
                            -42-

-------
            TABLE 20.  SUMMARY OF RESULTS OR UREA AND AMMONIA TESTS ON OCTOBER 13, 1978
                       OF GASES IN THE SYNTHESIS TOWER VENT AT AGRICO CHEMICAL COMPANY,
                                       BLYTHEVILLE, ARKANSAS











I
1
.p-
U)




Run No. (TRC Test No.)
Date
Time
q
Volume of Gas Sampled-DSCF
% Moisture by Volume
Average Duct Temperature - F
Duct Volumetric
Flow Rate - DSCFM
Duct Volumetric
Flow Rate - ACFMC
Urea - Concentrations and Mass
Mg ,
gr/DSCF
lb/hre
Ammonia Concentrations and Mass
Mg
gr/DSCF
Ib/hr
1 (3)
10-13-78
•0930 to 0945
4.31
87.97
175

1248

12458
Flow Rates, Analysis
1.71
0.0061
0.065
Flow Rates, Analysis
32730
117.2
1253.6
2 (4)
10-13-78
1030 to 1446
4:41
88.37
185

1202

12631
3 (5)
10-13-78
1130 to 1145
4.70
90.56
185

,990.9

12802
Average


4.47
88.97
182

1147

12630
Procedure - Colorimetric
0.36
0.00126
0.13
Procedure - Direct
39310
137.5
1417.6
4.64
0 .0152
0.130
Nesslerization
40120
131.7
1179.3
2.24
0 .00752
0.0713

37390
128.8
1283.5
Dry standard cubic feet @ 68°F, 29.92 in. Hg. includes Air, Ammonia  and  'Inerts1.

Dry standard cubic feet per minute @ 68°F, 29.92 in. Hg.
Actual cubic feet per minute.

Grains per dry standard cubic foot @ 68°F, 29.92 in. Hg.

-------
     Five tests were conducted on the synthesis tower Main Vent, however,




the first two were not used because of evidence of ammonia passing through




the sampling system.  This problem was alleviated by the use of additional




impingers in the sampling train and by using ION H2SOi+.   The Sampling




and Analysis Methodologies Section 5 explains in detail the changes which




were made to the sampling train.
                                  -44-

-------
                               SECTION 3




                   PROCESS DESCRIPTION AND OPERATION






FACILITY DESCRIPTION:




    I.  PROCESS EQUIPMENT




        Urea is produced by reacting liquid ammonia (Nl^)  with carbon dioxide




(C02) at elevated temperature and pressure.  The reaction is exothermic and




spontaneous and results in formation of liquid ammonium carbamate (^H2 C02




    .  The liquid ammonium carbanate is subsequently decomposed to urea




           and water.  The resulting solution of urea in water is concentra-




ted to 98+ percent urea when it will be subsequently solidified.




        The Stamicarbon C02 Stripping Process is the urea synthesis method




employed at this facility.  There are three continuous vents and  one intermit-




tent vent from this process which have been combined into one tall stack.   The




continuous vents are:  medium pressure absorber, low pressure scrubber and the




flash tank condenser from the vacuum evaporators.  The intermittent vent is




from the carbamate condenser steam drum.   Approximately 25 percent of the time




50 psig steam from this steam drum is vented through the common stack because




it is not usable elsewhere in the plant.




        Liquid 70 percent urea leaving the solution production area goes to




a holding tank prior to being concentrated to 99.5 percent in a two-stage  vacuum




evaporator.




        The concentrated molten urea, referred to as melt,leaves  the solution




synthesis process and is pumped to the solids formation equipment.  This facility




employs rotary drum granulators, designed by C&I Girdler,  as the  solids forming




devices.
                                 -45-

-------
        The molten urea is sprayed onto a bed of solid urea "seed" particles

at the higher end of the inclined granulator.  Lifting flights arrayed inside

the granulator cause the solid urea "seed" particles to continually fall

through the molten sprays and a counter-current flow of cooling air.  The

molten urea solidifies on these "seed" particles, increasing their size.  As

the particles grow in size, they eventually spill over a retaining dam into

the cooling section of the granulator.

        Cooled granules leaving the rotary drum granulator are screened.  Over-

size granules are crushed, combined with undersize granules, and returned in

solid form to the bed of material at the spray end of the granulator as make-up

"seed".  Product size granules are conveyed to a bulk storage warehouse.

        This facility does not coat the product urea granules.  Instead, a

formaldehyde-based additive is added to the molten urea before it is sprayed

in the granulator.

        At this facility, emissions .result from various vents in the solution

synthesis process and from the granulator cooling air exhaust.  The solution

synthesis process vents are combined into one stack before exhausting to ambient.

The granulator cooling air passes through a scrubber and fan before being ex-

hausted out a stack.  Scrubber liquid is returned to the solution synthesis

process for urea recovery.

        This facility employs three parallel granulators, each with its own

screens, scrubber, fan, and stack, for solid production.  A single solution

synthesis process supplies all three granulators (Figure 4).

        Plant personnel provided a process drawing during the testing which

EPA was allowed to retain.  It is entitled:

                            Utility Flow Diagram
                            1000 ST D Urea Plant
                          Agrico Chemical Company
                           Blytheville, Arkansas
                                1320-1-50-15


                                 -46-

-------
SAMPLE
LOCATION
 STACK
NH-
CO,
                                                   SAMPLE
                                                  LOCATION
                                                                STACK
                    SCRUBBER LIQUOR
      SOLUTION
      SYNTHESIS
      PROCESS
ROTARY DRUM

      GRANULATOR*
COOLING  AIR
                                                                                 PRODUCT
                                                                               -+•  TO
                   ADDITIVE
                      TYPICAL  FOR EACH OF THREE LINES AT  PLANT
                                                                                 WAREHOUSE
         Figure 4    Urea Manufacturing, Agrico Chemical Co., Blytheville, Arkansas,

-------
    II.  EMISSIONS AND EMISSIONS CONTROL EQUIPMENT




         The Stamicarbon C0£ Stripping urea synthesis process at this plant




incorporates emission reduction and energy recovery techniques in its standard




design.




         The high and low pressure scrubbers at this facility are typically




employed in this process to reduce ammonia losses to the exhaust streams that




are necessary for inerts removal from the system.  The medium pressure absorber




is employed only in those instances when the overheads stream from the reactor




has a high enough hydrogen content to make total ammonia removal in the high




pressure scrubber unsafe.  The exhausts at this facility from the medium pres-




sure absorber and the low pressure scrubber should therefore contain very




little ammonia by design.  In addition, the process design should result in




practically no urea in these exhausts.




         The exhaust from the steam jet ejector vacuum system on the evaporators




should also contain mostly inerts, very little ammonia, and little urea by




design.  The procedure employed to condense the steam used in this system acts




as an emission reduction device.




         The steam drum in this process is employed as a heat recovery device.




It uses "dirty" process condensate to produce 50 psig steam for use in the




process when needed.  However, when not usable in the process this "dirty" steam




must be vented to atmosphere.  Because the production of this steam is an inte-




gral heat removal step in the overall process, its production cannot be ceased




when there is no  demand.  When vented, this steam can be expected to contain




approximately 100 ppm of ammonia and carbon dioxide and traces of urea.




         This plant has combined the above four exhausts into a single tall




stack before release to the atmosphere.
                                 -48-

-------
         The granulators employed at this plant for solids production are




typically controlled by scrubbers.   These scrubbers must be used on the granu-




lators to reduce the product losses resulting from the cooling air passing




through the granulator.  This airstream entrains significant quantities of urea




as it passes through the granulator and, if exhausted untreated, would signi-




ficantly effect the economic viability of this solids production technique.




The Joy Turbulaire "Type D" impingement scrubbers normally employed can be




operated at varied pressure drops by adjusting scrubber liquid level.  This




plant maintains a pressure drop in excess of 14 in. W.G. to satisfy particulate




emission limitations.  Cleaned process condensate from the urea synthesis




operation is used as make-up scrubber liquid.  Specific gravity is monitored




to maintain the liquor at 45 to 50 percent urea in the scrubber.  Liquor blow-




down is returned to the synthesis operation for urea recovery.  The designers




of the granulation process guarantee emissions of urea particulate to no more




than 10 Ib/hr from the scrubber exhaust.  Some ammonia can be expected in the




additive into the urea melt before solidification, formaldehyde may also be




present.





FACILITY OPERATION DURING TESTING;




    GCA monitored and recorded process and control equipment operating para-




meters during sampling of the solution and granulation processes by TRC to




ensure that samples were collected only during representative, steady-state




process operation.




    Table  21  presents a list of 30 parameters monitored during testing.  The




raw data are presented in Appendix J of this report along with summaries of




the parameter values.




    Table  22  presents a summary of the test runs conducted by TRC, indicating




the date and times of testing, the time period over which the process and control
                                 -49-

-------
           TABLE 21.  PARAMETERS MONITORED DURING TESTING AT AGRICO CHEMICAL COMPANY IN BLYTHEVILLE,  ARKANSAS


Item No.


1

2

3




5

6

Parameter
Urea Solution
Feed Tank
Level
Additive
Feed Rate
Urea Melt
Temperature

"A" Granulator
Spray Pressure
"B" Granulator
Spray Pressure
"C" Granulator
Spray Pressure

Indication
of:
•
PR, PS*

PS,E*


PS,E*


PR, PS*
PR, PS*

PR, PS*

Appendix
Column
Heading

TK-101

APR


UMT


GSP-A
GSP-B

GSP-C


Conversion
factor



Reading x 100
(approx. )
~
None


None
None

None


Units



///HR

A°F from
design
valve

psig
psig

psig


Comments

See Note 1



Design value is
confidential








O
                                                     (continued)

-------
                                                  TABLE 21  (continued).

Item No.
7
a
9
10
11
12
Parameter
"A" Granulator
Inlet Air
Temperature
"A" Cranulator
Outlet Air
Temperature
Temperature of
Urea Solids
Exiting
"A" Granulator
"A" Granulator
Scrubber
Liquor Level .
"A" Granulator
Scrubber Fan
Amperage
"A" Granulator
Drive Motor
Amperage
Indication
of:
PS*
PS*
PS*
SO,E*
SO*
PS*
Appendix
Column
Heading
AIGT
AOGT
UST
SLL
SFA
GMA

Conversion
factor
None
None
None
None
None
None
Units
A°F from
standard
valve
A°F from
standard
valve
oF
% of total
gauge
Amps
A amps
from
standard
valve
Comments
Standard value
arbitrarily chosen to
protect confidential-
ity of this parameter
Same as Above
See Note 2
See Note 3
Non-recording
dial instrument
Standard value
arbitrarily chosen to
protect confidential-
ity of this parameter

I
Ul
                                                    (continued)

-------
TABLE 21  (continued)

Item No.
13
14
15
16
17
18
Parameter
Weight of Total
Solids Leaving
"A" Granulator
Product Weight
to Warehouse
"A" Granulator
Total Outlet
Solids Weight
"B" Granulator
Total Outlet
Solids Weight
"C" Granulator
Total Outlet
Solids Weight
"A" Granulator
Product Weight
Indication
of:
PR, PS*
PR, PS*
PR, PS*
PR, PS*
PR, PS*
PR, PS*
Appendix
Column
Heading
TWOD
PWTW
SOWT-A
SOWT-B
SOWT-C
PWTA
Conversion
factor
Reading x
1230
Reading x
358.8
Reading x
0.05
Reading x
0.05
Reading x
0.05
Reading x
0.05
Units
///HR
///HR
tons
tons
tons
tons
Comments
Weigh belt indicator
Weigh belt
indication - sum of
three granulators
Totalizer for TWOD
above
Totalizer
Totalizer
Totalizer for weigh
belt on product
leaving screens

   (continued)

-------
                                                 TABLE 21  (continued)

Item No.
19
20
21
22
23
24
Parameter
"B" Granulator
Product Weight
"C" Granulator
Product Weight
"A" Granulator
Scrubber
Liquor
Temperature
"A" Granulator
Scrubber
Liquor
Feed Rate
"A" Granulator
Scrubber Exit
Air
Temperature
C02 Feed Rate
Urea
Synthesis
Process
Indication
of:
PR, PS*
PR, PS*
SO,E*
SO,E*
SO*
PR, PS*
Appendix
Column
Heading
PWTB
PWTC
SLT
ISLF
AOS
C02 Feed
Conversion
factor
Reading x
0.05
Reading x
0.05
None
None
None
Reading x
80,000
Units
tons
tons
op
gpm
OF
SCFH
Comments
Totalizer for weigh
belt on product
leaving screens
Totalizer for weigh
belt on product
leaving screens
Dial thermometer
at scrubber
Dial instrument at
scrubber liquor ;
feed line
Dial thermometer at
scrubber outlet
duct
See Note 4
r
I
Ul
                                                   (continued)

-------
                                                   TABLE  21   (continued)

Item No.
25
26
27
28
29
30
Parameter
"Dirty" Steam
Exhaust Flow
late from Urea
Synthesis
"Dirty" Steam
Sxhaust Valve
Vctuator and
\ Valve Open
TH3 Feed Rate
to Urea
Synthesis
Jrocess
/acuum on
No. 1
Evaporator
Vacuum on
No. 2
Evaporator
Temperature of
Circulating H20
to Top of Low
Pressure Scrubb
Indication
of:
E*
PS*
PR, PS*
PS,E*
PS,E*
PS,E*
jr
Appendix
Column
Heading
DSEF
DSEP/
valve
ccnd.
NH3 Feed
EV-1
EV-2
TI 16
Conversion
factor
Reading x
5,000
See Note 5
Reading *
12.4
None
None
None
Units
///HR
See Note 5
% of Urea
Process
Design
Capacity
mm Hg
vacuum
mm Hg
vacuum
OF
Comments
Strip Chart

Design capacity is
1000TPD of 100% Urea



•P-
                                                       (continued)

-------
                                              TABLE  21  (concluded).
Ln
I
        NOTES

          1.
          2.
          3.
          5.
This tank is located before the concentrators.  In addition to the liquid level in the
tank, the concentration is necessary for determination of production rate.  However, the
liquid level alone indicates increase or decrease in production rate.

Inspection of the sensing device indicated that it was not in intimate contact with the
urea solids and was, therefore, not indicating actual solids temperature.

Scrubber liquid level is controlled by an overflow weir. ,The weir is set when the scrub-
is not operating.  Once the scrubber is operating, the liquid level indicator is used as
a gross indication of scrubber liquor feed pump operation.(i.e.,' level will fall if pump
fails).

The meter conversion factor of 80,000 applies for C02 at 257°F and 2100 psig which are
conditions applicable to the discharge stream of compressors at this plant.

These valves are monitored by plant personnel as an additional indication of the amount
of "dirty" steam being vented.  "Dirty" steam is at 295.9°F and 48 psig.
        *KEY

         PR:  Process Rate

         PS:  Process Stability

         E:   Emission Fluctuation

         SO:  Scrubber Operation

-------
TABLE 22.   SUMMARY OF TESTING AT AGRICO CHEMICAL COMPANY IN.BLYTHEVILLE,  ARKANSAS
Test type
Urea parciculace
Run 1
Urea parciculace
Run 2
Urea parciculace
Run 3
Formaldehyde
Run 1
Formaldehyde
Run 2
Formaldehyde
Run 3
Parcicle size
Run 1
Parcicle size
Run 2
Particle size
Run 3
Urea synched* cover
Run 1
Urea synthesis cover
Run 2
Urea synthesis cover
Run 3

Inlec
Ouclec
Inlec
Ouclec
Inlec
Ouclec
Inlec
Ouclec
Inlec
Ouclec
Inlec
Ouclec
Inlec
Ouclec
Inlec
Ouclec
Inlec
Ouclec
Outlet
Ouclec
Ouclec
Dace
10/10/78
10/10/78
10/10/78
10/10/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/12/78
10/12/78
10/13/78
10/12/78
10/13/78
10/13/78
10/13/78
10/13/78
10/13/78
Sampling
period
1130
1131
1500
1531
1616
1616
0920
0918
1120
1129
1335
1348
0919
1109
1316
1629
1508
0855
0930
1030
1130
CO
CO
CO
CO
to
to
to
CO
CO
co
co
co
CO
co
CO
CO
CO
CO
CO
CO
CO
1415
1336
1700
1737
1832
1832
1040
1028
1242
1237
1516
1515
0920
1509
1317
2029
1509
1255
094 5
1046
1145
Process No. of daca
paraaecer points in
averaging averaging
period period
1130
1130
1500
1530
1620
1620
0920
0920
1120
1130
1325
1345
0915
1059
1300
1630
1500
0915
0921
0955
1125
CO
CO
CO
co
CO
CO
co
CO
co
co
CO
CO
co
CO
CO
CO
CO
CO
to
CO
CO
1410
1340
1700
1730
1820
1820
1030
1030
1240
1240
1515
1515
0932
1500
1325
2030
1515
1300
0945
1057
1143
17
14
13
13
13
13
8
8
9
8
11
9
2
9
2
9
2
9
2
2
2
Tesc
designation
UP-l-I
UP-1-0.
UP-2-I
UP-2-0
UP-3-I
UP-3-0
F-l-I
F-l-0
F-2-I
F-2-0
F-3-I
F-3-0
PS-l-I
PS-1-0
PS-2-I
PS-2-0
PS-3-I
PS-3-0
ST-l-0
ST-2-0
ST-3-0
                                 -56-

-------
equipment parameters were averaged, and assignment of test designations.




    Table  23  is a summary of the data monitored and indicates the variations




of the parameters during each of the test runs.  The columns titled "Maximum




Value % Deviation" and "Minimum Value % Deviation" present the difference




between the highest and lowest values observed and the average value of the




parameter for that, run, expressed as a percent of the average value.




    Table 24  presents the variation of the average value of each parameter




between tests as a percent deviation from the overall average of that parameter




for all test runs of the designation.




    The average values of each parameter are presented in Appendix J.





    I.  GRANULATOR PARAMETERS MONITORED




        Of the 30 parameters monitored, items 1 through 9 and 12 through 20




in Table  21  were recorded specifically as indicators of the granulator pro-




duction rate, process stability, and  possible, emission fluctuation during




testing.  The third column of Table  21  designates what each parameter indicates.




        In addition to the instrument data recorded by GCA, TRC collected samples




from various portions of the granulation facility, whose analysis should aid




in characterizing the process operation.  These samples include:  a grab sample




of the molten urea feed to the granular for analysis of temperature, -pH, percent




urea, percent ammonia, and percent formaldehyde; a grab sample of the product




leaving the granular for analysis of temperature, moisture, percent urea,




percent ammonia, and percent formaldehyde; a second grab sample of the product




leaving the granulator for sieve size analysis, and; a grab sample of the




additive retained for future analysis.




        As indicated by the data in Tables  23 and  24 .  the granulator ran




quite steady during each test run and showed little variation when parameters




are compared between runs.
                                 -57-

-------
      TABLE  23.  PARAMETER DEVIATIONS DURING TESTING AT AGRICO
                CHEMICAL COMPANY IN BLYTHEVILLE, ARKANSAS
                  TEST DESIGNATION UP-l-I   'DATE 10/10/78   TIME  1130 TO 1410




1
Ul
oo
1

Process
parameter
Urea 70% solution
tank level
Additive feed
rate
Urea melt
temperature

Appendix
code
TK-101

AFR

UMT

Units
% of tank

Ib/hr

A°F from
design
value

Standard
deviation
0.33

9.93

-3.5°F5

Maximum
value
% deviation
1.0%

2.9%

-5°F6

Minimum
value
% deviation
0.9%

2.4%

-1°F6
"A" Granulator spray
  nozzle pressure

"B" Granulator spray
  nozzle pressure
GSP-A    psig
GSP-B    psig
1.18
1.98
2.7%
3.'
 8.5%
13.6%
"C" Granulator spray GSP-C
nozzle pressure
"A" Granulator inlet AIGT
air temperature
"A" Granulator outlet AOGT
air temperature
psig
A°F from
standard
r\
value
A°F from
standard
value2
1.72 2.9%
+0.5°F5 +3°F6

+8.8°F5 +15°F6

12.0%
-1°F6

+2°F6


                                    (continued)

-------
TABLE 23    (continued).

Process
parameter
Liquid level in
"A" granulator
scrubber
"A" Granulator
scrubber
fan amps
"A" Granulator
drive
motor amps
Liquor temperature
in "A" granulator
scrubber
Liquor feed rate to
"A" granulator
scrubber
"A" Granulator
scrubber
exit air
temperature
Production rate of
urea synthesis
process
.. „ , . .Maximum Minimum
Appendix ,. . Standard , ,
vv , Units , . . value value
code deviation „ . „. .
/» deviation /« deviation
SLL N.A.3 0.08 2.8% 2.5%
SFA amps 1.5 3.6% 3.6%

GMA A amps +2.7 amps5 +6 amps6 0 amps6
from
standard
value2
SLT °F 0.59 0.6% 1.1%
ISLF gpm 0.24 0.3% 4.7%
AOS °F 0.64 1.4% 1.0%



NH3 ton/day of
feed 99.5% urea (Parameter not recorded during this test)
solution

       (continued)

-------
           TABLE 23   (continued). TEST  DESIGNATION   UP-1-0  DATE  10/10/78  TIME 1130  TO  1340
 i
s
Process
parameter
Urea 70% solution
tank level
Additive feed
rate
Urea melt
temperature
"A" Granulator
spray nozzle
pressure
"B" Granulator
spray nozzle
pressure
"C" Granulator
spray nozzle
pressure
"A" Granulator inlet
air temperature
"A" Granulator outlet
air temperature
Appendix
code
TK-101

AFR

UMT

GSP-A

GSP-B

GSP-C

AIGT

AOGT

Units
% of tank

Ib/hr

A°F from
design
value
psig

psig

psig

A°F from
standard
value2
A°F from
standard
value2
„ . , Maximum
Standard ,
j • „• value
deviation « , .
% deviation
0.32 1.0%

8.70 2.4%

-3 ,7°F5 -5°F6

1.24 1.9%

2.08 4.6%

1.83 3.4%

+0.6°F5 +3°F6

+7.9°F5 +14°F6

Minimum
value
% deviation
0.8%

2.1%

-3°F6

8.2%

13.1%

11.6%

-0 . 5°F6

+2°F6


                                                    (continued)

-------
TABLE 23   (continued).

Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator SFA
scrubber
fan amps
"A" Granulator drive GMA
motor amps
Liquor temperature in SLT
"A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator scrubber AOS
exit air temperature
Production rate of NHa
urea synthesis feed
process
„ . , Maximum Minimum
., . Standard , ,
Units , . . value value
deviation «... ./ .
/» deviation % deviation
N.A.3 0.07 3.6% 1.8%
amps 1.40 3.4% 2.3%

A amps +2.6 amps5 +6 amps6 0 amps6
from
standard
r\
value
°F 0.59 0.5% 1.2%
gpm 0 0 0
°F 0.59 1.3% 1.0%

ton/day of
99.5% urea (Parameter not recorded during this test)
solution

      (continued)

-------
K>
I
          TABLE  23   (continued),. TEST DESIGNATION  UP-2-I   DATE 10/10/78   TIME  1500 TO  1700
Process
parameter
Urea 70% solution
tank level
Additive feed
rate
Urea melt
temperature
"A" Granulator spray
nozzle pressure
"B" Granulator spray
nozzle pressure
"C" Granulator spray
nozzle pressure
"A" Granulator inlet
air temperature
"A" Granulator outlet
air temperature
Appendix
code
TK-101

AFR

UMT

GSP-A
GSP-B
GSP-C
AIGT
AOGT

Units
% of tank

Ib/hr

A°F from
design
value
psig
psig
psig
A°F from
standard
value2
A°F from
standard
r\
value
Standard
deviation
0.88

12.79

-4.2°F5

0.63
1.11
0.89
-0.08°F5
i
+4.2°F5

Maximum
value
% deviation
2.1%

3.5%

-6°F6

2.1%
4.1%
3.0%
+2.5°F6
+10°F6

Minimum
value
% deviation
2.6%

3.3%

_2oF6

2.9%
6.0%
4.5%
-1.5°F6
0°F6


                                                  (continued)

-------
TABLE  23   (continued).
Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator scrubber SFA
fan amps
"A" Granulator drive GMA
motor amps
Liquor temperature SLT
in "A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of Nils
urea synthesis feed
process
Units
N.A.3
amps
A amps
from
standard
r\
value
oF
gpm
°F


ton/day of
99.5% urea
solution
„ . . Maximum Minimum
Standard , 1
value value
deviation „/ , • • «/ . •
% deviation /•> deviation
0.07 1.8% 3.5%
1.01 2.2% 2.2%
+3.1 amps5 +5 amps6 0 amps6
0.30 0.8% 0.3%
0.49 3.1% 2.1%
0.27 1.1% 0.1%


(Parameter 'not recorded during this test)

        (continued)

-------
TABLE 23 (continued). TEST DESIGNATION  UP-2-0  DATE  10/10/78  TIME  1530   TO  1730

Process
parameter
Urea 70% solution
tank level
Additive feed
rate
Urea melt
temperature
"A" Granulator spray
nozzle pressure
"B" Granulator spray
nozzle pressure
"C" Granulator spray
nozzle pressure
"A" Granulator inlet
air temperature
"A" Granulator outlet
air temperature
Appendix
code
TK-101

APR

UMT

GSP-A
GSP-B
GSP-C
AIGT

AOGT

Units
% of tank

Ib/hr

A°F from
design
value1
psig
psig
psig
A°F from
standard
value2
A°F from
standard
value2
Standard
deviation
0.91

13.94

-3.8°F5

0.58
0.99
0.79
-0.08°F5

+4.77°F5

Maximum
value
% deviation
3.4%

3.3%

-6°F6

2.3%
4.7%
3.5%
+2.5°F6

+10°F6

Minimum
value
% deviation
2.3%

3.5%

-2°F6

2.7%
5.5%
4.1%
-1.5°F6

+ 2°F6


                                         (continued)

-------
                                           TABLE  23     (continued).
Ul

Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator < SFA
scrubber
fan amps
"A" Granulator drive GMA
motor amps
Liquor temperature SLT
in "A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of NH3
urea synthesis feed
process '
Units
N.A.3
amps

A amps
from
standard
value2
°F
gpm
oF


ton/day of
99.5%
urea
solution
„ , , Maximum Minimum
Standard . ,
. . . value value
deviation <•/,•• °, .
fo deviation /<• deviation
0.07 1.8% 3.5%
1.00 2.0% 2.3%

+3.1 amps5 +6 arapse 0 amps6
0.30 0.8% 0.3%
0.36 4.2% 1.0%
00 0


(Parameter not recorded during this test)

                                                    (continued)

-------
                                       UP-3-I and
TABLE 23 (continued). TEST DESIGNATION  UP-3-0   DATE  10/11/78   TIME 1620   TO  1820

Process
parameter
Urea 70% solution
tank level
Additive feed
rate
Urea melt
temperature
i
i ,, ,,
Appendix
code
TK-101
APR
UMT
. nCTt A
Units
% of tank
Ib/hr
A°F from
design
value
.
Standard
deviation
0.58
14.87
-4.2°F5
n ia
Maximum
value
% deviation
5.6%
3.2%
-7°F6
i f.v
Min imum
value
% deviation
5.3%
4.8%
-1°F6
0 (.'/
          	—  f ~ J
     nozzle pressure

   "B" Granulator spray
     nozzle pressure
                          GSP-A    psig
GSP-B    psig
0.69
2.2%
4.1%
"C" Granulator spray GSP-C
nozzle pressure
"A" Granulator inlet AIGT
air temperature
"A" Granulator outlet AOGT
air temperature
psig
A°F from
standard
value^
A°F from
standard
r\
value
0.57 2.5% 3.4%
+9.1°F5 +11°F^ +7°F6

+5.0°F5 +9°F6 0°F6


                                        (continued)

-------
TABLE 23    (continued).

Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator SFA
scrubber
fan amps
"A" Granulator drive GMA
motor amps


Liquor temperature SLT
in "A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of NH3
urea synthesis feed
process
Units
N.A.3


amps


A amps
from
standard
value2
OF


gpm
•

Op


ton/day of
99.5% urea
solution
„ , , Maximum Minimum
Standard , ,
. . . value value
deviation „ . «,, .
/• deviation /•> deviation
0.04 0.4% 12.0%

•
0.83 2.7% 1.54%


+2.7 amps5 +6 amps6 0 amps6



0.31 0.8% 0.3%


00 0


0.63 1.7% 0.6%


6.99 1.0% 1.3%



      (continued)

-------
                                      F-l-I  and
TABLE 23 (continued).  TEST DESIGNATION F-l-0     DAT£  10/11/78   TIM£ 0920  T0  1030

Process
parameter
Urea 70% solution
tank level
Additive feed
rate
Urea melt
temperature

i
oo "A" Granulator spray
nozzle pressure
"B" Granulator spray
nozzle pressure
"C" Granulacor spray
nozzle pressure
"A" Granulator inlet
air temperature

"A" Granulator outlet
air temperature

Appendix „ .
rr . Units
code
TK-101 % of tank

APR Ib/hr

UMT A°F from
design
value

GSP-A psig

GSP-B 'psig

GSP-C psig

AIGT A°F from
standard
, n
value
AOGT A°F from
standard
value
Standard
deviation
0.85

7.04

-3.5°F5



0.30

0.35

0.35

•H.75°F5


+0.38°F5


Maximum
value
% deviation
6.1%

1.9%

-4°F6



1.1%

1.3%

1.2%

+3.5°F6


+2°F6


Minimum
value
% deviation
4.5%

2.0%

_30F6



1.4%

1.3%

1.2%

0°F6


_2°F6



                                        (continued)

-------
                                             TABLE  23  (continued).
>£>
I

Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator SFA
scrubber
fan amps
"A" Granulator drive GMA
motor amps


Liquor temperature in SLT
"A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of NHa
urea synthesis feed
process1*
UnU,
N.A.3


amps


A amps
from
standard
f\
value
°F


gpm


°F


ton/day of
99.5% urea
solution
c . , Maximum Minimum
Standard . , ,
. . . value value
deviation <./,-• »/ .
% deviation /» deviation
0.03 0 1.8%


0.93 2.7% . 1.5%


+2.0 amps5 +5 amps6 0 amps6



0.25 0.2% 0.3%


0.33 0.5% 4.3%


00 0


9.42 1.1% 1.1%



                                                 (continued)

-------
         TABLE 23  (continued).  TEST DESIGNATION  F-2-I   DATE  10/11/78  TIME  1120  TO 1240
o

Process Appendix
parameter code
Urea 70% solution TK-101
tank level
Additive feed rate AFR
Urea melt UMT
temperature
"A" Granulator spray GSP-A
nozzle pressure
"B" Granulator spray GSP-B
nozzle pressure
"C" Granulator .spray GSP-C
nozzle pressure
"A" Granulator inlet AIGT
air temperature
"A" Granulator outlet AOGT
air temperature
. , Maximum Minimum
„ . Standard . .
Units , . . value value
deviation «... «/ ,
, % deviation % deviation
% of tank- 1.18 . 7.7% 7.7%
Ib/hr 10.48 1.7% 3.0%
A°F from -4.1°F5 -5°F6 -2°F6
design
value
psig 0.34 0.7% 1.8%
psig 0.58 1.7% 2.2%
psig 0.62 1.2% 3.5%
A°F from +5.11°F5 +7.5°F6 +3.0°F6
standard
value2
A°F from +1.67°F5 +7.0°F6 -1°F6
standard
value2

                                                 (continued)

-------
TABLE  23  (continued).
.
Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator scrubberSFA
fan amps
"A" Granulator drive GMA
motor amps
Liquor temperature in SLT
"A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of NHa
urea synthesis feed
process
Units
N.A.3
amps
A amps
from
standard
value^
°F
gpm
OF


ton/day of
99.5% urea
solution
„ , , Maximum Minimum
Standard , .
. . . value value
deviation „, , ., ,
% deviation /» deviation
0.08 . 1.8% 3.5%
0.94 2.9% 1.4%
+2.8 amps5 +5 amps6 0 amps6
0.50 0.4% 1.2%
00 0
0.50 0.5% 0.7%


4.11 0.3% 0.8%

-------
TABLE 23 (continued).  TEST  DESIGNATION   F-2-0    DATE 10/11/78   TIME  1130 TO 1140

Process
parameter
Urea 70% solution
tank level
Additive feed rate
Urea melt
temperature
i
to "A" Granulator spray
nozzle pressure
"B" Granulator spray
nozzle pressure
"C" Granulator spray
nozzle pressure
"A" Granulator inlet
air temperature
"A" Granulator outlet
air temperature
Appendix
code
TK-101

APR
UMT

GSP-A
GSP-B
GSP-C
AIGT

AOGT

Units
% of tank

Ib/hr
A°F from
design
value1
psig
psig
psig
A°F from
standard
value2
A°F from
standard
value2
Standard
deviation
1.12

10.61
-4.0°F5

0.35
0.56
0.63
+5.63°F5

+ 1°F5

Maximum
value
% deviation
8.8%

1.6%
-5°F6

0.8%
1.9%
1.3%
+7.5°F6

+4°F6

Minimum
value
% deviation
6.8%

3.1%
_2°F6

1.7%
1.9%
3.4%
+3.5°F6

-1°F6


                                          (continued)

-------
                                             TABLE   23  (continued).
to

Process . Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator SFA
scrubber
fan amps
"A" Granulator drive GMA
motor amps

Liquor temperature SLT
in "A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of NH3
urea synthesis. feed
.process1*
Units
N.A.3
amps

A amps
from
standard
value2
•»
oF
gpm
oF


ton/day of
99.5% urea
solution
0 , . Maximum Minimum
Standard . ,
. . . value value
deviation „ . „, ,
/i deviation /» deviation
0.03 1.8% 0%
0.66 1.7% 1.1%

+2.6 amps +5 amps 0 amps6

0.35 0.3% 0.8%
00 0
0.48 0.5% 0.7%


4.24 0.3% 0.8%

                                                   (continued)

-------
TABLE 23 (continued). TEST DESIGNATION  F-3-I   DATE  10/11/78  TIME  1325  TO 1515

Process Appendix
parameter code
Urea 70% solution TK-101
tank level
Additive feed AFR
rate
Urea melt UMT
temperature
"A" Granulator spray GSP-A
nozzle pressure
"B" Granulator spray GSP-B
nozzle pressure
"C" Granulator spray GSP-C
nozzle pressure
"A" Granulator inlet AIGT
air temperature
"A" Granulator outlet AOGT
air temperature
Units
% of tank
Ib/hr
A°F from
design
value1
psig
psig
psig
A°F from
standard
f\
value
A°F from
standard
value2
Standard
deviation
1.14
5.14
-4.1°F5
0.26
0.33
0.31
+7.8°F5
+8.5°F5
Maximum
value
% deviation
14.6%
0.6%
-7°F6
1.1%
1.1%
1.1%
+9.5°F6
+20°F6
Min imura
value
% deviation
11.6%
1.7%
-3°F6
1.3%
1.3%
1.6%
+5°F6
0°F6

                                        (continued)

-------
                                         TABLE  23   (continued).
Ul
I

Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator scrubber SFA
fan amps
"A" Granulator drive GMA
motor amps


Liquor temperature SLT
in "A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit, air temperature
Production rate of NH3
urea synthesis feed
i,
process
„ . , Maximum Minimum
„ . Standard , ,
Units , . . value value
deviation v , . . « ,
7, deviation /•> deviation
N.A,3 • 0=09 3,5% 1.8%
.

amps 1.07 2.0% 2.3%
•
A amps +3.2 amps +5 amps6 +1 amps**
from
standard
value2
°F 0.39 0.8% 0.9%


gpm 0.94 5.8% 3.8%


°F 0.50 0.6% 0.6%


ton/day of 8.00 1.7% 1.1%
99.5% urea
solution

                                                (continued)

-------
TABLE 23 (continued).TEST DESIGNATION F-3-0    DATE  10/11/78  TIME  1345 TO 1515

Process Appendix
parameter code
Urea 70% solution TK-101
tank level
Additive feed rate AFR
Urea melt UMT
temperature
"A" Granulator spray GSP-A
nozzle pressure
"B" Granulator spray GSP-B
nozzle pressure
"C" Granulator spray GSP-C
nozzle pressure
"A" Granulator inlet AIGT
air temperature
"A" Granulator outlet AOGT
air temperature
Units
% of tank
Ib/hr
A°F from
design
value
psig
psig
psig
A°F from
standard
value2
A°F from
standard
value2
0 j , Maximum Minimum
Standard . .
. . . value value
deviation «/ , • • «/ ,
A deviation /•> deviation
0.84 10.8% 9.3%
5.50 0.6% 1.7%
-4.2°F5 -7°F6 -3°F6
0.28 1.1% 1.4%
0.37 1.1% 1.3%
0.33 0.8% 1.6%
+8.1°F5 +9.5°F6 +6°F6
-i-7.20F5 +20°F6 0°F6
                                        (continued)

-------
TABLE  23    (continued).

Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator scrubber SFA
fan amps
"A" Granulator drive GMA
motor amps
Liquor temperature in SLT
"A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of NHa
urea synthesis feed
process1*
„ , . Maximum Minimum
„ . Standard , ,
Units . . . value value
deviation „, . « ,
% deviation "> deviation
N.A.3 0.09 3,5% 1.8%
amps 1.17 2.0% 2.3%
A amps +3.4 amps5 +5 amps6 + 1 amps6
from
standard
value2
°F 0.28 0.6% 0.4%
gpm 0.94 4.8% 4.8%
°F 0.50 0.7% 0.4%


ton/day of 5.19 0.8% 0.9%
99.5% urea
solution

       (continued)

-------
          TABLE 23 (continued).  TEST DESIGNATION  PS-l-I   DATE  10/12/78  TIME  0915  TO 0932
03
I

Process
parameter
Urea 70% solution
tank level
Additive feed rate
Urea melt
temperature
"A" Granulator spray
nozzle pressure
"B" Granulator spray
nozzle pressure
"C" Granulator spray
nozzle pressure
"A" Granulator inlet
air temperature
"A" Granulator outlet
air temperature
Appendix „ .
vv . Units
code
TK-101 % of tank

APR Ib/hr
UMT A°F from
design
value1
GSP-A psig
GSP-B psig
GSP-C psig
AIGT A°F from
standard
f\
value
AOGT A°F from
standard
f\
value
„ , , Maximum
Standard ,
, . . value
deviation v , .
% deviation
0.25 1.5%

40.0 6.6%
-4.0°F5 -5°Fb . _

0 0
(Not operating during this
0 0
+8.0°F5 +9°F6

+8.5°F5 +16°F6

Minimum
value
% deviation
1.5%

6.6%
_30F6

0
test)
0
+7°F6

-fl°F6


                                                   (continued)

-------
TABLE  23  (continued).
Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator SFA
scrubber
fan amps
"A" Granulator drive GMA
motor amps
Liquor temperature in SLT
"A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of NH3
urea synthesis feed
process*4
Units
N.A.3
amps

A amps
from
standard
r\
value
OF
gpm
OF


ton/day of
99.5% urea
solution
_ , . Maximum Minimum
Standard value valug
devxation % deviation % deviation
00 0
0.5 0.7% 0.7%

+2 amps5 +2 amps6 +2 amps6
00 0
00 0
00 0


0 0 0

     (continued)

-------
          TABLE 23 (continued). TEST DESIGNATION  PS-1-0   DATE  10/12/78   TIME  1059 TO 1500
i
oo
o

Process
parameter
Urea 70% solution
tank level
Additive feed rate
Urea melt
temperature
"A" Granulator spray
nozzle pressure
"fi" Granulator spray
nozzle pressure
"C" Granulator spray
nozzle pressure
"A" Granulator inlet
air temperature
"A" Granulator outlet
air temperature
Appendix
code
TK-101
APR
UMT
GSP-A
GSP-B
GSP-C
AIGT
AOGT
Units
% of tank
Ib/hr
A°F from
design
value1
psig
psig
psig
A°F from
standard
f\
value
A°F from
standard
value2
„ , , Maximum
Standard ,
, . . value
deviation ./ . • • «/
A deviation /*
N.V.* N.V.*
58.21 13.6%
-5.3°F5 -12°F6
1.71 5.0%
(Not operating during this
1.70 4.7%
+12.4°F5 +15.5°F6
-«-7.90F5 +18°F6
Min iraura
value
deviation
.5.
N.V.
27.4%
-3°F6
7Q "/
. O/o
test)
8.2%
+10.5°F6
+3°F6

                                                   (continued)

-------
                                           TABLE 23   (continued).
00
Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator SFA
scrubber
fan amps
"A" Granulator drive GMA
motor amps

Liquor temperature in SLT
"A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator scrubber AOS
exit air temperature
Production rate of NHa
urea synthesis feed
process"4
_ , , Maximum Minimum
Units Standard value value
deviation % deviation % deviation
N.A.3 00 0
amps 1.23 2.6% 3.2%

A amps +4.0 amps^ +6 amps6 + 1 amps
from
standard
value2
°F 0.67 0.8% 1.3%
gpm 1.40 18.8% 5.9%
°F 1.05 1.8% 1.4%

ton/day of 0 0 0
99.5% urea
solution

                                                (continued)

-------
TABLE 23 (continued). TEST DESIGNATION  PS-2-I   DATE   10/13/78   TIME   1300  TO 1325
-




co
NJ '
1

Process
parameter
Urea 70% solution
tank level
Additive feed rate
Urea melt
temperature
"A" Granulator spray

Appendix
code
TK-101

AFR
UMT

GSP-A

Units
% of tank

Ib/hr
A°F from
design
value1
psig

Standard
deviation
0

2.5
_3oF5

0.25

Max iraum
value
% deviation
0

0.4%
-3°F6

0.7%

Minimum
value
% deviation
0

0.4%
-3°F6
x
0.7%
   "B" Granulator spray
     nozzle pressure

   "C" Granulator spray
     nozzle pressure
GSP-B    psig
GSP-C    psig
0.25
0.25
0.8%
0.7%
0.8%
0.7%
"A" Granulator inlet AIGT
air temperature
"A" Granulator outlet AOGT
air temperature
A°F from +0.25°F5 +0.5°F6
standard
r\
value
A°F from -3°F5 -4°F6
standard
f\
value
0°F6

_2°F6


                                         (continued)

-------
                                           TABLE  23   (continued).
00

Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator . SFA
scrubber
fan amps
"A" Granulator drive GMA
motor amps

Liquid temperature in SLT
"A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of Nh"3
urea synthesis feed
process**
„ , , Maximum Minimum
., . Standard , ,
Units , . . value value
deviation „, , «, ,
% deviation % deviation
N.A.3 0 0 0
amps 0 0 0

A amps +3 amps5 +4 amps6 +2 amps6
from
standard
value2
°F 0.0 0
gpm 000
°F 0.5 0.6% 0.6%


ton/day of 3.0 0.3% 0.3%
99.5% urea
solution

                                                 (continued)

-------
         TABLE 23  (continued). TEST DESIGNATION  PS-2-0  DATE  10/12/78   TIME   1630  TO 2030
I
00

Process Appendix
parameter code
Urea 70% solution TK-101
tank level
Additive feed rate AFR
Urea melt UMT
temperature
"A" Granulator spray GSP-A
nozzle pressure
"B" Granulator spray GSP-B
nozzle pressure
"C" Granulator spray GSP-C
nozzle pressure
"A" Granulator inlet AIGT
air temperature
"A" Granulator outlet AOGT
air temperature
Units
% of tank

Ib/hr
A°F from
design
value1
psig
psig
psig
A°F from
standard
o
value
A°F from
standard
value
_ . , Maximum Minimum
Standard , ,
, . . value value
deviation ./ , • • •>/ j
k deviation /•> deviation
1.36 7.2% 11.0%

34.57 8.3% . 15.6%
-4.4°F5 -5°F6 -4°F6

1.58 7.3% 5.3%
2.74 12.2% 10.3%
2.18 9.9% 8.0%
+10.6°F5 +13°F6 +8.0°F6

+5.1°F5 +9°F6 +2°F6


                                                  (continued)

-------
                                               TABLE 23   (continued).
00

Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator SPA
scrubber
fan amps
"A" Granulator drive GMA
motor amps
Liquor temperature in SLT
"A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of NH3
urea synthesis feed
process
Units
N.A,3
amps

A amps
from
standard
r\
value
oF
gpm
OF


ton/day of
99.5% urea
solution
n , . Maximum Minimum
Standard , .
, . . value value
deviation »/ , • • <•/ ,
% deviation /• deviation
0 0 0
0.96 2.3% 2.3%

+3.2 amps5 +5 amps6 +1 amps6
0.31 0.1% 1.0%
000
0.31 0.1% 1.0%


10.84 1.2% 1.7%

                                                    (continued)

-------
        TABLE 23 (continued).  TEST DESIGNATION  ps-3-I  DATE  10/13/78  TIME   1500  TO   15x5
oo

Process
parameter
Urea 70% solution
tank level
Additive feed rate
Urea melt
temperature
"A" Granulator spray
nozzle pressure
"B" Granulator spray
nozzle pressure
"C" Granulator spray
nozzle pressure
"A" Granulator inlet
air temperature
"A" Granulator outlet
air temperature
Appendix
code
TK-101

AFR
UMT

GSP-A
GSP-B
GSP-C
AIGT

AOGT

Units
% of tank

Ib/hr
A°F from
design
value
psig
psig
psig
A°F from
standard
value2
A°F from
standard
f\
value
0 . . Maximum Minimum
Standard - ..
. . value value
deviation ., , . . • ,. ,
h deviation /» deviation
000

0 0 0
-A.5°F5 -6°F6 -3°F6

0.25 0.7% 0.7%
0.25 0.8% 0.8%
000
+2.25°F5 +3°F6 -H.5°F6

-0.5°F5 -1°F6 0°F6


                                                 (continued)

-------
                                             TABLE  23   (continued).
00

Process Appendix
parameter code
Liquid level in SLL
"A" granulator
scrubber
"A" Granulator SFA
scrubber
fan amps
"A" Granulator drive GMA
motor amps
Liquor temperature in SLT
"A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of NHa
urea synthesis feed
process1*
Units
N.A.3
amps

A amps
from
standard
value2
oF
gpm
OF


ton/day of
99.5% urea
solution
„ , . Maximum Minimum
Standard ..
. . . value value
deviation «/ . • • «/ ,
% deviation f» deviation
000
000

+3 amps +4 amps6 +2 amps
0.5 0.6% 0.6%
00 0
0.5 0.6% 0.6%


3.0 0.3% 0.3%

                                                   (continued)

-------
         TABLE 23 (continued).    TEST  DESIGNATION   PS-3-0  DATE  10/13/78  TIME  0915 TO 1300
I
oo
Process Appendix
parameter code
Urea 70% solution TK-101
tank level
Additive feed rate AFR
Urea melt UMT
temperature
"A" Granulator spray GSP-A
nozzle pressure
"B" Granulator spray GSP-B
nozzle pressure
"C" Granulator spray GSP-C
nozzle pressure
"A" Granulator inlet AIGT
air temperature
"A" Granulator outlet AOGT
air temperature
Units
% of tank
Ib/hr
A°F from
design
value1
psig
psig
psig
A°F from
standard
value2
A°F from
standard
r\
value
„ . . Maximum
Standard ,
, . . value
deviation ., . . .
h deviation
0.50 6.4%
14.53 4.2%
-4.1°F5 -8°F6
0.33 0.5%
0.67 2.1%
0.48 3.7%
+1.1°F^ +2.5°F^

-3.2°F5 -7°F6

Minimum
value
% deviation
2.7%
3.9%
-3°F6
2.2%
3.9%
3.4%
0°F6

+2°F6

                                                   (continued)

-------
                                             TABLE  23    (continued).
oo
VO
I
Process Appendix
parameter code
Liquid level in SLL
"A" granulacor
scrubber
"A" Granulator SFA
scrubber
fan amps
"A" Granulator drive GMA
motor amps
Liquor temperature in SLT
"A" granulator
scrubber
Liquor feed rate to ISLF
"A" granulator
scrubber
"A" Granulator AOS
scrubber
exit air temperature
Production rate of NH's
urea synthesis feed
process'*
Units
N.A.3
amps

A amps
from
standard
value
oF
gpm
OF


ton/day of
99.5% urea
solution
. Maximum Minimum
Standard value valu£
deviation % deviation % deviation
000
1.20 3.0% 2.7%

+3.1 amps5 +5 amps6 +1 amps6
0.42 0.9% 0.2%
000
0.57 1.1% 1.3%


6.18 0.4% 1.2%

                                                    (continued)

-------
             TABLE 23 (continued) . TEST DESIGNATION  ST-1-0  DATE  10/13/78  TIME  0921  TO  0945
i
VO
o

Process
parameter
C02 feed rate to urea
synthesis process
"Dirty" steam exhaust
flow rate from urea
synthesis process
"Dirty" steam exhaust
valve actuator and
% valve open
NH3 feed rate to urea
synthesis process
Vacuum on No . 1
evaporator
Vacuum on No . 2
evaporator
Temperature of cir-
culating H20 to
top of low pres-
sure scrubber
Appendix „ .
vv , Units
code
C02 feed SCFH
DSEF Ib/hr
DSEP/ psig/% open
valve
cond
NH3 ton/day of
feed urea
EV-1 mm Hg
EV-2 mm Hg
TI 16 °F
„ . . Maximum Minimum
Standard . ,
... value value
deviation „ . . „,
A, deviation /» deviation
2,000 0.3% 0.3%
0 0 0
0/2.5 0/9.1% 0/9.1%
3.0 0.3% 0.3%
2.5 0.7% 0.7%
5.0 0.8% 0.8%
000

                                                    (continued)

-------
I
VO
         TABLE 23  (continued).  TEST  DESIGNATION   ST-2-0   DATE   10/13/78   TIME  0955 TO 1057

Process Appendix ' „ . Standard
vv . Units- ,
parameter . code deviation
C02 feed rate to C02 feed SCFH 0
urea synthesis
process
"Dirty" steam exhaust DSEF Ib/hr 0
flow rate from urea
synthesis process
"Dirty" steam exhaust DSEP/valve psig/% open 0/2.5
valve actuator and cond
% valve open
NH3 feed rate to urea NHa feed ton/day of urea 0
synthesis process
Vacuum on No. 1 EV-1 mm Hg 2.5
evaporator
Vacuum on No. 2 EV-2 mm Hg 0
evaporator
Temperature of cir- 'TI 16 °F 1°F
culating H20 to
top of low pres-
sure scrubber
Maximum
value
% deviation
0

0

0/9.1%

0
0.7%

0

0.9%
Minimum
value
% deviation
0

0

0/9.1%

0
0.7%

0

0 . 9%

                                                   (continued)

-------
TABLE 23 (continued). TEST DESIGNATION  ST-3-0  DATE  10/13/78  TIME  1125 TO 1143
         Process
         parameter
Appendix
  code
   Units
Standard
deviation
Maximum      Minimum
 value        value
deviation  % deviation
   C02 feed rate to
     urea synthesis
     process

   "Dirty" steam ex-
     haust flow rate
     from urea syn-
     thesis process

   "Dirty" steam ex-
     haust valve ac-
     tuator and %
     valve open
       feed rate to
     urea synthesis
     process
C02 fee
DSEF
   SCFH
Ib/hr
DSEP/valve psig/% open       0.25/0
cond
NH3 feed   ton/day of urea    0
                              0.6%/0
                                0
                              0
                           0.6%/0
                              0
Vacuum on No. 1 EV-1 mm Hg
evaporator
Vacuum on No . 2 EV-2 mm Hg
evaporator
Temperature of cir- TI 16 °F
culating H20 to
top of low pres-
sure scrubber
2.5 0.7% 0.7%

2.5 0.4% 0.4%

0 0 0

                                        (continued)

-------
                                          TABLE  23   (concluded).
             N.V. = Not Valid.  Because only two granulators were operating, level in this tank
             increased from 20.6 to 28.5 during this test.
            NOTES:
            Design value considered confidential.
            2Standard value arbitrarily chosen by Agrico to protect confidentiality of this
             parameter.
            3This parameter used by plant personnel as indicator of scrubber status.  Translation
             to specific units was not available.
            ''Control board instrument reading multiplied by 12.4 equals production rate of syn-
             thesis process as percent of design capacity.  Percent of design capacity multiplied
             by 1000 ton/day equals ton/day production rate.                              <
i            s
2            Average deviation from design or standard value.
i            g
             Values presented are maximum and minimum deviations from design or standard value
             observed during test.

-------
                         TABLE  24.  PARAMETER DEVIATIONS BETWEEN TESTS AT AGRICO

                                   CHEMICAL COMPANY IN BLYTHEVILLE, ARKANSAS
I
so
Process
Parameter
Additive Feed Rate
"A" Cranulator Spray Nozzle
Pressure
"B" Granulator Spray Nozzle
Pressure
"C" Granulator Spray Nozzle
Pressure
Liquid Level in "A" Granulator
Scrubber
"A" Granulator Scrubber Fan
Amps
Liquor Temperature in "A"
Granulator Scrubber
Liquor Feed Rate to "A"
Granulator Scrubber
"A" Granulator Scrubber Exit
Air Temperature
Production Rate of Urea
Synthesis Process

PS-l-I
+7.6%
+ 5.0%
not
operating
+8.0%
0%
+ 1.4%

+0.2%
+19.8%
+0.7%

+0.6%
Test Designation
PS-2-I
0%
-4.8%
-5 . 6%
-7.5%
0%
-0.7%

-3.1%
-5 . 2%
-3.3%

+1.4%
PS-3-I
-1.5%
-3.5%
-2.7%
-5.5%
0%
+ 2.1%

-1.4%
-5.2%
-2 . 1%

-2.0%
PS-1-0
-4.7%
+2.6%
not
operating
+4.4%
0%
-1.8%

+3.7%
+0.8%
+4.4%

+0.6%
PS -2-0
0%
+4.0%
+10.9%
+ 5.6%
0%
-1.6%

+3.4%
-5 . 2%
+4.0%

-1.7%
PS -3-0
-1.1%
-3.4%
-2.6%
-5.0%
0%
+0 . 6%

-2.9%
-5.2%
-3.7%

+ 1.2%
                                                              (continued)

-------
              TABLE  24  (continued).  UREA PARTICULATE  TEST  RUNS
Process
Parameter
Additive Feed Rate
"A" Granulator Spray Nozzle
Pressure
"B" Granulator Spray Nozzle
Pressure
"C" Granulator Spray Nozzle
Pressure
Liquid Level in "A" Granulator
Scrubber
"A" Granulator Scrubber Fan Amps
Liquor Temperature in "A"
Granulator Scrubber
Liquor Feed Rate to "A"
Granulator Scrubber
"A" Granulator Scrubber Exit
Air Temperature
Production Rate of Urea
Synthesis Process

UP-l-I
+2.3%
+4.2%
+8 . 1%
+6.5%
-1.2%
-0.3%
-0.8%
+2.5%
-0 . 8%

N.R.

Test Designation
UP -2 -I
+0.9%
+3.6%
+6.5%
+5.1%
+0.6%
-0.3%
-1.6%
0%
-1.6%

N.R.

UP-3-I
-3.2%
-7.5%
-13.9%
-11.1%
+0.6%
+0.2%
+2.3%
-2 . 1%
+ 2.4%

N.R.

.UP-1-0
+2.0%
+3.8%
+7.4%
+6.0%
-1.2%
-0.2%
-0.7%
+3.0%
-0.7%

N.R.

UP -2-0
+ 1.1%
+3.4%
+5 . 9%
+4.6%
+0.6%
-0.2%
-1.6%
-1.1%
-1.7%

N.R.

UP -3-0
-3 . 2%
-7 . 5%
-13.9%
-11.1%
+0 . 6%
+0.2%
+2.3%
-2 . 1%
+2.4%

N.R.

N.R. = not recorded during testing.
                                                 (continued)

-------
TABLE 24 (continued).   FORMALDEHYDE TEST RUNS
Process
Parameter
Additive Feed Rate
"A" Granulator Spray Nozzle
Pressure
"B" Granulator Spray Nozzle
Pressure
"C" Granulator Spray Nozzle
Pressure
Liquid Level in "A" Granulator
Scrubber
"A" Granulator Scrubber Fan Amps
Liquor Temperature in "A"
Granulator Scrubber
Liquor Feed Rate to "A"
Granulator Scrubber
"A" Granulator Scrubber Exit
Air Temperature
Production Rate of Urea
Synthesis Process

F-l-I
+0.3%
-0.9%
-1.5%
+ 1.1%
0%
+ 1.3%
-2 . 0%
+ 1.5%
-2.7%

+0.9%
Test Designation
F-2-I
-0.3%
-0.5%
-0.7%
+ 1.1%
0%
-0.3%
0%
-2.9%
+0.3%

0%
F-3-I
0%
+ 1.5%
+2.3%
-2 . 1%
0%
-0.8%
+ 1.9%
+1.0%
+2.4%

-0.8%
(
F-l-0
+0 . 3%
-0.9%
-1.5%
+ 1.1%
0%
+ 1.3%
-2 . 0%
+1.5%
-2.7%

+0 . 9%
F-2-0
-0 . 2%
-0.6%
-0.9%
+0.9%
0%
-0.6%
+0.1%
-2.9%
+0.3%

0%
F-3-0
0%
+ 1.5%
+2.3%
-2 . 1%
0%
-0.8%
+ 2.0%
+ 1.9%
+2.3%

-1 . 1%
                                   (continued)

-------
    TABLE  24  (continued) .  SYNTHESIS TOWER TEST RUNS
          Process
         Parameter
                                      Test Designation
C02 Feed Rate to Urea
   Synthesis Process

"Dirty" Steam Exhaust
   Flow Rate from Urea
   Synthesis Process

"Dirty" Steam Exhaust
   Valve Actuator and
   % valve open

NH3 Feed Rate to Urea
   Synthesis Process

Vacuum on No. 1 Evaporator

Vacuum on No. 2 Evaporator

Temperature of Circulating
   H20 to top of Low
   Pressure Scrubber
                              ST-1-0
-0.2%



  0%



-0.2%/-2.9%



-0.2%


+2.4%

-0.6%


-2.0%
               ST-2-0
+0.1%



  0%



-0.2%/-2.9%


+0.1%


-0.5%

+0.1%

    «
-2.0%
               ST-3-0
+0.1%



  0%



+0.4%/+5.9%


+0.1%


-1.9%

+0.5%


+4.0%

-------
                     TABLE 24 (concluded). PRODUCTION  RATES DURING TESTING - AGRICO
i
so
Oo
I

Test type
Urea particulate
Run 1
Urea particulate
Run 2
Urea particulate
Run 3
Formaldehyde
Run 1
Formaldehyde
Run 2
Formaldehyde
Run 3
Particle size
Run 1
Particle size
Run 2
Particle size
Run 3
Test _ t
• j -j Date
designation
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
UP-l-I
UP-1-0
UP-2-I
UP-2-0
UP-3-I
UP-3-0
F-l-I
F-l-0
F-2-I
F-2-0
F-3-I
F-3-0
PS-l-I
PS-1-0
PS-2-I
PS-2-0
PS-3-I
PS-3-0
10/10/78
10/10/78
10/10/78
10/10/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/12/78
10/12/78
10/13/78
10/12/78
10/13/78
10/13/78
Time pel
of rat
calculat
1130
1130
1500
1530
1620
1620
0920
0920
1120
1130
1325
1345
0915
1059
1300
1630
1500
0915
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
riod
:e
:ion
1410
1340
1700
1730
1820
1820
1030
1030
1240
1240
1515
1515
0932
1500
1325
2030
1515
1300
Production
Tons Ton/minute
44
35
32
32
29
29
19
19
22
19
31
26
4
68
6
65
3
55
.07
.40
.22
.59
.18
.18
.29
.29
.20
.43
.98
.08
.92
.04
.32
.75
.84
.49
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
2754
2723
2685
2716
2431
2431
2756
2756
2775
2776
2908
2898
2892
2835
2529
2740
2560
2466
Ton/day
397
392
387
391
350
350
397
397
400
400
419
417
417
408
364
394
369
355

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        The plant personnel indicated that the factor which had the greatest




influence on quantities of "dust" entering the scrubber was the additive to




urea ratio.  The data indicates some variance in this ratio and therefore the




dus't loading into the scrubber is expected to be somewhat higher when the




ratio is smaller.





    II.  CONTROL EQUIPMENT PARAMETERS MONITORED




         Of the 30 parameters monitored, items 10,  11 and 21 through 23 in




Table  21  were recorded specifically as indicators  of the granulator scrubber




operation during testing.




         In addition to the instrument data recorded by GCA, TRC collected




samples from various portions of the scrubber solution, whose analysis should




aid in characterizing the process operation.  These samples include:  composite




samples of the scrubber solution entering and leaving the scrubber for analysis




of urea, ammonia and formaldehyde content and the pressure drop across the




scrubber.




         As was the case with the granulator, the process parameters listed in




Table 21  for the granulator scrubber showed little variation during or between




runs.  The only significant change was the rate of  liquor fed to the scrubber




during test PS-l-I.  As requested in Table 16, the scrubber pressure drop did




vary considerably during each test.  This was probably due to variation in




scrubber liquid level, however, this could not be confirmed by the recorded




process data.





    III.  SOLUTION PROCESS




          Items 24 through 30 in Table  21 were monitored during testing of




the solution process vent as indicators of process  stability and rate.




          No significant changes in the parameters  during or between tests is




discernable from the data.





                                   -99-

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    IV.  PRODUCTION RATE DETERMINATION




         This plant is typical of the industry in that it does not determine




"instantaneous" production rates.  A calculation of daily production is made




each day by applying conversion factors to the quantity of ammonia consumed




by the urea synthesis plant for a 24-hour period.  All solid urea is weighed




as it leaves the plant.  Thus, a rough comparison between what should have




been produced and what was actually shipped can be obtained.  This comparison




is sufficiently accurate to satisfy the company's requirements.




         Plant operators monitor three major parameters which give them an




indication of overall plant rate.  These parameters are ammonia feed rate,




70 percent urea tank level, and the spray pressure of the granulator nozzles.




         Other instrumentation which is available to monitor production rates




at this plant consists solely of weigh belts.   Weigh belts monitor the amount




of unscreened solids leaving each granulator separately, the amount of screened




product leaving each of the three lines separately, and the combined total




amount of screened product from all three granulators being conveyed to the




warehouse.




         With the exception of the weigh belt measuring total combined product




to the warehouse, the weigh belt rates were indicated on totalizers as well as




strip charts.  The total product weigh belt rate was recorded only on a strip




chart.  Production rates recorded during testing are presented in Table 25.




         Plant personnel were quick to state that the accuracy of any production




rate calculated from a weigh belt indication could not be assured.  The inaccuracy




results from the inherent design of the weigh belt and accumulation of urea




solids which fall off the belt onto the device.  Plant personnel cleaned the




accumulated solids off the "A" Granulator weigh belt devices in anticipation of




testing.






                                 -100-

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                        TABLE 25.  PRODUCTION RATES DURING TESTING AT AGRICO

                                   CHEMICAL COMPANY IN BLYTHEVILLE, ARKANSAS
I
i-1
o
i-1
i

Test type
Urea particulate
Run 1
Urea particulate
Run 2
Urea particulate
Run 3
Formaldehyde
Run 1
Formaldehyde
Run 2
Formaldehyde
Run 3
Particle size
Run 1
Particle size
Run 2
Particle size
Run 3
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
A I"' < Date
designation '
UP-l-I
UP-1-0
UP-2-I
UP-2-0
UP-3-I
UP-3-0
F-l-I
F-l-0
F-2-I
F-2-0
F-3-I
F-3-0
PS-l-I
PS-1-0
PS-2-I
PS-2-0
PS-3-I
PS-3-0
10/10/78
10/10/78
10/10/78
10/10/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/11/78
10/12/78
10/12/78
10/13/78
10/12/78
10/13/78
10/13/78
Time period
of rate
calculation
1130
1130
1500
1530
1620
1620
0920
0920
1120
1130
1325
1345
0915
1059
1300
1630
1500
0915
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
1410
1340
1700
1730
1820
1820
1030
1030
1240
1240
1515
1515
0932
1500
1325
2030
1515
1300
Production
Tons Ton/minute
44.
35.
32.
32.
29.
29.
19.
19.
22.
19.
31.
26.
4.
68.
6.
65.
3.
55.
07
40
22
59
18
18
29
29
20
43
98
08
92
04
32
75
84
49
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
o.
0.
0.
0.
0.
0.
0.
2754
2723
2685
2716
2431
2431
2756
2756
2775
2776
2908
2898
2892
2835
2529
2740
2560
2466
Ton/day
397
392
387
391
350
350
397
397
400
400
419
417
417
408
364
394
369
355

-------
         On Wednesday, 11 October 1978, a 1-1/2 hour production rate test was




conducted in an effort to determine the accuracy of the various production




rate measuring methods.  This test was conducted between 1300 and 1430.  At




1300 all three granulators were placed on total recycle.  The readings on




each of the three totalizers recording screened product from each line to the




warehouse were recorded at that time.  When the strip chart for the weigh belt




recording total combined screened product to the warehouse reached zero, the




granulators were returned to normal operation.  The reading of zero indicated




a blank space on the product belt.




         When the blank space reached the warehouse, an operator diverted the




belt from the warehouse floors such that all subsequent product coming down




the belt was loaded directly into a tared railcar.  Until approximately 1430,




all product leaving the granulators was loaded directly into this railcar.




When the railcar approached capacity, the granulators were again placed on




total recycle, totalizer readings recorded, and a blank space on total product




belt generated.  When the blank space reached the warehouse, an operator




diverted the product back to the warehouse floor and the railcar was sealed




and weighed.  The third test run for formaldehyde on the scrubber inlet and




outlet was ongoing during part of this production test, but testing was sus-




pended while the granulators were being placed on total recycle and returned




to normal operation.




         The weight of urea granules produced during the production rate check




was found to be 78 tons from the railcar weighings.  Thus, the plant's production




rate was 0.8667 ton/minute or 1248 ton/day.  During the test the "A" line




screened product totalizer indicated 27.6 tons produced or a rate of 0.3067




ton/minute (441.6 ton/day).
                                   -102-

-------
         Fluid mechanics principles indicate that flow through a nozzle is

proportionate to the square root of the pressure drop across the nozzle.

Thus, if all the nozzles in the three granulators were operating and the

pressures were all equal, the flow rate into each granulator would theoretic-

ally be equal.  Also, if the pressures at each granulator were not equal then

the production rate of a particular granulator could be determined by multi-

plying the total production by the ratio of the square root of the pressure

to all three granulators.  This method of apportioning the production assumes

that all the nozzles have identical configurations which may not be the case

because of differing wear rates.

         Based on the above discussion the production rate of the "A" Granulator

should be given by the following equation;
                TP x     .      	,	,        = PA
                                                  GSP-C
y  GSP-A  +  /GSP-B   + y
where;     TP = total production of all three granulators during the
                given time.

        GSP-A = the average nozzle pressure for the subject granulator
                during the given time.

           PA = production of the "A" Granulator during the given time.

         The accuracy of the above equation is influenced by the standard

deviation of the nozzle pressures during the averaging time.

         Thus, using the weight produced as determined by the railcar (78 tons)

for TP and the average nozzle pressure for the A, B and C Granulators (41.0,

41.6, 41.7 psig, respectively) for the period from 1300 to 1430, a value for

PA can be calculated;                     /
                                         V 41.0
                       78 x	  = PA

                              7 41.0   + /41.6   + /41.7
                                                             PA = 25.85 tons
                                    -103-

-------
         However, the production of the "A" Granulator was indicated to be

27.6 tons by the weigh belt totalizer.  Assuming that the above calculation

more accurately determines the actual production rate, a factor (C.F.) can

be calculated which can be used to correct the "A" Granulator totalizer

readings for any time period;

                              27.6 (C.F.) = 25.85

                                    C.F.  = 0.9366


         The actual production of the "A" Granulator for any time period can

now be determined from the totalizer readings by the equation:

                              PAT x 0.9366 = PAA

where; PA™ = the production in tons for a given time period as indicated by
             the "A" Granulator product weigh belt totalizer.

       PAA = the actual production in tons of the "A" Granulator for the
             given time period.

         PAj is determined by calculating the difference of the totalizer

readings at the beginning and end of the time period and multiplying this

difference by 0.05 to convert to tons.

         A sample calculation using data for urea particulate, run 1, outlet

on 10 October 1978 is presented below.


         Example:  (Refer to Table 3-2 and Appendix J)

                   Test started - 1131
                   Test ended   - 1336
                   Totalizer reading at 1130* = 3976
                   Totalizer reading at 1340* = 4732
                   Time between initial and final
                     totalizer readings = 130 minutes
                   PAT = (4732-3976)  x 0.05 = 37.8 tons

                         37.8 x 0.9366 = PA.  =35.4 tons
*  Data from column designated PWTA in Appendix J.
                                  -104-

-------
                      35.4  tons           ton/minute average
                     130 minutes             ,
                                          production rate
             -,r /        1440 minutes/day    orio    ,,
             35.4 tons x —T-T-	:	L  = 392 ton/day
                            130 minutes
Production rates for all test runs  are  presented in Table 25.
                                -105-

-------
                             SECTION 4





                    LOCATION OF SAMPLING POINTS









     Testing was conducted on the "A" Granulator and the Synthesis Tower




Vent at the Agrico Chemical Company in Blytheville,  Arkansas.   This section




presents the detailed descriptions of the sampling locations for the urea,




ammonia, formaldehyde,  particle sizing and the opacity measurements.









SCRUBBER INLET, TP-I




     The scrubber inlet sampling site was located in a 48-inch I.D. horizontal




section of a steel duct.  A schematic of the sampling site including the tra-




verse point sampling locations and duct dimensions is presented in Figure 5.




Two 4-inch I.D. pipe-flange sampling ports positioned 90  apart were located




20 feet (5 stack diameters) upstream of a short-radius, right  angle bend.




The distance from the ports to the nearest downstream disturbance (another




right-angle bend) was 10 feet (2.5 stack diameters).




     The inlet sampling location did not meet the" "eight and two diameters"




criteria as outlined in EPA Method 1; consequently,  12 sampling points were




chosen for each axis traverse for a total of 24 sampling points (as specified




by the method).  These points were located as shown in Figure  5.  This




figure shows the cross-sectional view of the duct at the sampling loca-




tion and lists the exact distance each traverse point is located from the




outside flange edge.  The identifying number sequence and point locations




were the same for all testing conducted at the inlet location.
                                 -106-

-------
      SCRUBBER
 SCRUBBER
INLET PORTS
                                                                   4'
                                  •10'-
                                        •DILUTION
                                           AIR
                           SOUTH
                                                    NORTH
A - LOCATION OF TEST PORTS
TRAVERSE POINT NO.
1
2
3
4
5
6
7
8
9
10
11
12
TRAVERSE POINT
FROM OUTSIDE EDGE
(INCHES)
7
9 1/4
11 5/8
14 1/2
18
23 1/8
36 7/8
42
45 1/2
48 3/8
50 3/4
53
DISTANCE
OF NIPPLE












      FIGURE 5:  LOCATIONS OF "A" GRANULATOR SCRUBBER  INLET TEST PORTS & POINTS AT
                       AGRICO CHEMICAL COMPANY IN BLYTHEVILLE,  ARKANSAS
                                          -107-

-------
SCRUBBER OUTLET, TP-.2




     The cleaned gases exiting the scrubber unit are ducted to an induced draft




fan adjacent to the emission control unit.  The fan discharge is directed ver-




tically through a steel stack to the atmosphere.




     The "A" scrubber 60-inch I.D. outlet stack was fitted with two 4-inch I.D.




pipe-flanged sampling ports positioned 90° apart in a horizontal plane.  The




two ports were located 65-feet (.13 stack diameters) downstream of the fan out-




let, and 20 feet (4 stack diameters) upstream of the stack discharge; See Figure 6.




The port locations met the "eight and two diameters" criteria as delineated in EPA




Method 1.  Consequently, six sampling points were calculated for each axis




traverse for a total of twelve sampling points (as specified in the method).









INLET PARTICLE SIZING SAMPLING LOCATION, TP-.1




     Particle sizing tests were performed in the "A" Granulator Scrubber inlet




gas stream by sampling with an in-stack cascade impactor positioned in the duct




through the test ports used for the emissions tests shown in Figure 5.  The




impactor nozzle was located at the centroid of the duct for each impactor




run.









OUTLET PARTICLE SIZING SAMPLING LOCATION, TP-2




     The size distribution of the particulate in the "A" Granulator Scrubber




outlet stream was measured with an in-stack cascade impactor positioned in the




stack through the tests ports used for the emissions tests (see Figure 6).  The




impactor nozzle was located at the centroid of the stack for each, impactor




run.
                                    -108-

-------
20'
65'
I
M
O
I
               I-*-
            t
                      5'
         .   SCRUBBER
          OUTLET PORTS
i
                            SCRUBBER
                FAN
     A -  LOCATION  OF  TEST  PORTS
                                                                            NORTH WEST
                                                                                   65 3/4'
                                                                               NORTH EAST
TRAVERSE POINT NO.
                                                        1
                                                        2
                                                        3
                                                        4
                                                        5
                                                        6
  TRAVERSE POINT DISTANCE
FROM OUTSIDE EDGE OF NIPPLE
         (INCHES)
                                8  5/8"
                               14  3/4"
                               23  3/4"
                               48  1/8"
                               57"
                               53  1/8"
                                                                             B - LOCATION OF TEST POINTS
                           FIGURE 6:  LOCATIONS OF "A" GRANULATOR SCRUBBER OUTLET JEST PORTS & POINTS AT
                                            AGRICO CHEMICAL COMPANY IN BLYTHEVILLE, ARKANSAS

-------
VISIBLE EMISSIONS OBSERVATION LOCATIONS




     Figure 7 indicates the relative position of the two different observation




sites employed to observe the white scrubber stack plume.  These locations were




chosen in order to conform to EPA Method 9 guidelines and specifications.   The




stack discharge was approximately 100 feet above ground level.   The observer was




positioned at distances of 100 to 150 feet from the stack.   Heights of the




observation sites ranged from ground level to about 100 feet above grade.   De-




pending upon the sun position and the cloud cover, the observer either posi-




tioned himself on the synthesis tower and used the trees as a dark background or




he stood in a field and used the synthesis tower for a dark background.









SCRUBBER" PRESSURE DROP PRESSURE TAPS LOCATIONS




     Pressure drop across the "A" Granulator Scrubber was measured with a  ver-




tical U tube water manometer which was connected to pressure taps at the scrub-




ber inlet and outlet.  The inlet pressure tap consisted of a stainless steel tube




inserted into the middle of the duct through the dilution air damper.   The




tubing was fixed in place so that the open end was perpendicular to the flow




stream.  The outlet pressure tap consisted of a hole drilled through the section




of ducting between the scrubber outlet and the inlet of the fan.









SCRUBBER LIQUID COLLECTION LOCATIONS




     Scrubber solution samples were collected from the streams  entering and




leaving the "A" Granulator Scrubber (see Figure 8).  The inlet  sample was  tapped




from the line immediately before entering the scrubber.  The outlet sample was




tapped from the pump discharge.
                                   -110-

-------
                      ^100 FT
   SYNTHESIS
     TOWER
OBSERVER X (1001 ABOVE GRADE)
                           FT
                          OBSERVER X (GROUND LEVEL)

'A" GRANULATOR SCRUBBER STACK



"B" GRANULATOR SCRUBBER STACK



"" GRANULATOR SCRUBBER STACK
            FIGURE 7:  LOCATIONS OF SMOKE OBSERVER FOR OCTOBER 10 - 12,1978
                       OPACITY READINGS ON "A" GRANULTOR SCRUBBER STACK AT
                       AGRICO CHEMICAL COMPANY IN BLYTHEVILLE, ARKANSAS
                                       -1-11-

-------
INLET TAP
                                'A1 GRANULATOR  SCRUBBER
                                          PUMP
                       OUTLET TAP
FIGURE 8:  LOCATION OF SCRUBBER LIQUID COLLECTION TAPS FOR OCTOBER
           10 & 11. 1978.  TESTS ON "A" GRANULATOR AT AGRICO CHEMICAL
                        COMPANY IN BLYTHEVILLE,  ARKANSAS
                                 -112-

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PROCESS SAMPLES COLLECTION LOCATIONS
    Throughout the testing program, various process samples were collected
directly from their applicable process units/operations.  Included were
samples of urea melt, a formaldehyde-based additive, and the granulator un-
screened and screened products.

UREA SYNTHESIS TOWER VENT LOCATION
    The urea synthesis tower sampling site was located in a 14-inch I.D.
vertical section of a heavy gauge stainless steel pipe.  A schematic of the
sampling site including the velocity traverse points and duct dimensions is
presented in Figure 9.  One 6-inch I.D. pipe-flange sampling port was positioned
approximately 30 feet (25 stack diameters) upstream of a connecting exhaust
vent.  The distance between the sampling port and the stack vertex was approx-
imately 15 feet (12 stack diameters).  The port location met the EPA Method 1
criteria.  However, only a single sampling point located 12 inches inside the
stack from outside the flange (the centroid of the duct) was used during the
five test runs.   This was requested by the Technical Manager, due to the fol-
lowing problems encountered during the testing periods.

    1.  Excessive moisture content (80 percent).
    2.  High ammonia concentrations.
        (1,300 Ib/hour)
    3.  Extremely high stack gas velocities.
        (12,000 feet/minute)
    4.  Hostile working environment
        a.   Cold temperature (0 F windchill)
        b.   High winds (40 to 50 miles per hour)
        c.   Raining
    5.  Plugging of pitot and orifice pressure lines with water.
                                    -113-

-------
 .ft
FLOW
 ft

 ft
                   .14"
                                                 \.
              15'
              30'
                                                      6"—'
     VELOCITY
TRAVERSE POINT NO.
                                      1
                                      2
                                      3
                                      4
  TRAVERSE POINT DISTANCE
FROM OUTSIDE EDGE OF NIPPLE
         (INCHES)
                                 7.0
                                 9.5
                                16.5
                                19.0
      FIGURE 9:    LOCATION OF SYNTHESIS TOWER SOLUTION  VENT
                 SAMPLING PORT AND VELOCITY TRAVERSE POINTS
                     .  AT AGRICO CHEMICAL COMPANY IN
                          BLYTHEVILLE, ARKANSAS
                                 -114-

-------
                              SECTION 5
                  SAMPLING AND ANALYSIS METHODOLOGIES


     This section presents the descriptions of the sampling and analysis
methodologies employed' at the Agrico Chemical Company facility in Blytheville,
Arkansas during October 9-13, 1978.
     The EPA designated methods are contained in the respective Appendices.
This section presents general descriptions and deviations from the methods
in the Appendices.


UREA AND AMMONIA "A" GRANULATOR SCRUBBER INLET AND OUTLET
     Urea and ammonia in the "A" Granulator Scrubber inlet and outlet gas
streams were sampled at points identified by EPA Method 1 in accordance with
the relationship of the sampling ports to upstream and downstream diameters.
The velocity of the duct gas was measured using a calibrated, S-type pitot
 tube  in accordance with EPA Method 2.  Construction and calibration of the
S-type pitot tubes was consistent with EPA Method 2.  The complete method
of sampling and analysis for urea and ammonia is contained in Appendix M.
     The sampling train is shown schematically in Figure 10 and consists of
a nozzle, probe, filter, Teflon line connector, five impingers, vacuum
pump,  dry gas meter, and an orifice flow meter.  The nozzle (1) is stainless
steel and is of a buttonhook shape.  It was connected to a 5/8" stainless
steel glass lined probe (2) that is wrapped with nichrome heating wire
and jacketed.  The probe temperature was maintained at 160 F to prevent
condensation of the sampled gas.  Following the probe, the gas stream
impacted on a 4V glass filter supported on a coarse fritted glass disc
in a glass filter holder (3).  Reeve Angel Type 934 AH filter paper
                                   -115-

-------
                   THERMOMETER
STACK WALL
                                                         THERMOMETER
                       13
CHECK VALVE

__
\
_
.1
nr
I
5
M»

_

                    FIGURE 10:  MODIFIED EPA PARTICULATE SAMPLING TRAIN
                                   AUGUST 18,1977, FEDERAL REGISTER
                                                                                         LEGEND
                                                                         i- NOZZLE
                                                                         a- PROBE
                                                                         3- FILTER HOLDER
                                                                         4- FILTER OVEN
                                                                         3- ICE BATH
                                                                         6- TYGON TUBING
                                                                         7- VACUUM GAGE
            «- NEEDLE VALVE
            9- PUMP
            10- VALVE
            11- DRY GAS MEETEI
            w- ORIFICE
            13- PITOT TUBE
            u- POTENTIOMETER

-------
was used.  Enclosing the whole filter assembly was a heated box (4) to




maintain temperature of the gas leaving the filter at 160 F.  EPA Reference




Method specifies a temperature of 248 F - 25 F, however, urea melts and




readily decomposes to ammonia at temperatured above 200 .   The filter and




heated box were not used for outlet run 3 (test #7).  An ice bath containing




five impingers(S) was attached to the back end of the filter via a section




of Teflon tubing.  The first impinger contained deionized distilled water




(100 ml), the second and third contained 100 ml of  IN  E2SO^ each, the




fourth was dry and the fifth contained silica gel (200 grams).   Leaving




the fifth impinger, the dry sample stream flowed through flexible tubing




(6), a vacuum gauge (7), needle valve (8), pump (9), and a dry gas meter (11).




A calibrated orifice and inclined manometer (12)  complete the sampling




train.  The stack velocity pressure was measured using a pitot tube (13)




and inclined manometer.  Stack temperature was monitored by a thermocouple




attached to the probe and connected to a potentiometer (14).  A nomograph




determined the orifice pressure drop required for any pitot velocity




pressure and stack temperature in order to maintain isokinetic sampling




conditions.




     Test data recorded included test time, sampling duration of each traverse




point, pitot pressure, stack temperature, meter volume, meter inlet-outlet




temperature and orifice pressure drop.  At completion of each run the probe




was removed from the stack and was purged for 15-20 minutes with ambient




air.  This was done so that any remaining ammonia in the train would be




collected in the impingers.  A final leak check was then performed.
                                 -117-  -

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The nozzle and probe were then washed and brushed three times into a glass

sample jar which was sealed with a Teflon-lined cap.  The probe washes were

performed on site near the stack.  The Teflon line between the filter and

first impinger was rinsed with, distilled, deionized water three times into

a second glass sample jar and sealed.  The sample jars and impingers were

returned to the sample train prep and clean-up room.

     The contents of impingers were transferred to tare weighted sample

jars at the clean-up area.  The sample containers were used as follows:


     Container #1 - Filter
         (
     Container #2 - Deionized distilled water wash of nozzle, probe
                    and all glassware up to the filter.

     Container #3 - Silica gel from the fifth impinger.

     Container #4 - Contents of first impinger and deionized distilled
                    water wash of first impinger, Teflon line and glass-
                    ware between filter and first impinger.

     Container #5 - Contents of second, third, and fourth impingers and
                    deionized distilled water wash of impingers plus
                    connecting glassware.


     Aliquots of some of the samples were analyzed for urea and ammonia by

Agrico chemists.  The remainder of the samples were transported to TRC's

laboratory and analyzed for urea and ammonia.  The urea concentration was

measured by adding urea color reagent (see Appendix M) to the samples and

measuring the absorbance of the solutions with a spectrophotometer at 420

nm.   The ammonia concentration was measured by adding Nessler reagent to the

samples and measuring the absorbance of the solutions with a spectrophoto-

meter at 405 nm.  Calibration curves were drawn from the corresponding

absorbances of standard urea and ammonia solutions.   The calibration curves

were used to determine the urea and ammonia concentrations of the samples.
                                   -118-

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The sample concentration was multiplied by the sample volume to determine the

total urea and ammonia.  It should be noted that a aliquot was removed for analy

 sis., by Agrico .chemists, however, this aliquot volume was included in the sample

volume for calculation of total urea, ammonia and formaldehyde collected.
FORMALDEHYDE "A" GRANULATOR SCRUBBER

     The complete method for sampling and analysis for formaldehyde is

contained in Appendix M.  Formaldehyde in the "A" Granulator Scrubber

inlet and outlet gas streams was sampled using the methodology and

equipment described in the subsection entitled Urea and Ammonia "A"

Granulator Scrubber with the following modifications:


     1.  There were only four impingers used.  Impingers one and
         two contained 100 ml each of distilled deionized water,
         impinger three was dry and impinger four contained 200
         grams af silica gel (See Figure 11),

     2.  The filter and heated box were not used for the outlet
         tests.

     The contents of the impingers were transferred to tare weighted sample

jars at the clean-up area.  The sample containers were used as follows:


     Container #1  -  Filter (inlet only)

     Container #2  -  Deionized distilled water wash of nozzle,
                      probe, Teflon line, filter holder (inlet
                      only), impingers 1, 2 and 3 and their
                      connecting glassware, plus the contents
                      of impingers 1,2, and 3.

     Container #3  -  Silica gel from the fourth impinger
                                   -119-

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                              THERMOMETER
           STACK WALL	*~
                                                                                      CHECK  VALVE
NJ
O
                                                                                              LEGEND
                                                                              i- NOZZLE
                                                                              2- PROBE
                                                                              3- FILTER HOLDER
                                                                              4- FILTER OVEN
                                                                              5- ICE BATH
                                                                              6- TYGON TUBING
                                                                              7- VACUUM GAGE
 e-  NEEDLE  VALVE
 9-  PUMP
10-  VALVE
11-  DRY  GAS MEETER
»2-  ORIFICE
 13-  PITOT TUBE
 14-  POTENTIOMETER
                        FIGURE 11 :   MODIFIED EPA PARTICULATE SAMPLING  TRAIN
                                        AUGUST 18,1977,  FEDERAL  REGISTER

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     The samples were analyzed for urea and ammonia in addition to




formaldehyde.  The analyses for urea and ammonia were performed as de-




scribed previously.  The analysis for formaldehyde consisted of reacting




an aliquot of the sample solution with chromatropic-sulfuric acid reagent




to form a purple chromogen.  This colored solution was analyzed colori-




metrically using a spectrophotometer at 580 nm.  The absorbance of the




colored solution is proportional to the quantity of formaldehyde.  Standard




formaldehyde solutions were prepared to produce a calibration curve which




was nsed-to determine formaldehyde concentration of the individual sample.




The sample concentration was multiplied by the sample volume to determine




the total formaldehyde in the sample.









VISIBLE EMISSIONS "A" GRANULATOR




     The visible emissions measurements were conducted by a certified




visual emission evaluator in accordance with EPA Reference Method 9.




The readings were taken at 15 second intervals.  Since the plume was




white, it was necessary to read the emissions against a dark back-




ground.  The dark background was provided by either the synthesis tower




or a row of trees.









PARTICLE SIZE "A" GRANULATOR




     A Sierra Model 226 multi-stage cascade impactor was operated in its




instack mode.  Sampling was performed isokinetically from a single point




at the center of the scrubber inlet and outlet ducts.  Prior to the
                                   -121-

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initiation of sampling, the impactor was leak tested and placed in the




flow stream for 20 minutes to allow for heating to duct temperature and




thereby prevent condensation.  Sampling was initiated immediately




upon rotation of the nozzle into the flow stream.  The brief sampling




time at the inlet necessitated presetting of the sampling valve so




that when the nozzle was pointed into the flow stream and the pump




started, only a minimal adjustment of the valve was necessary for isoki-




netic flow.




     The impactor was loaded before each run with preweighed glass fiber




collection substrates.  After sampling the impactor was removed to the




clean up room and the substrates placed in plastic petri dishes and sealed.




The cyclone was brushed and washed with distilled deionized water into a




sample jar and sealed.  These samples were returned to TRC and weighed




on an analytical balances to 0.01 mg.  The filters were dessicated for




at least 24 hours before the initial weighing.   The filters were then




weighed until a constant weight was reached.   If constant weight was




not attained,  the filters were then redessicated for at least six hours.




The weighing room had an environment where the relative humidity was




less than 50 percent.  More information on particle sizing can be found in




Appendix B.








SCRUBBER LIQUID "A" GRANULATOR




     Samples (approximately 500 ml)  of the scrubbing liquid streams




entering and exiting  the "A" Granulator Scrubber were collected at




approximately 15 minute intervals during the  urea and ammonia tests.




The sample temperature was measured immediately upon collection.
                                  -122-

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The sample was then allowed to reach room temperature and then the




pH was measured with a- pH meter.




     The individual samples were then composited into one inlet and




one outlet sample for each associated run.  The pH of the composite




sample was also measured with the pH meter.  The composited samples




were returned to TRC's laboratory and analyzed for urea, ammonia,




and formaldehyde concentration in accordance with Appendix M.









PROCESS SAMPLES "A" GRANULATOR




     Grab samples of the urea melt, unscreened and screened product




were collected at their respective locations in the process.  A grab




formaldehyde additive sample was also collected and retained for pos-




sible future analysis.




     The urea melt, unscreened and screened product samples were pre-




pared for analysis by dissolving a known weight (approximately 200 mg)




into 100 ml of distilled deionized water.  The solution was then analyzed




for urea, ammonia and formaldehyde using the procedures in Appendix M




and Appendix E.









UREA AND AMMONIA SYNTHESIS TOWER MAIN VENT




     Urea and ammonia in the Synthesis Tower Main Vent Stack were sampled




from a single point located in the geometric center of the duct.  The




velocity of the duct gas was measured using a S-type pitot tube in




accordance with EPA Method 2.  Construction of the S-type pitot tube




was consistent with EPA Method 2.  The velocity profile across the duct




was found to be flat during the preliminary traverse.
                                  -123-

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     The sampling train is shown schematically in Figure 12 and consists




of a nozzle, instack orifice, probe, Teflon line, eight impingers, vacuum




pump and a dry gas meter.  The nozzle  (1) is stainless steel and is of a




buttonhook shape.  An instack orifice  (.3) was used to permit isokinetic




sampling of a stream with a moisture content greater than 50%.  The instack




orifice meters the sample at the stack conditions and, therefore, changes




in moisture will not affect isokinetic sampling.  The instack orifice




was connected to a 5/8" stainless steel glass lined probe (2).  An ice




bath containing eight impingers (5) was attached to the probe via a




section of Teflon tubing.  Impingers one through four contained 100 ml




each of distilled deionized water, impinger five was empty and numbers




six and seven each contained 100 ml of ION H2S01+.  The ION E2SO^ was




necessary because of the high ammonia concentration.  The smell of




ammonia was noticed in the exhaust of the train during tests 1 and 2




and the silica gel turned purple during these tests indicating in-




complete ammonia collection in the impingers.  The eighth impinger




contained silica gel (200 grams).   Leaving the eight impinger, the




dry sample stream flowed through flexible tubing (6), a vacuum gauge




(.7),  needle valve (8),  pump (9), and a dry gas meter (11).  A cali-




brated orifice and included manometer (12), complete the sampling train.




The stack velocity pressure was measured using a pitot tube (13) and




inclined manometer.   Stack temperature was monitored by a thermocouple




attached to the probe and connected to a potentiometer (14).   A calcula-




tion was made to determine the instack orifice pressure drop required




for any pitot velocity pressure in order to maintain isokinetic sampling




conditions.





                                  -124-

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                                                                             THERMOMETER
STACK HALL
                                                             CHECK VALVE
     N.
     Ol
     I
                                                                                      LEGEND
                                                                      l- NOZZLE
                                                                      1- PROBE
                                                                      J- INSTACK ORIFICE
                                                                      4- TEFLON TUBING
                                                                      •- ICE BATH
                                                                      •- TYGON TUBING
                                                                      7- VACUUM GAGE
                                                  •-  NEEDLE  VALVE
                                                  f-  PUMP
                                                 »0-  VALVE
                                                 11-  DRY GAS MEETER
                                                 n-  ORIFICE
                                                 13-  PITOT TUBE
                                                 14-  POTENTIOMETER
                               FIGURE 12:
MODIFIED EPA PARTICULATE  SAMPLING TRAIN WITH INSTACK ORIFICE
         AUGUST 18,1977,  FEDERAL REGISTER,

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     Test data recorded included test time, pitot pressure, stack temperature,

meter volume, meter inlet-outlet temperature and orifice pressure drop.  At

completion of each run the train was leak checked, then purged for 15 minutes

to assure complete collection of ammonia.  The nozzle and probe were washed

and brushed three times on site into a glass sample jar which was sealed with a

Teflon-lined cap.  The Teflon line between the probe and 1st impinger was

rinsed three times with distilled, deionized water into a second glass

sample jar and sealed.  The sample jars and impingers were returned to the

sample train prep and clean up room for storage and measurement of volume

of liquid collected.

     The contents of impingers were transferred to tare weighted sample

jars at the clean up area.  The sample containers were used as follows:


     Container #1  -  Contents of first five impingers and deionized
                      distilled water wash of impingers, Teflon line,
                      nozzle and probe.

     Container #2  -  Contents of impingers six and seven and deionized
                      distilled water wash of impingers.

     Container #3  -  Silica gel from eighth impinger.


     The samples were transported to TRC's laboratory and analyzed for

urea, ammonia and formaldehyde.  The urea concentration was measured by

adding urea color reagent (see Appendix M) to the samples and measuring

the absorbance of the solutions with a spectrophotometer at 420 nm.   The

ammonia concentration was measured by adding Nessler reagent to the samples

and measuring the absorbance of the solutions with a spectrophotometer

at 405 nm.  The formaldehyde concentration was measured by reacting an

aliquot of the sample solution with chromatropic-sulfuric acid reagent.
                                 -126-

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to form a purple chromogen.  This colored solution was analyzed colori-




metrically using a spectrophotometer at 580 run.  Calibration curves were




drawn from the corresponding absorbances of urea, NHa, and formaldehyde




standard solutions.  The calibration curves were used to determine the




urea and ammonia concentrations of the samples.  The sample concentration




was multiplied by the sample volume to determine the total urea, ammonia




and formaldehyde.    Special calculations were performed to determine the




volume of dry gas sampled, percent moisture and molecular weight of duct




gas.  The gaseous volume of ammonia collected in the impingers was added




to the volume measured by the dry gas meter to equal the total dry sample




volume.  The gaseous equivalent volume of water collected in the impingers




was divided by the total sample volume (H20 gaseous equivalent volume +




NHs gaseous equivalent volume + dry gas volume measured by dry gas meter)




to determine the percent moisture in the duct gas stream.  The molecular




weight of the duct gas stream was calculated from the percent moisture,




percent ammonia and the percent CQ2, 02,  and N2 of the dry gas volume




based on measurements at a similar synthesis tower.  Appendix G contains




the complete calculations.
                                 -127-

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