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
-------
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-
-------
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-
-------
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-
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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-
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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-
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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-
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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-
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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-
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^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-
-------
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-
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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- -
-------
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-
-------
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-
-------
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
-------
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-
-------
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-
-------
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.
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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.
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