SERA
United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
EMB Report 80-NHF-14
August 1980
Air
Urea Manufacture
Emission Test Report
Reichhold Chemicals,
Incorporated
St. Helens, Oregon
-------
REPORT ON
PROCESS EMISSIONS TESTS AT THE
REICHHOLD CHEMICALS, INC.
UREA MANUFACTURING FACILITY IN
ST. HELENS, OREGON
Thomas M. Bibb
EPA Project Officer
EPA Technical Manager
Clyde E. Riley
EPA Contract # 68-02-2820
Work Assignment #19
TRC Project #0988-E80-90
Prepared By:
Willard A. Wade III, P.E., Project Manager
Leigh A. Ganunie, Project Engineer
August 27, 1980
-------
PREFACE
The work reported herein was performed by personnel from TRC Environmental
Consultants, Inc. (TRC), the Radian Corporation, Reichhold Chemicals, Inc.,
St. Helens, Oregon, and the U.S. Environmental Protection Agency (EPA).
The scope of work, issued under EPA Contract No. 68-02-2820, Work Assign-
ment No. 19, was under the supervision of the TRC Project Manager, Mr. Willard
A. Wade III, P.E. Mr. Leigh A. Gammie of TRC served as Project Engineer and
was responsible for summarizing the test and analytical data presented in this
report. Sample analysis was performed at Reichhold Chemicals, Inc., St.
Helens, Oregon plant under the direction of Ms. Margaret M. Fox, and at the
TRC laboratory in Wethersfield, Connecticut under the direction of Mr. Samuel
S. Cha.
Mr. Mark S. Jennings of Radian was responsible for monitoring the process
operations during the emissions testing program. Radian personnel were also
responsible for preparing Section 3.0, Process Description and Operation, of
this report.
Personnel of Reichhold Chemicals, Inc., St. Helens, Oregon, whose assist-
ance and guidance contributed greatly to the success of this emission test
program include Mr. E.J. Stipkala, Vice President, and Mr. John H. Cramer,
Operations Manager.
Mr. Eric A. Noble, Office of Air Quality Planning and Standards, Industri-
al 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.
-ii-
-------
TRC-Environmental Consultants, Inc.
Willard A. Wade III, P.E.
Senior Project Manager
August 27, 1980
NOTE: Mention of trade names or commercial products in this publication does
not constitute endorsement or recommendation for use by the United
States Environmental Protection Agency.
-111-
-------
TABLE OF CONTENTS
SECTION PAGE
PREFACE ii
1.0 INTRODUCTION 1
1.1 Overview 1
1.2 Brief Process Description 4
1.3 Emissions Measurement Program .... 4
1.4 Description of Report Sections 5
2.0 SUMMARY OF RESULTS 6
2.1 Comparison of CHEAF Scrubber Series A and
Series B Outlet Emission Test Results 6
2.2 CHEAF Scrubber Emission Test Results 11
2.3 Visible Emissions 17
2.4 Particle Size Tests 17
2.5 Pressure Drops Across the CHEAF Scrubber 29
2.6 Analysis of Scrubber Liquor 29
2.7 Ambient Air Temperature and Relative Humidity
Measurements 34
3.0 PROCESS DESCRIPTION AND OPERATION . 38
3.1 Urea Production Process Description 38
3.2 Prill Tower Emission Control System Description . . 40
3.3 Monitoring of Plant Processes During Emissions
Tests 44
3.3.1 Urea Production Process Monitoring 44
3.3.2 Emission Control System Monitoring 53
3.4 Summary of Plant Operations 61
4.0 LOCATION OF SAMPLING PORTS AND POINTS 68
4.1 CHEAF Inlet (Downcomer) '. . . . 68
4.2 CHEAF Outlet 68
4.3 Inlet Particle Sizing Locations 71
4.4 Visible Emissions Observation Locations 71
4.5 Scrubber Liquor Collection Locations 71
4.6 Ambient Air Temperature and Relative Humidity
Measurement Location 74
5.0 SAMPLING AND ANALYSIS METHODS 75
5.1 EPA Reference Methods Used in this Program 75
5.2 Urea Sampling and Analysis at the Cleanable High
Efficiency Air Filter Scrubber (CHEAF) 76
5.2.1 Sampling Methods 76
5.2.1.1 CHEAF Inlet 78
5.2.1.2 CHEAF Outlet 79
5.2.2 Sample Recovery and Preparation 79
5.2.3 Sample Analysis 80
5.2.3.1 Inlet 80
5.2.3.2 Outlet 80
-iv-
-------
TABLE OF CONTENTS (Continued)
SECTION PAGE
5.3 Ammonia Sampling and Analysis at the Cleanable
High Efficiency Air Filter Scrubber (CHEAP) ... 81
5.3.1 Sampling and Sample Recovery 81
5.3.1.1 Inlet 81
5.3.1.2 Outlet 82
5.4 Visible Emissions 82
5.5 Particle Size Tests 83
5.6 Scrubber Liquor Sampling and Analysis 84
5.7 Pressure Drop Measurements Across the CHEAP
Scrubber 85
5.8 Ambient Air Temperature and Relative Humidity ... 85
-v-
-------
LIST OF FIGURES
FIGURES PAGE
1-1 General Plant Production Process Flow Diagram .... 2
1-2 Diagram of Prill Tower Emission Control System. ... 3
2-1 Six Minute Averages of April 15-16, 1980, Opacity
Readings on the CHEAP Scrubber Stack, Reichhold
Chemicals, Inc., St. Helens, Oregon 18
2-2 Six Minute Averages of April 17, 1980, Opacity
Readings on the CHEAP Scrubber Stack, Reichhold
Chemicals, Inc., St. Helens, Oregon 19
2-3 Six Minute Averages of April 18-21, 1980, Opacity
Readings on the CHEAP Scrubber Stack, Reichhold
Chemicals, Inc., St. Helens, Oregon 20
2-4 Six Minute Averages of April 22, 1980, Opacity
Readings on the CHEAP Scrubber Stack, Reichhold
Chemicals, Inc., St. Helens, Oregon 21
2-5 Six Minute Averages of April 23, 1980, Opacity
Readings on the CHEAP Scrubber Stack, Reichhold
Chemicals, Inc., St. Helens, Oregon 22
2-6 Cumulative Size Distributions of Particulate in
the CHEAP Downcomer Stack at Reichhold Chemi-
cals, Inc., St. Helens, Oregon 31
3-1 General Plant Production Process Flow Diagram .... 39
3-2 Diagram of Prill Tower Emission Control System. ... 41
3-3 Diagram of CHEAP Scrubber 43
4-1 Schematic of Prill Tower and CHEAP Scrubber at
Reichhold Chemicals, Inc., St. Helens, Oregon ... 69
4-2 CHEAP Inlet (Downcomer) Sampling Location,
Reichhold Chemicals, Inc., St. Helens, Oregon ... 70
4-3 CHEAP Outlet Sampling Location, Reichhold Chemi-
cals, Inc., St. Helens, Oregon 72
4-4 Visible Emissions Observer Locations, Reichhold
Chemicals, Inc., St. Helens, Oregon 73
5-1 Modified EPA Particulate Sampling Train 77
-vi-
-------
LIST OF TABLES
TABLE
2-la(English)
PAGE
2-lb(Metric)
2-lc(English)
2-ld(Metric)
2-2a (English)
2-2b(Metric)
2-3
2-4
2-5
2-6
Summary of Results of Urea and Ammonia Tests on
Gases Exiting the CHEAP Scrubber (Series A & B)
on April 15-22, 1980 at Reichhold Chemicals,
Inc., St. Helens, Oregon
Summary of Results of Urea and Ammonia Tests on
Gases Exiting the CHEAP Scrubber (Series A & B)
on April 15-22, 1980 at Reichhold Chemicals,
Inc., St. Helens, Oregon
Summary of Results of Urea and Ammonia Tests on
Gases Exiting the CHEAP Scrubber (Series A & B)
on April 15-22, 1980 at Reichhold Chemicals,
Inc., S.t. Helens, Oregon
Summary of Results of Urea and Ammonia Tests on
Gases Exiting the CHEAP Scrubber (Series A & B)
on April 15-22, 1980 at Reichhold Chemicals,
Inc., St. Helens, Oregon
Summary of Results of Urea and Ammonia Tests on
Gases Entering and Exiting the CHEAP Scrubber
(Series A) on April 15-17, 1980 at Reichhold
Chemicals, Inc., St. Helens, Oregon
Summary of Results of Urea and Ammonia Tests on
Gases Entering and Exiting the CHEAP Scrubber
(Series A) on April 15-17, 1980 at Reichhold
Chemicals, Inc., St. Helens, Oregon
Summary of Results of Urea and Ammonia Tests on
Gases Entering and Exiting the CHEAP Scrubber
(Series A) on April 15-17, 1980 at Reichhold
Chemicals, Inc., St. Helens, Oregon ......
Summary of Results of Urea and Ammonia Tests on
Gases Exiting the CHEAP Scrubber (Series A)
on April 15-17, 1980 at Reichhold Chemicals, Inc.,
St. Helens, Oregon
10
12
13
14
15
Summary of Results of Urea and Ammonia Tests on
Gases Exiting the CHEAP Scrubber (Series B)
on April 18-22, 1980 at Reichhold Chemicals, Inc.,
St. Helens, Oregon
Six Minute Arithmetic Average Opacity Readings on
the CHEAP Scrubber Outlet at Reichhold Chemicals
Inc, St. Helens, Oregon
16
23-28
-vii-
-------
LIST OF TABLES (Continued)
TABLE PAGE
2-7 Summary of Results of the CHEAP Downcomer Particle
Size Tests at Reichhold Chemicals, Inc.,
St. Helens, Oregon 30
2-8 Summary of Results of the CHEAP Scrubber Pressure
Drops at Reichhold Chemicals, Inc., St. Helens,
Oregon 32-33
2-9 Summary of the CHEAP Scrubber Liquor Analysis
Results at Reichhold Chemicals, Inc., St. Helens,
Oregon 35
2-10 Summary of Results of the Ambient Air Temperature
and Relative Humidity Measurements at Reichhold
Chemicals, Inc., St. Helens, Oregon 36-37
3-1 Average (Corrected) Prill Tower Production Rates
During Emissions Tests at Reichhold Chemicals,
Inc., St. Helens, Oregon 45
3-2 General Plant Process Operating Parameters
(4/15/80, Series A, Run 1) . 46
3-3 General Plant Process Operating Parameters
(4/16/80, Series A, Run 2) 47
3-4 General Plant Process Operating Parameters
(4/17/80, Series A, Run 3) 48
3-5 General Plant Process Operating Parameters
(4/18/80, Series B, Run 1) 49
3-6 General Plant Process Operating Parameters
(4/21/80, Series B, Run 2) 50
3-7 General Plant Process Operating Parameters
(4/22/80, Series B, Run 3) 51
3-8 Preconditioner Operating Parameters (4/15/80,
Series A, Run 1) 55
3-9 Preconditioner Operating Parameters (4/16/80,
Series A, Run 2) 56
3-10 Preconditioner Operating Parameters (4/17/80,
Series A, Run 3) 57
3-11 Preconditioner Operating Parameters (4/18/80,
Series B, Run 1) 58
3-12 Preconditioner Operating Parameters (4/21/80,
Series B, Run 2) 59
-viii-
-------
LIST OF TABLES (Continued)
TABLE PAGE
3-13 Preconditioner Operating Parameters (4/22/80,
Series B, Run 3) 60
3-14 CHEAP Operating Parameters (4/15/80, Series A,
Run 1). . 62
3-15 CHEAP Operating Parameters (4/16/80, Series A,
Run 2) 63
3-16 ' CHEAP Operating Parameters (4/17/80, Series A,
Run 3) 64
3-17 CHEAP Operating Parameters (4/18/80, Series B,
Run 1) 65
3-18 CHEAP Operating Parameters (4/21/80, Series B,
Run 2) 66
3-19 CHEAP Operating Parameters (4/22/80, Series B,
Run 3) 67
-ix-
-------
APPENDICES
A Urea and Ammonia Emission Test Results
A.I CHEAP Scrubber Downcomer
A.2 CHEAP Scrubber Outlet
A.2.1 Series A Test
A.2.2 Series B Test
A.3 Example Equations and Sample Calculations
B Pield Data Sheets and Sampling Task Logs for Urea and Ammonia Testing
B.I CHEAP Scrubber Downcomer
B.2 CHEAP Scrubber Outlet
B.2.1 Series A Test
B.2.2 Series B Test
C Visible Emissions Results
C.I Visible Emission Summary Tables
C.2 Visible Emissions Recertification Certificate
C.3 Visible Emissions Pield Data Sheets
C.3.1 Series A Test
C.3.2 Series B Test
C.3.3 Miscellaneous Observations Performed on April 23, 1980
D Particle Size Tests
D.I Discussion of Particle Size Testing
D.2 Particle Size Pield Data Sheets
D.3 Copy of Lab Weighing Data
E Miscellaneous Pield Data
E.I Scrubber Liquor
E.2 CHEAP Scrubber Pressure Drops
E.2.1 Series A Test
E.2.2 Series B Test
E.3 Ambient Air Temperature and Relative Humidity
E.3.1 Series A Test
E.3.2 Series B Test
-x-
-------
APPENDICES (Continued)
F Daily Summary Logs
F.I Daily Summary Logs
F.2 Field Laboratory Log and Moisture Data
G EPA Sampling and Analytical Procedures
G.I EPA Urea Method 28
G.2 Ammonia
H Analytical Data
H.I Summary of Analytical Results
H.2 Summary of Analytical Procedures
H.3 Discussion of Methods and Results
H.4 Sample Recovery and Preservation
H.5 Laboratory Notebook
I Sampling Train Calibration Data
I.I Orifice Calibrations
1.2 Nozzle Measurements
1.3 Pitot Tube Calibrations
J EPA Audit Samples Analysis Results
J.I Discussion of Audit Sample Analysis and Results
J.2 Audit Sample Analysis Data
K Cleanup Evaluation Results
K.I Discussion of Cleanup Evaluation, Analysis, and Results
K.2 Cleanup Evaluation Analysis Data
L Project Participants
M Scope of Work Data
M.I Work Assignment
M.2 Technical Directives
M.3 Associated Correspondence
-xi-
-------
1.0 INTRODUCTION
1.1 Overview
Section 111 of the Clean Air Act of 1970 charges the administrator of the
United States Environmental Protection Agency (EPA) with the responsibility of
establishing Federal Standards of Performance for New Stationary Sources
(SPNSS) which may significantly contribute to air pollution. When promulgat-
ed, these standards of performance for new stationary sources are to reflect
the degree of emissions limitation achievable through application of the best
demonstrated emission control technology. Emission data collected from
controlled sources in the particular industry of concern provide a portion of
the data base used by EPA to develop the SPNSS.
EPA's Office of Air Quality Planning and Standards (OAQPS) selected the
Reichhold Chemicals, Inc., urea manufacturing plant in St. Helens, Oregon as a
site for an emission test program. This plant produces fertilizer grade urea,
and is considered to employ process and emission control technology represen-
tative of modern urea solution formation and prilling processes. The urea
production rate at this plant is approximately 300 tons per day.
EPA engaged TRC to conduct tests designed to characterize and quantify
uncontrolled emissions from the solids production and cooling (prill tower)
processes, and to determine emission control equipment efficiencies. Emission
tests were performed in April 1980 on the inlet and outlet of the Cleanable
High Efficiency Air Filter (CHEAF) scrubber during production of fertilizer
grade urea. Figure 1-1 shows a flow diagram of the urea production process
and Figure 1-2 shows a schematic of the prill tower emission control system.
-1-
-------
Exhaust
Exhaust
I
NJ
Scrubber
NIU CO., Liquor
|J 1 Recycle
1
Anuionia Urea
c i ,1 Carbamate , , , Solution _ . .
Solution ^_ Solution ^_ Solul
Synthesis Decoiupo- Concc
sition tic
\ It
Ion
stra-
in
Carbdniate Recycle Urea Recycle
4
SOLUTION PROCESSES
(air emissions not shown)
CIIEAF
Scrubber
A
Urea
Crystals
Prilling
Moving
Bed
Scrubber
/
s
Urea
Prills
SOLID
1 FORMATION
Rotai
Drum
Cook
\
Bagying &
i »- Bag Shi|Miieni
•y
r
urea
Prills Warehouse
1 ^ Bulk
Storage
Bulk
*" Sht|Miient
SOLID FINISHING
(subject of
source
test)
FIGURE 1-1: GENERAL PLANT PRODUCTION PROCESS FLOW DIAGRAM
-------
PRILL
TOWER
EXHAUST
PRECONDITIONING
SYSTEM
*DETAILS OF
PRECONDITIONING
SYSTEM WITHHELD
AT REQUEST OF REICHHOLD
DOWNCOMER
SUMP
CHEAF SCRUBBER
— 1
I
\1
ENTRAPMENT
SEPERATOR
A
t
EXHAUST
STACK
FIGURE 1-2: DIAGRAM OF PRILL TOWER EMISSION CONTROL SYSTEM.
0988-004
-------
1.2 Brief Process Description
Urea is produced by combining ammonia and carbon dioxide in a reactor
under a pressure of 3,000 psi. Excess carbon dioxide and ammonia are boiled
off and returned to the reactor while the urea left in solution is crystal-
lized and dried. Urea crystals are conveyed to the top of the prill tower
where they are melted and sprayed downward against a counter current of ambi-
ent air drawn through the prill tower. The molten material separates into
small droplets and solidifies. At the bottom of the tower the solid prills
are screened and then conveyed to a bagging operation or to bulk storage.
Approximately 100,000 SCFM of air is drawn through the prill tower to cool
and dry the prills. This air is exhausted from the top of the tower and is
ducted down through a series of preconditioning sprays. The preconditioned
gas stream then enters the variable flow Cleanable High Efficiency Air Filter
(CHEAP) Scrubber. From the CHEAF the gas stream passes through an entrainment
separator and fan, and then exhausts to the atmosphere. The pressure drop
across the CHEAF and entrainment separator ranges from 10 to 19 inches water,
and is adjusted on a seasonal basis to maintain consistent product quality.
1.3 Emissions Measurement Program
The emissions measurement program was conducted from April 15 to April 23,
1980 at the Reichhold Chemicals, Inc., St. Helens, Oregon urea manufacturing
plant. The measurement program consisted of the following:
1. Urea and ammonia sampling in the inlet and outlet gas streams of the
CHEAF scrubber with preconditioning sprays off (test Series A).
These inlet and outlet emissions tests were run concurrently.
2. Urea and ammonia sampling in the outlet gas stream of the CHEAF
scrubber with the preconditioning sprays on (test Series B).
3. Visible emissions readings from the CHEAF scrubber outlet during both
test series.
-4-
-------
4. Pressure drop measurements across the CHEAF scrubber during both test
series.
5. Urea and solids content, temperature, and pH of the inlet and outlet
CHEAF scrubber liquor during both test series.
6. Ambient air temperature and relative humidity during both test series.
7. Particle size tests on the CHEAF downcomer (inlet) during Series A.
TRC personnel were responsible for collecting the above emissions data.
Concurrently, Radian was responsible for monitoring and recording pertinent
process operation parameters. The chronology of the emission tests is
contained in the Daily Summary Logs in Appendix F.
1.4 Description of Report Sections
The following sections of this report contain the Summary of Results
(Section 2.0), Process Description and Operation (Section 3.0), Location of
Sampling Points (Section 4.0), and Sampling and Analysis Methods (Section
5.0). Descriptions of methods and procedures, field and laboratory data, and
calculations are presented in the various appendices, as noted in the Table of
Contents.
Appendix K contains the results of the cleanup evaluations performed on
the sampling train equipment. The sampling train was assembled and charged as
if ready to perform a test for urea and ammonia. The unexposed impinger
contents were then recovered, prepared, and analyzed according to procedure in
order to establish background/contamination levels resulting from the sample
collection equipment.
Appendix J contains the results of audit sample analyses. Urea standards
were prepared by EPA and then analyzed by TRC in accordance with EPA instruc-
tions in order to assess the accuracy of the urea analysis procedure.
-5-
-------
2.0 SUMMARY OF RESULTS
This section presents summary tables of results and narrative on the emis-
sions testing conducted during the weeks of April 14-18 and April 21-25, 1980
at the Reichhold Chemicals, Inc. urea manufacturing facility in St. Helens,
Oregon. Testing was performed on gas and liquid streams entering and exiting
the Clean High Efficiency Air Filter (CHEAP) scrubber.
The program consisted of two test series: simultaneous inlet and outlet
emissions tests with the scrubber preconditioning sprays off (Series A) , and
outlet emissions tests with the preconditioning sprays on (Series B).
Urea concentrations were determined with the p-dimethylaminobenzaldehyde
colorimetric (with preliminary distillation) analysis method. The outlet urea
samples were analyzed in the field and at the TRC laboratory within 20 days.
Two methods of ammonia analysis were used throughout this testing program:
the direct nessler method and the specific ion electrode method. The specific
ion electrode analysis results are presented here as the primary ammonia
data. All three analysis methods are discussed in Section 5.0 and Appendices
G and H.
2.1 Comparison of CHEAP Scrubber Series A and Series B Outlet Emission Test
Results
The Series A and Series B comparison test results are shown in Table 2-1.
Table 2-la and 2-lb present the TRC laboratory analysis results. Table 2-lc
and 2-Id present the field analysis results. In Series A the preconditioning
sprays were off and in Series B the preconditioning sprays were on. For the
TRC laboratory analyses, the Series B urea concentrations (grams/DSCE) are 38%
less than the Series A urea concentrations. For the field analyses, the
Series B urea concentrations are 10% less than the Series A concentrations.
The difference between the Series A and Series B data is less for the field
-6-
-------
TABLE 2-la (English)
SUMMARY OF RESULTS OF UREA AND AMMONIA TESTS ON GASES EXITING
Run Number
Date
Secies
Volume of Gas Sampled (DSCF)a
Stack Gas Flow Rate (DSCFM)b
Stack Temperature <°F)
Percent Moisture
Percent Isokinetic
Production Hate (Tons/Hour)
Pressure Drop (Inches water)
Average Opacity (»)
Urea Datac
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Ammonia Data
Total Sample Weight (milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
THE CHEAF SCRUBBER (SERIES A & B) ON APRIL 15-22, 1980 AT
REICHHOLD CHEMICALS INC., ST. HELENS, OREGON
1
04-15-80
A
174.4
72910
99
4.81
100.6
12.2
14.7
0.1
NA*
1167
0.1032
64.51
5.29
4
04-18-80
B
248.9
82610
98
5.16
101.4
12.3
12.0
12.4
11.8
0.0007315
0.5179
0.0421
1196
0.1237
87.61
7.12
2
04-16-80
A
305.2
84200
97
4.98
101.7
12.1
12.1
6.2
16.6
0.0008392
0.6056
0.0050
2214
0.1119
80.77
6.68
5
04-21-80
B
249.5
85400
95
4.32
98.3
11.9
12.0
12.5
11.8
0.0007299
0.5342
0.0450
1591
0.09841
72.03
6.05
3
04-17-80
A
261.3
86590
96
5.06
101.5
12.1
12.2
14.5
21.6
0.001276
0.9467
0.0782
1517
0.08959
66.49
5.50
6
04-22-80
B
246.8
84210
97
4.74
98.6
12.5
12.0
10.8
12.4
0.0007753
0.5596
0.0448
1341
0.08385
60.52
4.84
Average
A
247
80903 c
97
4.74
101.3
12.1
13.0
6.9
19.1**
0.001193
0.8275
0.0641
1633
0.1020
70.59
5.82
B
248.4
^Bfft&tti
97
4.74
99.4
12.2
12.0
11.9
12.0
0.0007454
0.5371
0.0440
1643
0.1021
73.56
6.00
a Dry Standard Cubic Feet € 68°F, 29.92 Inches llg
b Dry Standard Cubic Feet Per Minute £ 68°F 29.92 Inches llg
c P-dimethylaminobenzaldehyde Colorimetric (with preliminary distillation) Analysis Method.
d Direct Nessler Analysis Method. Analyses performed at TRC.
* Not analyzed. Insufficient sample volume remained after field analysis.
"Urea data averages are based on total sample weights from Runs 2 and 3 only.
Analyses performed at TKC.
-------
TABLE 2-lb (Metric)
SUMMARY OF RESULTS OF UREA AND AMMONIA TESTS ON GASES EXITING
I
CD
Run Number
Date
Series
Volume of Gas Sampled (DNm3)3
Stack Gas Flow Rate (DNm3/mln)b
Stack Temperature (°C)
Percent Moisture
Percent Isokinetic
Production Rate (Mg/llour)
Pressure Drop (mm Hg)
Average Opacity (%)
Urea Datac
" Total Sample Weight (Milligrams)
Grams/Nm3
Kg/Hour
Kg/My
Ammonia Data*^
Total Sample Weight (Milligrams)
Grams/Nm3
Kg/Hour
Kg/Mg
TUB CHEAP SCRUBBER (SERIES A & B)
ON APRIL 15-22, 1980 AT
REIC1IIIOLD CHEMICALS INC., ST. HELENS, OREGON
1
04-15-80
A
4.940
2065
37
4.81
100.6
11.1
373
0.10
NA*
1167
0.2361
29.29
2.6
4
04-18-80
B
7.049
2340
37
5.165
101.4
11.2
305
12.4
11.8
0.001674
0.2349
0.0209
1996
0.2830
39.74
3.5
2
04-16-80
A
8.643
2385
36
4.98
101.7
11.0
307
6.2
16.6
0.001920
0.2747
0.0250
2214
0.256
36.64
3.3
5
04-21-80
B
7.066
2419
35
4.325
98.3
10.8
305
12.5
11.8
0.001670
0.2423
0.0224
1591
0.2252
32.67
3.0
3
04-17-80
A
7.400
2452
36
5.06
101.5
11.0
310
14.5
21.6
0.002920
0.4294
0.0390
1517
0.205
30.16
2.7
6
04-22-80
B
6.989
2385
36
4.744
98.6
11.3
305
10.8
12.4
0.001774
0.2536
0.0225
1341
0.1919
27.45
2.4
Average'
A
6.994
2304
36
4.95
101.3
11.0
330
6.9
19.1"
0.002730 0.
0.3754 0
0.0320 0
1633
0.2334 0
32.03
2.9
B
7.035
2291
36
4.745
99.4
11.1
305
11.9
12.0
001706
.2436
.0225
1643
.2336
33.29
3.0
a Dry Normal Cubic Meters g 20°C, 760 mm Hg
b Dry Normal Cubic Meters Per Minute g20°C, 760 mm Hg
c P-dimethylaminobenzaldehyde Colorimetric (with preliminary distillation) Analysis Method.
d Direct Nessler Analysis Method. Analyses performed at TRC.
* Not Analyzed. Insufficient sample volume remained after field analysis.
"Urea Data averages are based on total sample weights from Runs 2 and 3 only.
Analyses performed at TRC.
-------
TABLE 2-lc (English)
SUMMARY OF RESULTS OF UREA AND AMMONIA TESTS ON GASES EXITING
Run Number
Date
Series
Volume of Gas Sampled (DSCF)A
Stack Gas Flow Rate (DSCFM)B
Stack Gas Temperature (°F)
Percent Moisture
Percent Isokinetlc
Production Rate (Tons/Hour)
Pressure Drop (inches water)
Average Opacity (%)
Urea Datac
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Ammonia Data0
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
THE CHEAP SCRUBBER (SERIES A & B) ON APRIL 15-22, I960 AT
REICIUIOLD CHEMICALS INC., ST
1
04-15-80
A
174.4
72910
99
4.81
100.6
12.2
14.7
0.10
6.0
0.0005308
0.3317
0.0272
1089
0.0633
60.20
4.9
4
04-18-80
B
248.9
82610
98
5.16
101.4
12.3
12.0
- 12.4
11.9
0.0007377
0.5223
0.0425
2235
0.1386
98.10
8.00
2
04-16-80
A
305.2
84200
97
4.98
101.7
12.1
12.1
6.2
17.1
0.0008645
0.6239
0.0516
2358
0.1192
86.03
7.1
. HELENS, OREGON
5
04-21-80
B
249.5
85400
95
4.32
98.3
11.9
12.0
12.5
13.0
0.0008041
0.5886
0.0495
1654
0.1023
74.88
6.29
3
04-17-80
A
261.3
86590
96
5.06
101.5
12.1
12.2
14.5
20.3
0.001199
0.8899
0.0735
1579
0.09325
69.20
5.7
6
04-22-80
B
246.8
84210
97
4.74
98.6
12.5
12.0
10.8
14.6
0.0009129
0.6589
0.0527
1507
0.09423
68.01
5.44
Average
A
247.0
81230
97
4.74
101.3
12.1
13.0
6.9
14.5
0.000906 0
0.6152
0.0507
1675
0.1046
71.81
5.9
B
248.4
84070
97
4.74
99.4
12.2
12.0
11.9
13.1
.0008137
0.5863
0.0482
1799
0.1117
80.49
6.58
A Dry Standard Cubic Feet g 68°F, 29.92 inches Hg
B Dry Standard Cubic Feet Per Minute 9 68°F, 29.92 inches Hg
c P-dimethylaminobenzaldehyde Colorimetric (with preliminary distillation) Analysis Method. Analyses performed in the field.
D Specific Ion Electrode Method. Analyses performed in the field.
-------
TABLE 2-ld (Metric)
SUMMARY OF RESULTS OF UREA AND AMMONIA TESTS ON GASES EXITING
O
Run Number
Date
Series
Volume of Gas Sampled (DNra-*)A
Stack Gas Flow Hate (DNra3/min)B
Stack Gas Temperature (°C)
Percent Moisture
Percent Isokinetic
Production Rate (Mg/llour)
Pressure Drop (mm Hg)
Average Opacity (%)
Urea Datac
Total Sample Weight (Milligrams)
Granis/Nin^
Kg/Hour
Kg/Mg
Ammonia Data0
Total Sample Weight (Milligrams)
Grams/Nm^
Kg/Hour
Kg/Mg
THE CHEAP SCUUBBEU (SERIES A i B)
ON APRIL 15-22, 1980 AT
REICHIIOLD CHEMICALS INC., ST. HELENS, OREGON
1
04-15-80
A
4.94
2 065
37
4.81
100.6
11.1
373
0.10
6.0
0.00121
0.1506
0.0136
1167
0.2362
27.33
2.46
4
04-18-80
B
7.049
2340
37
5.165
101.4
11.2
305
12.4
11.9
0.001688
0.2369
0.0212
2235
0.3171
44.50
4.00
2
04-16-80
A
8.643
2385
36
4.98
101.7
11.0
307
6.2
17.1
0.00198
0.2832
0.0257
2214
0.2561
36.67
3.33
5
04-21-80
U
7.066
2419
35
4.325
98.3
10.8
305
12.5
13.0
0.001840
0.2670
0.0247
1654
0.2341
33.97
3.15
3
04-17-80
A
7.400
2452
36
5.06
101.5
11.0
310
14.5
20.30
0.00274
0.4036
0.0370
1517
0.0205
30.18
2.74
6
04-22-80
U
6.989
2385
36
4.744
98.6
11.3
305
10.8
14.6
0.002089
0.2989
0.0264
1507
0.2156
30.85
2.72
Average
A
6.994
2300
36
4.95
101.3
11.0
330
6.9
14.5
0.00207 0
0.2791
0.0254
1633
0.2335
31.39
2.84
U
7.035
2381
36
4.745
99.4
11.1
305
11.9
13.1
.001862
0.2659
0.0241
1799
0.2556
36.51
3.29
A Dry Normal Cubic Meters 8 20°C, 760 mm Hg
B Dry Normal Cubic Meters Per Minute @ 20°C, 760 mm llg
C P-dimethylaminobenzaldehyde Colorimetric (with preliminary distillation) Analysis Method.
u Specific Ion Electrode Analysis Method. Analyses performed in the field.
Analyses performed in the field.
-------
analyses due to the relatively small amount of urea collected during the first
test run of Series A. There is little difference between Series A and Series
B ammonia data.
Because of the relatively short sampling time used in test run 1 Series A
(320 minutes) , the amount of urea collected was too low to be measured by the
proposed EPA method. In order to detect the urea in this sample, a larger
aliquot was concentrated during the preliminary ammonia removal step. For the
subsequent test runs, the sampling time was extended to 400 minutes and the
concentration step was performed during the ammonia removal step.
The acid impinger urea analysis results were not added to the water
impinger results, in accordance with instructions from the Technical Manager.
No urea was detected in the outlet acid impingers; the average inlet acid
impinger urea results were about three percent of the inlet water impingers
results.
2.2 CHEAF Scrubber Emission Test Results
The Series A test results (inlet and outlet, with preconditioning sprays
off) are shown in Table 2-2. The average urea collection efficiency is 98.6
percent, and the average ammonia collection efficiency is less than zero
percent. This negative ammonia collection efficiency is probably due to
ammonia stripping from the liquor by the gas stream.
The Series A inlet and outlet data are presented separately in Tables 2-3
and 2-4, respectively.
The Series B test results (outlet only, with preconditioning sprays on)
are shown in Table 2-5.
-11-
-------
TABLE 2-2a (English)
SUMMARY OF RESULTS OF UREA AND AMMONIA TESTS
ON GASES ENTERING AND EXITING THE CHEAP SCRUBBER (SERIES A)
ON APRIL 15-17, 1980
AT REICIIHOLD CHEMICALS, INC., ST. HELENS, OREGON
Run Number
Date
Locat ion
Volume of Gas Sampled (DSCF»a
Stack tias Flow Rate (DSCFM)"
Stack Temperature (°F)
Percent Moisture
Percent Isokinetic
Production Rate (Tons/Hour)
Pressure Drop (inches water)
Average Opacity (%)
Urea Datac
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (Percent)
Ammonia Data**
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (Percent)
04-15-80
Inlet Outlet
04-16-80
Inlet Outlet
04-17-80
Inlet Outlet
14.7
0.1
730.0 6.0
0.07211 O.OOOS308
42.03 0.3317
3.5 0.0272
99.2
180.5
0.01783
10.39
0.87
1089
0.09633
60.20
4.9
12.1
6.2
83.00
0.01669
10.88
0.87
2358
0.1192
86.03
7.1
12.2
14.5
76.10
0.01510
10.24
0.86
1579
0.09325
69.20
5.7
Average
Inlet Outlet
156.2
68010
105
0.58
100.4
12.0
174.4
72910
99
4.81
100.6
12.2
76.75
76100
101
1.46
106.9
12.7
305.2
84200
97
4.98
101.7
12.1
77.78
79170
98
1.17
104.2
11.9
261.3
86590
96
5.06
101.5
12.1
103.6
74430
101
1.07
103.8
12.2
247.0
81230
97
4.95
101.3
12.1
13.0
6.9
232.0
0.04664
30.42
2.4
97.9
17.1
0.0008645
0.6239
0.0516
481.0
0.09542
64.75
5.4
98.6
20.3
0.001199
0.8899
0.0735
481.0
0.07165
45.71
3.8
98.6
14.5
0.000906
0.6152
0.0507
113.2
0.01685
10.75
0.87
1675
0.1046
71.81
5.9
<0
<0
<°
a Dry Standard Cubic Feet S 68°F, 29.92 inches Hg.
b Dry Standard Cubic Feet per minute.
c P-dimethylaminobenzaldehyde Colorimetric (with preliminary distillation) Analysis Method.
Inlet analyses performed at TRC. Outlet analyses performed in field.
d Specific Ion Electrode Analysis Method. Analyses performed in the field.
-------
TABLE 2-2b (Mettle)
SUMMARY OF RESULTS OF UREA AND AMMONIA TESTS
ON GASES ENTERING AND EXITING THE CHEAF SCRUBBER (SERIES A)
ON APRIL 15-17, 1980
AT REICIIIIOLD CHEMICALS, INC., ST. HELENS, OREGON
Run Number
Date
Location
Volume of Gas Sampled (Nm3)a
Stack Gas Flow Rate (Nm3/Min)b
Stack Temperature (°C)
Percent Moisture
Percent Isokinetic
Production Rate (Mg/Hour)
Pressure Drop (mm Hg)
Average Opacity (»)
Urea Datac
1
04-15-80
Inlet
4.424
1926
40
0.58
100.4
10.9
Outlet
4.940
2065
37
4.81
100.6
11.1
2
04-16-80
Inlet
2.174
2155
39
1.46
106.9
11.5
Outlet
8.643
2385
36
4.98
101.7
11.0
3
Average
04-17-80
Inlet
2.203
2242
37
1.17
104.2
10.8
- Outlet
7.400
2452
35
5.06
101.5
11.0
Inlet
2.934
2108
39
1.07
103.8
11.1
Outlet
6.994
2300
36
4.95
101.3
11.0
373
6.10
307
6.2
310
14.5
330
6.9
U)
I
Total Sample Height (Milligrams) 730.0 6.0 232.0 17.1 481.0 20.30 481.0 14.5
Grams/Nm3 0.1650 0.00121 0.1067 0.00198 0.2184 0.00274 0.1639 0.00207
Kg/Hour 19.08 0.1506 13.81 0.2832 29.40 0.4036 20.74 0.2791
Kg/Mg 1.8 0.0136 1.2 0.0257 2.7 0.0370 1.9 0.0254
Collection Efficiency (Percent) 99.2 97.9 98.6 98.6
Ammonia Data
Total Sample Weight (Milligrams) 180.5 1167 83.00 2214 76.10 1517 113.2 1633
Grains/Nm3 0.0408 0.2362 .0382 0.2561 ' 0.0346 0.0205 0.0379 0.2335
Kg/Hour 4.713 27.33 4.935 36.67 4.645 30.18 4.764 31.39
Kg/Ton 0.432 2.46 0.429 3.33 0.430 2.74 0.430 2.84
Collection Efficiency (Percent) <0 <0 <0 <0
a Normal Cubic Meters 9 20°C, 760 mm Hg.
h Normal Cubic Meters per minute.
c P-dimethylaminobenzaldehyde Colorimetric (with preliminary distillation) Analysis Method.
Inlet analyses performed at TRC. Outlet analyses performed in field.
" Specific Ion Electrode Analysis Method. Analyses performed in the field.
-------
TABLE 2-3
SUMMARY OF RESULTS OF OREft AND AMMONIA TESTS
ON GASES ENTERING THE CHEAP SCRUBBER (SERIES A)
ON APRIL 15-17, 1980
AT REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON
Run Number
Date
04-15-80
04-16-80
04-17-80
Average
Volume of Gas Sampled (DSCF)a
Stack Gas Flow Rate (DSCFM)b
Stack Temperature (°F)
Percent Moisture
Percent Isokinetic
Production Rate (Tons/Hour)
Urea Data0
156.2
68010
105
0.58
100.4
12.0
76.75
76100
101
1.46
106.9
12.7
77.78
79170
98
1.17
104.2
11.9
103.6
74430
101
1.07
103.8
12.2
Total Sample Weight (Milligrams) 730.0
Grains/USCF 0.07211
Pounds/Hour 42.03
Pounds/Ton 3.5
232.0
0.04664
30.42
2.4
481.0
0.09542
64.75
5.4
481.0
0.0716
45.71
3.8
Ammonia Data"
-P-
I
Total Sample Weight (Milligrams) 180.5
Grains/DSCF 0.01783
Pounds/Hour 10.39
Pounds/Ton 0.87
83.00
0.01669
10.88
0.87
76.10
0.0151
10.24
0.86
113.2
0.01685
10.75
0.87
a Dry Standard Cubic Feet § 68°F, 29.92 inches Hg.
b Dry Standard Cubic Feet per minute.
c P-dimethylaminobenzaldehyde Colorimetric (with preliminary distillation) Analysis Method.
Specific Ion Electrode Analysis Method. Analyses performed in the field.
Analyses performed at THC.
-------
TABLE 2-4
SUMMARY OF RESULTS OF UREA AND AMMONIA TESTS
ON GASES EXITING THE CHEAP SCRUBBER (SERIES A)
ON APRIL 15-17. 1980
AT REICIIIIOLO CHEMICALS, INC., ST. HELENS, OREGON
Run Number
Date
Volume of Gas Sampled (DSCF)a
Stack Gas Flow Rate (DSCFM)°
Stack Temperature (°F)
Percent Moisture
Percent Isokinetic
Production Rate (Tons/Hour)
Urea Datac
Total Sample Hieght (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton'
Ammonia Data
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
1
04-15-80
174.4
72910
99
4.81
100.6
12.2
TRC
NA*
DN°
1167
0.0132
64.51
5.29
FIELD
6.0
0.0005308
0.3317
0.0272
SIEe
1089
0.09633
60.20
4.93
04-16-80
305.2
84200
97
4.98
101.7
12.1
TRC
FIELD
16.6 17.1
0.0008392 0.0008645
0.6056 0.6239
0.0500 0.0516
DN
2214
0.1119
80.77
6.68
SIE
2358
0.1192
86.03
7.11
04-17-80
261.3
86590
96
5.06
101.5
12.1
TRC
21.6
0.001276
0.9467
0.0782
DN
1517
0.08959
66.49
5.50
FIELD
20.3
0.001199
0.8897
0.0735
SIE
1579
0.09325
69.20
5.72
Average
247
81230
97
4.95
101.3
12.1
TRC"
19.1
0.001193
0.8275
0.0641
DN
1163
0.102
70.59
5.82
FIELD
14.5
0.000906
0.6152
0.0507
SIE
1675
0.1046
71.81
5.92
a Dry Standard.Cubic Feet e 68°F, 29.92 inches llg.
" Dry Standard Cubic Feet per minute.
c P-dimethylaminobenzaldehyde Colorimetric (with preliminary distillation) Analysis Method.
Analysis done in the field and at TRC.
d Direct Nessler Analysis Method. Analyses performed at TRC.
e Specific Ion Electrode Analysis Method. Analyses performed in the field.
* Not analyzed: Insufficient sample volume remaining after field analysis. (See Section 2.1)
'•Urea data averages are based on total sample weights from Runs 2 and 3 only.
-------
TABLE 2-5
SUMMARY OF RESULTS OF UREA AND AMMONIA TESTS
ON GASES EXITING TUB CHEAP SCRUBBER (SERIES B)
CT>
I
ON APRIL 18-22,
AT REICIII10LD CHEMICALS, INC.,
Run Number
Date
Volume of Gas Sampled (DSCF)a
Stack Gas Flow Rate (DSCFM)°
Stack Temperature (°F)
Percent Moisture
Percent Isokinetlc
Production Rate (Tons/Hour)
Pressure Drop (Inches water)
Average Opacity (%)
Urea Datac
Total Sample Height (Milligrams)
Grains/DSCF
Pounds/Hour
rounds/Ton
Ammonia Data
Total Sample Height (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
4
04-18-80
248.9
82610
98
5.16
101.4
12.3
12.0
12.4
TRC
11.8
0.0007315
0.5179
0.0421
ON"3
1996
0.1237
87.61
7.12
5
04-21-80
249.5
85400
95
4.32
98.3
11.9
12.0
12.5
FIELD TRC
11.9 11.8
0.0007377 0.0007299
0.5223 0.5342
0.0425 0 0450
SIEe DN
2235 1591
0.1386 0.09841
98.10 72.03
8.00 6.05
1980
ST. HELEN:
FIELD
13.0
0.0008041
0.5886
0 0495
SIE
1654
0.1023
74.88
6.29
6
04-22-80
246.8
84210
97
4.74
98.6
12.5
12.10
10.8
TRC
12.4
0.0007753
0.5596
0.0448
DN
1341
0.08385
60.52
4.84
FIELD
14.6
0.0009129
0.6589
0.0527
SIE
1507
0.09423
68.01
5.44
Average
248.4
84070
97
4.75
99.4
12.2
12.0
11.9
TRC
12.0
0.0007454
0.5371
0.0440
DN
1643
0.1021
73.56
6.00
FIELD
13.1
0.0008137
0.5863
0.0482
SIE
1799
0.1117
80.49
6.58
a Dry Standard Cubic Feet e 68°F, 29.92 inches Hg.
Dry Standard Cubic Feet per minute.
c P-dimethylaminobenzaldehyde Colorimetric (with preliminary distillation) Analysis Method.
Analysis done in the field and at TRC.
d Direct Nessler Analysis Method. Analyses performed at TRC.
e Specific Ion Electrode Analysis Method. Analyses performed in the field.
* Not analyzed; Sample volume too low after field analysis. (See Section 2.1)
-------
2.3 Visible Emissions
The opacity of the plume from the CHEAP scrubber outlet was monitored dur-
ing both the Series A tests and the Series B tests. Observations were made by
a certified smoke observer from atop an ammonium nitrate tank and from ground
level.
The white plume exiting the outlet stack was observed against green trees
that were on the side of a mountain. During Series A tests (April 15-17,
1980), the 6-minute average opacities ranged from 3% to 27%. During Series B
tests (April 18-22, 1980) the 6-minute average opacities ranged from 3% to
28%. These data are shown graphically in Figures 2-1 through 2-5. Figures
2-1 and 2-2 refer to Series A; Figures 2-3 and 2-4 refer to Series B. Table
2-6 presents a summary of .the 6-minute arithmetic average opacity readings
from both Series A and Series B. An additional day of observations were made
on April 23, 1980. These observations were taken under several CHEAF scrubber
operating conditions as monitored by Reichhold personnel. These operating
conditions were as follows:
Period of Observation Scrubber Condition
30 minutes baffle open; preconditioning sprays on
30 minutes baffle open; preconditioning sprays off
30 minutes " baffle closed; preconditioning sprays off
30 minutes baffle closed; preconditioning sprays on
The opacity readings obtained from these test's are shown graphically in
Figure 2-5. All visible emissions data are contained in Appendix C.
2.4 Particle Size Tests
Particle size distribution tests were performed on the inlet gas stream of
the CHEAF scrubber during the Series A emission tests. The particle size tests
were performed with a Sierra Series 226 impactor with cyclone preseparator at
-17-
-------
00
11
10
9
§»
CJ
Of
LU
~ 7
2 6
o
LU
CD
a: 5
LU
-------
25
20
o
a:
15
D-
O
C3
00
LU
( — t
o:
LU
to
10
IS1
_T
1100
1200
1300
1400
1500
1600
1700
1800
04-17-80
OBSERVATION TIMES
FIGURE 2-2: SIX MINUTE AVERAGES OF APRIL 17,1980. OPACITY READINGS ON THE CHEAF SCRUBBER STACK.
REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON.
0988-010
-------
to
o
I
20
a:
ui
a.
a.
o
C3
15
£ 10
ca
a;
LU
to
0
0900
h-
i
1000
1100
04-18-80-
1200
1000
1100
1200
•04-21-80
1300
1400
TIME^HOURS
FIGURE 2-3: SIX MINUTE AVERAGES OF APRIL 18-21, 1980. OPACITY READINGS ON THE CHEAF SCRUBBER STACK.
REICHHOLD CHEMICALS, INC., ST. HELENS,OREGON.
0988-011
-------
I
NJ
25
20
o
CXL
O
O.
o
Cfl
CO
to
LU
l— i
a:
LU
to
15
10
0800
V
Jl
Jl
~\\
0900
1000
1100 1200
04-22-80
1300
1400
1500
—H
TIME HOURS
FIGURE 2-4: SIX MINUTE AVERAGES OF APRIL 22, 1980. OPACITY READINGS ON THE CHEAF SCRUBBER STACK.
REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON.
0988-012
-------
NJ
KJ
I
30
25
o
LU
O.
>- 20
D-
O
e>
§ 15
CO
CO
co
10
j
I
0900
1000
1300
1400
1100 1200
- 04-23-80 -
TIME~HOURS
FIGURE 2-5: SIX MINUTE AVERAGES OF APRIL 23, 1980. OPACITY READINGS ON THE CHEAF SCRUBBER STACK-
REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON.
0988-013
-------
TABLE 2-6
SIX MINUTE ARITHMETIC AVERAGE OPACITY READINGS
ON THE CHEAP SCRUBBER OUTLET AT
REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON
Six-Minute
Test Date Time Period
1 04-15-80 1543
Series A 1549
1555
1601
1607
1613
1619
1625
1631
1637
1645
1651
1657
1703
1709
1715
1721
1727
1733
1739
2 4-16-80 0925
Series A 0931
0937
0943
0949
0955
1001
1007
1013
1019
1034
1040
1046
1052
1058
1104
1548
1554
1600
1606
1612
1618
1624
1630
1636
1642
1650
1656
1702
1708
1714
1720
1726
1732
1738
1744
0930
0936
0942
0948
0954
1000
1006
1012
1018
1024
1039
1045
1051
1057
1103
1109
Average
Opacity
0
0.4
0.2
0.4
0
0
0.2
0.2
0.2
0.2
0
0
0
0
0
0.2
0.2
0
0.2
0
9.2
11.7
11.9
6.3
5.6
5.0
4.4
2.5
3.8
4.0
3.5
3.3
7.1
8.5
6.5
7.5
-23-
-------
TABLE 2-6 (Continued)
SIX MINUTE ARITHMETIC AVERAGE OPACITY READINGS
ON THE CHEAP SCRUBBER OUTLET AT
REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON
Six-Minute
Test Date Time Period
2 1110
Series A 1116
(Cont.) 1122
1128
1158
1204
1210
1216
1248
1254
1300
1306
1312
1318
1324
3 04-17-80 1104
Series A 1110
1116
1122
1128
1134
1140
1146
1152
1158
1205
1211
1217
1253
1259
1305
1311
1317
1323
1329
1115
1121
1127
1133
1203
1209
1215
1220
1253
1259
1305
1311
1317
1323
1325
1109
1115
1121
1127
1133
1139
1145
1151
1157
1203
1210
1216
1223
1258
1304
1310
1316
1322
1328
1334
Average
Opacity
7.7
4.4
7.9
9.2
3.8
3.5
6.0
5.3
4.0
5.0
4.6
7.7
6.7
8.8
6.4
9.6
9.2
8.1
6.9
7.5
6.3
6.3
4.6
7.9
8.8
7.1
7.1
9.6
11.5
9.0
6.5
9.2
11.7
13.8
15.5
-24-
-------
TABLE 2-6 (Continued)
SIX MINUTE ARITHMETIC AVERAGE OPACITY READINGS
ON THE CHEAP SCRUBBER OUTLET AT
REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON
Six-Minute
Test Date Time Period
3 - 1340
Series A 1346
(Cont.) 1352
1358
1404
1410
1416
1422
1428
1434
1541
1547
1553
1559
1605
1610
1617
1623
1629
1 04-18-80 0900
Series B 0906
0912
0918
0924
0930
0936
0942
0948
0954
1010
1016
1022
1028
1034
1040
1046
1052
1058
1104
1345
1351
1357
1403
1409
1415
1421
1427
1433
1439
1546
1552
1558
1604
1609
1613
1622
1628
1631
0905
0911
0917
0923
0929
0935
0941
0947
0953
0959
1015
1021
1027
1033
1039
1045
1051
1057
1103
1109
Average
Opacity
14.4
11.0
19.6
32.9
10.0
10.8
11.0
11.9
12.9
11.7
16.3
17.1
27.1
20.8
13.8
5.4
9.8
6.5
5.8
— —
—
—
—
—
—
— —
12.8
11.5
14.0
13.1
10.8
17.9
12.7
11.9
12.3
19.4
11.3
11.0
12.9
-25-
-------
TABLE 2-6 (Continued)
SIX MINUTE ARITHMETIC AVERAGE OPACITY READINGS
ON THE CHEAP SCRUBBER OUTLET AT
REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON
Six-Minute
Test Date Time Period
1 1115
Series B 1121
(Cent.) 1127
1133
1139
1145
1151
1157
1203
1209
2 4-21-80 1005
1011
1017
1023
1029
1035
1041
1047
1053
1059
1120
1126
1132
1138
1144
1150
1156
1202
1208
1214
s
3 04-22-80 0845
Series B 0851
0857
0903
0909
0915
0921
0927
1120
1126
1132
1138
1144
1150
1156
1202
1208
1214
1110
1016
1022
1028
1034
1040
1046
1052
1058
1104
1125
1131
1137
1143
1149
1155
1201
1207
1213
1219
0850
0856
0902
0908
0914
0920
0926
0932
Average
Opacity
10.8
9.0
9.2
12.1
11.7
9.6
10.0
13.8
13.3
14.8
13.5
12.5
17.9
16.5
12.3
13.8
8.8
13.8
12.7
9.6
11.5
9.17
15.4
10.0
8.8
14.0
9.8
12.5
12.1
14.6
23.7
26.9
21.9
19.0
23.3
13.5
14.2
12.1
-26-
-------
TABLE 2-6 (Continued)
SIX MINUTE ARITHMETIC AVERAGE OPACITY READINGS
ON THE CHEAP SCRUBBER OUTLET AT
REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON
Six-Minute
Test Date Time Period
3 0933
Series B 0939
(Cont.)
1010
1016
1022
1028
1034
1040
1046
1052
1058
1104
1110
1128
1134
1140
1146
1152
1158
1204
1210
1216
1222
1300
1306
1312
1318
1324
1330
1426
1432
1438
1444
04-23-80 0920
0926
0932
0938
0944
1015
1021
1027
1033
1039
1045
1051
1057
1103
1109
1115
1133
1139
1145
1151
1157
1203
1209
1215
1221
1227
1305
1311
1317
1323
1329
1335
1431
1437
1443
1447
0925
0931
0937
Average
Opacity
13.3
14.2
12.3
13.1
5.8
10.0
15.0
12.3
10.0
8.0
4.2
5.7
7.6
9.5
11.1
9.8
5.0
6.1
5.2
6.1
2.5
5.3
10.0
5.0
13.1
9.0
6.5
4.4
4.8
6.1
5.0
7.7
12.0
13.1
19.0
18.1
-27-
-------
TABLE 2-6 (Continued)
SIX MINUTE ARITHMETIC AVERAGE OPACITY READINGS
ON THE CHEAP SCRUBBER OUTLET AT
REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON
Six-Minute
Test Date Time Period
3 0938
Series B 0944
(Cont.)
0955
1001
1007
1013
1019
1036
1042
1048
1054
1100
1110
1116
1122
1128
1134
0943
0949
1000
1006
1012
1018
1024
1041
1047
1053
1059
1105
1115
1121
1127
1133
1139
Average
Opacity
26.0
27.9
31.3
29.8
18.8
16.9
19.0
14.8
11.3
11.7
11.0
15.8
23.1
23.2
24.4
18.8
12.3
-28-
-------
a single average flow point in the inlet duct. r
The results for Series A are summarized in Table 2-7 and and are shown
as a cumulative size distribution curve in Figure 2-6.
All particle size field and laboratory data are contained in Appendix D.
2.5 Pressure Drops Across the CHEAP Scrubber
The pressure drop measurements were made on the CHEAF scrubber using a
vertical U-tube water manometer connected to pressure taps across the throat
of the scrubber. The pressure drops were recorded approximately every 60
minutes during the emission test periods (Series A and B). Table 2-8 shows
the time and pressure drop (inches of water) for each test. During Test No.
1 (Series A) the pressure drop averaged 14.7 inches of H-0. Throughout
the remaining five tests, the pressure drops remained at approximately 12
inches of water. The pressure drop reduction after the first test
represented a normal process operations adjustment for existing ambient
conditions.
2.6 Analysis of Scrubber Liquor
The scrubbing liquor entering and exiting the CHEAF scrubber was sampled
approximately every hour during both Series A and B emission test runs.
During Series A and B, TRC personnel collected aliquots from the combined
lower sprays from solution formation and Downcomer sump, and from the CHEAF
sump. During Series B, Reichhold Chemical personnel collected aliquots from
the combined sprays from strippers and middle sprays from crystallizer and
from the scrubber bottom and hot well to sump.
-29-
-------
TABLE 2-7
SUMMARY OF RESULTS OF THE
CHEAP DOWNCOMER PARTICLE SIZE TESTS
AT REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON
I
LO
o
Participate
Test Test Concentration Aerodynamic Size
Run No. Date Time Grains/DSCF Range, (Pm)
1 04-16-80 1513-1520 0.069 >3.8
1.71-2.81
1.08-1.71
0.58-1.08
<0.58
2 04-17-80 0844-0904 0.053 >6.4
2.22-3.64
1.41-2.22
0.76-1.41
<0.76
3 04-17-80 1357-1411 0.050 >14.0
5.15-13.00
3.15-5.15
2.01-3.15
1.10-2.01
<1.10
Mass In
Size Range (%)
80.0
5.8
8.8
4.1
1.3
67.1
2.3
8.2
10.2
12.2
66.8
0.8
2.3
5.6
9.2
15.3
Cumulative
(Percent)
20.0
14.2
5.4
1.3
32.9
30.6
22.4
12.2
33.2
32.4
30.1
24.5
15.3
-------
10.0
9
8
7
6
4
3
/
<
Q
U 1.0
I 8
5 7
§ 6
LU
< 5
2%
10 20 30 40 50 60 70 80 85 90
PERCENTAGE OF MASS ^ CORRESPONDING SIZE
95
98%
CHEAP DOWNCOMER LEGEND
®—TEST #1 4/16/80
—* TEST #2 4/17/80
X * TEST #3 4/17/80
FIGURE 2-6: CUMULATIVE SIZE DISTRIBUTIONS OF PARTICULATE IN THE CHEAF DOWNCOMER
STACK AT ST. HELENS, OREGON.
-31-
0988-007
-------
TABLE 2-8
SUMMARY OF THE- CHEAP SCRUBBER
PRESSURE DROPS AT REICHHOLD CHEMICALS, INC.,
ST. HELENS, OREGON
SERIES A
Pressure Drop
Run No. Date Time (Inches Water)
1250 15.0
1310 14.7
1316 14.8
1330 14.7
1410 14.7
1440 14.5
1515 14.6
1535 14.7
1615 14.7
1645 14.7
1715 14.7
Average 14.7
04-16-80 0930 12.0
1000 12.3
1030 12.2
1100 12.1
1130 12.3
1200 12.1
1300 12.2
1330 12.1
1400 12.3
1430 12.2
1500 12.2
1530 12.2
1600 12.2
1630 12.0
1700 12.0
1730 12.0
' 1800 12.0
Average 12.1
04-17-80 0830 12.2
0930 12.3
1030 12.3
1130 12.3
1230 12.2
1330 12.2
1430 12.2
1530 , 12.2
Average 12.2
-32-
-------
TABLE 2-8 (Continued)
SUMMARY OP THE CHEAF SCRUBBER
PRESSURE DROPS AT REICHHOLD CHEMICALS, INC.,
ST. HELENS, OREGON
SERIES B
Pressure Drop
Run No. Date Time (Inches Water)
0830 12.0
0930 12.1
1030 12.1
1130 12.0
1230 11.9
1330 12.1
1430 11.9
1530 11.9
Average 12.0
04-21-80 0900 12.0
1000 11.9
1100 11.9
1200 12.0
1300 12.0
1400 12.0
1500 12.1
Average 12.0
04-22-80 0830 12.4
0930 11.8
1030 12.3*
1130 12.0
1230 12.0
1330 11.9
1430 11.9
1530 11.8
Average 12.0
CHEAF pressure was adjusted at 1000 from 11.6 to 12.5 inches water.
-33-
-------
The results of the urea and undissolved solids analyses of the TRC-col-
lected samples and the Reichhold-collected scrubber-bottom and hot-well-to-
sump samples are shown in Table 2-9 for Series A and B. The Series B average
urea and undissolved solids concentrations for the Downcomer sump and CHEAP
sump are higher than those of Series A due to the fact that during Series B
the preconditioning sprays were on and during Series A the sprays were off.
As noted in Section 2.1, the scrubber outlet gas stream urea concentrations
for Series B were lower than those for Series A. This shows that some of the
urea is picked up by the preconditioning sprays. The temperature and pH data
for each individual scrubber liquor sample are shown in Appendix E.
2.7 Ambient Air Temperature and Relative Humidity Measurements
The temperature and relative humidity of the ambient air were measured
approximately every half hour at the base of the CHEAF scrubber during the
Series A and B emission test runs. These data are presented in Table 2-10.
The individual temperature data as recorded are contained in Appendix E.
-34-
-------
TABLE 2-9
SUMMARY OF THE CHEAP SCRUBBER LIQUOR ANALYSIS
RESULTS AT REICIIIIOLD CHEMICALS, INC.,
ST. HELENS, OREGON
Ul
I
Series A
Run Number
Sampling Location:
Urea (ppra)
Undissolved Solids (mg/1)
Average Temperature (°F)
Average pH
Series B
Run Number:
Sampling Location:
Urea (ppm)
Undissolved Solids(mg/l) 129.0
Average Temperature (°F) 134
Average pH
Average
Downconter CHEAF
Sump Sump
85,000 114,000
151.4 65.4
130 92
9.00 8.67
1
Downcomer CHEAP Scrubber
Sump Sump Bottom
127,000 136,000 95.7
129.0 89.8 1.0
134 91 nm*
8.97 8.62 nm
Downcome r
Sump
89,000
62.1
137
9.21
Downcome r
Sump
133,000
117.9
128
8.97
CHEAF
Sump
108,000
54.6
91
8.80
2
CHEAF
Sump
141,000
81.4
88
8.64
Downcomer
Sump
130,000
67.6
139
9.18
Downcome r
Sump
138,000
168.0
134
9.19
CHEAP
Sump
128,000
49.4
89
8.79
3
CHEAP Hot
Sump To
138,000 1
Downcomer CHEAF
Sump Sump
101,300 116,700
93.7 56.5
135 91
9.13 8.75
Average
Well Downcomer CHEAP
Sump Sump Sump
,740 132,700 138,300
188.9 99.9 138.3 120.0
90
8.77
nm 133 90
nm 9.04 8.68
Not measured.
-------
TABLE 2-10
SUMMARY OF THE AMBIENT AIR TEMPERATURE
AND RELATIVE HUMIDITY MEASUREMENTS AT REICHHOLD CHEMICALS, INC.,
ST. HELENS, OREGON
SERIES A
Run No.
Date
04-15-80
04-16-80
04-17-80
Time
1250
1316
1440
1535
1615
1645
Average
1000
1030
1100
1130
1200
1300
1330
1440
1430
1500
1530
1600
1630
1700
1730
1800
Average
0830
0930
1030
1130
1230
1330
1430
1530
Wet Bulb
(°F)
49
47
52
49
52
50
50
51
51
52
54
55
57
57
57
57
57
58
58
58
58
56
55
56
51
51
51
54
57
59
57
57
Dry Bulb
(°F)
59
58
63
63
65
62
62
59
61
61
64
66
68
72
72
71
72
72
72
76
69
66
63
67
56
60
60
64
68
69
66
67
Average
55
64
Relative Humidity
47
46
46
33
39
41
42
57
49
54
51
48
50
38
38
41
38
42
42
48
51
53
60
48
71
53
53
51
50
55
57
53
55
-36-
-------
TABLE 2-10 (Continued)
SUMMARY OF THE AMBIENT AIR TEMPERATURE
AND RELATIVE HUMIDITY MEASUREMENTS AT REICHHOLD CHEMICALS, INC.,
ST. HELENS, OREGON
SERIES B
Run No.
Date
04-18-80
04-21-80
04-22-80
Time
0830
0930
1030
1130
1230
1330
1430
1530
Average
0900
1000
1100
1200
1300
1400
1500
Average
0830
0930
1030
1130
1230
1330
1430
1530
Wet Bulb
<°F)
51
51
51
54
57
59
57
57
55
50
48
52
53
53
51
53
51
51
51
53
54
56
56
56
56
Dry Bulb
(°F)
56
60
60
64
68
69
66
67
67
55 "
57
61
60
64
63
63
60
56
56
59
63
65
66
67
66
Average
54
62
Relative Humidity
71
53
53
51
50
55
57
53
55
70
50
54
63
47
42
50
54
71
71
67
55
56
53
49
53
59
-37-
-------
3.0 PROCESS DESCRIPTION AND OPERATION
This section discusses the urea production process and prill tower emis-
sion control system at the Reichhold Chemical Inc. urea manufacturing plant in
St. Helens, Oregon. Emission measurements were made at this plant on April
24-28, 1980 in order to obtain data necessary for the development of a new
source performance standard for the urea manufacturing industry. This plant
is considered to employ process and emission control technology representative
of modern urea solution formation and prilling processes.
The purpose of the emissions testing was to characterize and quantify
uncontrolled and controlled emissions from the nonfluidized bed prill tower
process. During the emissions tests, process parameters pertinent to the
operation of the prill tower were monitored in order to characterize the oper-
ation of the urea production process and emission control system, and to en-
sure that the plant was operating at representative conditions.
3.1 Urea Production Process Description
A flow diagram of the urea production process is presented in Figure 3-1.
The reaction section of the plant is a modified Chemico design. Urea solution
is produced by reacting liquid ammonia (NH-) with carbon dioxide (CO-) at
an elevated temperature and pressure. The reaction is exothermic and results
in the formation of liquid ammonium carbamate (NH_ C0_ NHJ. The liquid
ammonium carbamate is subsequently decomposed to urea (CO(NH2>2) and
water. The resulting solution of urea in water is concentrated by a crystal-
lization process. The urea crystals are then dried of free water by a centri-
fuge followed by a rotary drum dryer.
The dry urea crystals (consisting of greater than 99.5 percent urea) are
conveyed via elevator to the top of the prill tower. They are subsequently
-38-
-------
Exhaust
Exhaust
Nil., C02
* I 1
I Aninonla
.... Carbania
Solution
Synthesis
f
te
"~ Oecompo-
sition
T
Scrubber
Liquor
Recycle
Urea
Solution
Solution
Concentra-
tion
||
CHEAP
Scrubber
Urea
Crystals
Carbamate Recycle Urea Recycle
SOLUTION PROCESSES
(air emissions not shown)
• ^—
/\
\
Prilling
||
Huvlny
lied
Scrubber
/
Urea
Prills
*-
SOLID
1 FORMAT ION
\
Bagging ft
i ^— Bag Slti|MK
Rotary
Drum
Cooler
Urea
Prills Warehouse
*" Bulk
Storage
Bulk
ShlpuM-nt
SOLID FINISHING
(subject of
source
test)
FIGURE 3-1: GENERAL PLANT PRODUCTION PROCESS FLOW DIAGRAM
-------
melted in two steam-jacketed crystal melters. Each melter feeds four multiple
stream spray heads. Plugging of the spray heads is a common problem and
requires their removal and cleaning at frequent intervals.
The molten urea falls through the prill tower against a countercurrent
airstream. During the fall the melt solidifies into a hard, spherical prill.
After striking the floor of the tower, the prills are raked through two slots
and are then directed onto a vibrating screen. Fines and oversizes are
removed and sent to be dissolved in a UAN blending tank.
Conveyors transfer the properly sized prills across an adjacent warehouse
to a rotary drum cooler. Here the prills are cooled to a temperature suitable
for bulk storage. From the cooler, conveyors transfer the prills into one of
two connected warehouses where the prills are dumped into large bulk storage
piles.
When a shipment is needed, a front-end loader is used to move the prills
from the bulk storage piles onto a conveyor. The conveyor then dumps the urea
into railroad cars or trucks, or may supply the bagging operations. All prill
loading and bagging takes place in a separate building next to' the bulk stor-
age warehouses.
3.2 Prill Tower Emission Control System Description
A general flow diagram of the emission control system used on the prill
tower is shown in Figure 3-2. The two major components in the system are the
Downcomer and the Cleanable High Efficiency Air Filter (CHEAF) scrubber
system. Instrumentation indicated in Figure 3-2 is identified and described
in subsection 3.3.2, Emission Control System Monitoring.
The prill tower air flow exhausts through four horizontal exhaust ports
located near the top of the tower. The ductwork converges to a single
-40-
-------
rr M i —
Tower
Exhaust
Preconditioning*
System •»
A A
AA
*Details of
Preconditioning
System withheld
at request of
Reichhold
Down comer
Sump
I
/A /TV
/ r
A
f
:LA / '. \
/\ Instrumentation on Downcomer
C j Instrumentation on CHEAF
DOWNCCMER
A
^
1 CHEAF SCRUBBER
\ / s~^.
\ / 111
/r~^~\tf~ \y~
• N/ ^
Filter Entrainment N^.
^^| *^ Section Separator ^
(*) /\
©
i i
** nirflr
1 "^
^ — s
1
i
\;
^j
NS/Q
>
Exhaust
Stack
FIGURE 3-2: DIAGRAM OF PRILL TOWER EMISSION CONTROL SYSTEM
-------
self-supporting Downcomer. Preconditioning sprays are located at various
points on the Downcomer and a sump is located at the base of the Downcomer to
catch and recycle preconditioning liquor. Mist entrained in the Downcomer is
carried over to the scrubber. The preconditioning system's primary purpose,
according to plant personnel, is to enhance agglomeration of fine particulate
and thus reduce opacity at the scrubber outlet. Details of the precondition-
ing system are considered proprietary by company personnel.
The Series A emissions tests (April 14, 15, 16, 1980) were conducted using
only partial preconditioning. The Series B tests (April 18, 21, 22, 1980)
were conducted using full preconditioning (as the plant normally operates).
A horizontal takeoff ducts the airflow from the Downcomer to the CHEAP
inlet. A general diagram of the CHEAP scrubber is shown in Figure 3-3. The
actual scrubber installed at Reichhold differs somewhat from this diagram,
particularly in the filter drum area.
©
The scrubber utilizes a reticulated Teflon mat installed over a perfor-
ated drum. Gases pass from the exterior of the drum, through the wetted
filter and into a mist eliminator section. The filter drum rotates slowly and
is irrigated by spray nozzles located throughout the drum chamber. The
demister housing is a horizontal cylinder with an inclined demister element
located near the scrubber exit.
The CHEAP design allows the pressure drop to be adjusted while the unit is
in operation. This adjustment is accomplished by moving a baffle plate to
cover a portion of the filter drum. The entire airflow then must travel
through a smaller section of the filter at higher velocity. This increases
particulate removal at the expense of a higher pressure drop.
Flow through the entire prill tower-scrubber system is induced with a 400
hp centrifugal fan mounted concentrically with the demister section. Air
exiting the fan is fed into a carbon steel outlet stack approximately 85 feet
tall.
-42-
-------
mist Eliminator
Rotating Perforated Filtration Drum
Liquor
Sprays
Figure 3-3. Diagram of CIIEAF Scrubber
-------
All urea collected in the scrubber is recycled back to the crystallizers
via the Downcomer sump. A return line exists between the scrubber sump and
the Downcomer sump to prevent overflow of the scrubber sump.
3.3 Monitoring of Plant Processes During Emissions Tests
3.3.1 Urea Production Process Monitoring
The urea production process was monitored during the emissions tests for
the following reasons:
1. to insure the prill tower was operating at or near capacity throughout
the tests;
2. to insure the plant was operating within normal day-to-day .tolerances;
3. to record production data to be used in determining emission factors
(pounds emitted/tons of production) ; and
4. to provide a data base to assist EPA in characterizing normal plant
operating conditions.
Data concerning the preconditioning system is considered confidential by
Reichhold. This data is reported as standardized values. The standardized
value is defined as:
X - X
sv
X X
avg avg
where x = actual data value, and x = average value for the data set.
0 vy
Averages for each data set are contained in confidential files.*
Nine plant operating parameters were monitored during the emissions
tests. Tables 3-1 through 3-7 are a compilation of these data. Each para-
meter is described in the following list:
*See Confidential Addendum, Contact Eric Noble, EPA (919) 541-5213.
-44-
-------
TABLE 3-1
AVERAGE (CORRECTED) PRILL TOWER PRODUCTION RATES
DURING EMISSIONS TESTS AT
REICHHOLD CHEMICALS, INC., ST. HELENS, OREGON
Test
Downcomer Inlet
(Ton/Hr.)
CHEAP Outlet
(Ton/Hr.)
Series A Run 1
Series A Run 2
Series A Run 3
12.0
12.7
11.9
12.2
12.1
12.1
Series B Run 1
Series B Run 2
Series B Run 3
12.3
11.9
12.5
Particle Size 1
Particle Size 2
Particle Size 3
11.8
12.5
12.6
-45-
-------
TABLE 3-2
GENERAL PLANT PROCESS OPERATING PARAMETERS
(4/15/80, Series A, Run 1)
Production
Rate
Time (TPD)
11:22
11:38
12:00
12:11
12:16
12:30
12:45
12:59
13:15
13:29
13:44
I 13:59
£ 14:14
1 14:32
14:48
14:59
15:15
15:29
15:46
15:59
16:14
16:34
16:45
16:59
17:16
17:30
17:36
Inlet
286
280
294
Test Started
284
288
298
286
276
281
281
273
281
285
289
290
302
298
287
309
298
307
307
304
310
306
Test Ended
Test Average
Outlet Test Average
a
Feed
8.0
8.0
7.9
8.0
7.9
8.0
7.9
7.4
7.4
7.5
7.5
7.5
7.5
7.5
7.5
7.5
7.4
7.5
7.5
7.5
7.5
7.5
7.5
7.5
7.5
287
293
a
Feed
7.5
7.5
7.4
7.5
7.4
7.4
7.4
7.4
7.4
7.5
7.5
7.5
7.5
7.5
7.5
7.5
7.4
7.5
7.5
7.5
7.5
7.5
7.5
7.5
7.5
TPD
TPD
Prill
Temp
(°F)
150
153
155
165
165
155
158
163
160
165
162
163
165
168
168
166
167
170
170
170
172
173
170
170
173
Xtallizer3 Xtallizer3
Level #1 Level 12
46
47
46
48
48
48
48
48
48
48
49
49
50
50
49
50
50
49
V
49
49
48
48
48
48
48
42
42
41
42
42
42
43
43
44
44
44
44
46
44
44
45
45
44
44
44
44
44
44
43
43
Xtallizer
Power
(amps)
59
58
58
58
58
58
57
57
57
57
57
57
59
60
60
60
60
60
61
61
61
60
61
61
62
Melt Trough
Level 11
1.3
1.4
1.5
4.5
1.5
1.4
1.5
1.4
1.6
1.4
1.5
1.4
1.5
2.0
1.9
2.0
2.5
2.3
1.8
1.8
2.0
2.0
2.0
1.9
1.9
Melt Trough3
Level 12
1.3
1.6
1.2
3.5
1.3
1.1
1.0
1.1
1.0
1.1
1.2
1.0
1.5
1.5
1.6
1.6
2.0
1.9
1.4
1.4
1.4
1.5
1.5
1.4
1.6
Raw recorder readings (arbitrary units)
Production rate adjusted by factor of 85 percent (see text)
-------
TABLE 3-3
GENERAL PLANT PROCESS OPERATING PARAMETERS
(4/16/80, Series A, Run 2)
Production a .... a Prill
Time
9:00
9:15
9:24
9:29
9:59
10:29
11:01
12:01
12:20
12:59
. 13:00
J 13:34
14:02
14:29
15:09
15:37
16:04
16:30
16:57
17:35
18:00
18:17
Rate
(TPD)
310
313
Test
321
309
305
289
294
Test
Test
292
284
282
288
280
286
287
290
291
279
267
Test
Inlet Test
CU0 NH_
_ 2 , 3 , Temp
Feed Feed o ^
7.9
7.9
Started
8.0
7.9
8.0
7.8
7.8
Interrupted
Restarted
7.8
7.8
7.8
7.8
7.8
7.8
7.8
7.8
7.8
7.8
7.8
Ended
Average
Outlet Test Average'
a Raw
b PrnrJ
recorder
nnfion ra
7.5
7.5
7.6
7.6
7.6
7.6
7.6
7.6
7.6
7.6
7.6
7.6
7.6
7.6
7.4
7.4
7.4
7.4
304 TPD
290 TPD
152
150
153
155
157
162
163
156
152
157
158
160
162
175
173
172
165
163
Xtallizer3 Xtallizer3
Level #1 Level #2
44
44
43
43
42
42
43
44
44
45
45
45
45
45
45
45
44
45
38
38
38
38
38
38
38
40
40
40
41
40
40
40
40
40
40
40
Xtallizer
Power
(amps)
51
51
50
50
49
48
47
47
47
47
47
48
48
48
48
47
47
47
Melt Trough3
Level 11
2.8
3.4
1.5
1.3
1.8
1.5
1.4
1.5
1.5
1.3
1.6
1.6
1.4
1.7
1.5
1.4
1.4
1.5
Melt Trough
Level #2
4.2
5.2
3.6
3.4
2.6
2.6
2.3
2.1
2.1
1.7
1.7
2.0
2.5
2.2
2.3
1.7
1.4
1.7
readings (arbitrary units)
i"o arf'iiici'ori 1
->v fstr't-nr nf fl
17. 7 nor
font- fsoo t-ovt
•\
-------
TABLE 3-4
GENERAL PLANT PROCESS OPERATING PARAMETERS
(4/17/80, Series A, Run 3)
.00
Production a
Rate
Time (TPD)
8:22
8:30
9:17
10:00
10:42
11:10
11:40
12:03
12:16
12:37
13:00
13:36
14:06
14:36
15:09
15:30
15:44
Inlet
299
Test
294
302
291
285
278
274
Test
Test
277
290
303
299
306
298
Test
Test
C°2
Feed
7.9
Started
8.0
7.9
7.9
7.8
7.8
7.8
Interrupted
Restarted
7.8
7.8
7.8
7.8
7.8
7.8
Ended
Average 285
Outlet Test Average 290
a Raw recorder
t> Product ir
->n ra
.__ a Prill
NH_ „
Feid ^
7.3
7.3
7.3
7.3
7.2
7.2
7.2
7.2
7.2
7.2
7.2
7.2
7.2
TPD
TPD
140
135
132
133
134
137
132
141
143
140
141
142
142
Xtallizer3
Level #1
44
44
44
44
44
44
44
45
45
44
44
44
44
Xtallizer9
Level #2
40
39
39
39
40
40
40
40 '
40
39
38
38
38
Xtallizer
Power
(amps)
47
47
47
47
46
46
46
47
47
47
47
46
46
Melt Trough9
Level 11
1.4
1.7
1.5
1.5
1.3
1.4
1.5
1.4
1.4
1.4
1.4
1.5
1.4
Melt Trough3 .
Level #2
1.6
2.3
2.1
2.0
2.0
1.7
1.0
1.4
1.4
1.4
1.4
1.5
1.3
readings (arbitrary units)
t*> arHiist-^ri bv ft
sctor of 9
4.5 oe r
cpnh (SPP t
oxtl
-------
TABLE 3-5
GENERAL PLANT PROCESS OPERATING PARAMETERS
(4/18/80, Series B, Run 1)
Production Q a
Rate 2
Time (TPD) ee
.P>
vo
8:11
8:23
9:14
9:31
10:00
10:29
10:59
11:30
12:29
13:00
13:37
13:59
14:29
15:00
15:28
15:35
304
Test
318
309
298
291
291
294
297
303
299
295
275
283
292
Test
Average
7.8
Started
7.8
7.8
7.8
7.8
7.8
7.8
7.9
7.8
7.8
7.8
7.9
7.8
7.9
Ended
295 TPD
NH 3
Feed
7.2
7.3
7.3
7.3
7.3
7.2
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
Prill
Temp
<°F)
152
163
157
152
150
152
152
155
156
156
155
156
160
163
Xtallizer3
Level #1
44
43
43
42
42
43
43
42
42
41
43
42
41
40
Xtallizer3
Level #2
38
38
36
36
36
36
36
38
37
36 .
37
36
34
34
Xtallizer
Power
(amps)
47
47
47
45
46
45
44
46
46
45
45
45
46
46
Melt Trough3
Level il
1.6
1.8
2.3
1.5
1.5
1.5
1.4
1.5
1.5
1.6
1.4
1.3
1.6
1.8
Melt Trough
Level #2
1.3
1.5
1.7
1.4
1.3
1.3
1.3
1.3
1.3
1.2
1.2
1.3
1.2
1.4
Raw recorder readings (arbitrary units)
Production rate adjusted by factor of 94 percent
-------
TABLE 3-6
GENERAL PLANT PROCESS OPERATING PARAMETERS
(4/21/80, Series B, Run 2)
i
Ul
Production
Rate
Time (TPD)
7:58
8:58
9:28
9:57
10:24
10:53
11:29
12 :30
13:04
13:31
14:04
14:30
15:00
15:28
15:47
Average
275
Test Started
270
307
295
298
288
290
289
281
281
282
276
280
284
277
Test Ended
286 TPD
coa
Feed
7.9
7.9
7.9
8.0
8.0
8.0
8.0
8.0
8.0
8.0
8.0
7.9
8.0
8.0
8.0
a
Feed
7.3
7.4
7.4
7.3
7.3
7.4
7.4
7.4
7.4
7.4
7.3
7.3
7.3
7.3
7.3
Prill
Temp
158
157
158
156
157
156
157
158
156
158
154
170
164
166
166
Xtallizer3
Level il
44
44
44
43
43
43
43
43
43
43
43
43
43
43
43
Xtallizer3
Level #2
47
47
46
46
46
46
46
46
46
46
46
46
46
46
46
Xtallizer
Power
(amps)
49
45
50
50
50
49
49
49
49
49
49
49
49
49
49
Melt Trough
Level #1
1.4
1.7
1.5
2.4
2.3
2.2
2.6
2.4
2.3
2.1
3.4
1.8
2.1
2.1
2.2
Melt Trough
Level 12
1.4
1.3
1.4
2.1
1.6
1.6
1.9
1.6
1.6
1.5
3.1
1.3
0.8
1.1
1.1
Raw recorder readings (arbitrary units)
Production rate not adjusted (see text)
-------
TABLE 3-7
GENERAL PLANT PROCESS OPERATING PARAMETERS
(4/22/80, Series B, Run 3)
I
Ul
Production a
Rate p 2
Time (TPD) ee
7:55
8:31
8:36
8:40
8:50
8:55
9:14
9:30
9:50
10:03
10:40
10:58
11:27
12:40
13:00
13:29
14:01
14:30
15:00
15:30
15:35
Average
295
310
Test
Test
Test
300
300
305
305
305
300
280
315
290
305
300
290
295
310
300
Test
8.0
8.0
Started
Interrupted
Restarted
7.9
7.9
7.9
7.9
7.9
7.9
7.9
8.0
7.9
7.9
7.9
7.9
7.9
7.9
7.9
Ended
NH a
Feed
7.3
7.3
7.3
7.3
7.3
7.3
7.2
7.2
7.3
7.2
7.2
7.3
7.2
7.2
7.2
7.2
7.2
Prill
Temp
(°F)
160
163
161
161
158
160
160
160
163
168
165
168
163
164
166
167
168
Xtallizer3
Level #1
46
45
45
45
45
46
46
46
46
48
46
46
46
45
44
43
42
Xtallizer3
Level 12
43
42
42
42
42
43
43
44
44
45
43
43
43
42
41
40
39
Xtallizer
Power
(amps)
50
50
49
49
49
49
49
49
49
49
50
50
50
50
50
50
50
Melt Trough3
Level il
2.3
2.3
2.5
1.8
1.8
1.8
1.6
1.3
1.5
-c
2.7
2.2
1.9
1.4
2.2
3.1
3.5
Melt Trough
Level *2
2.0
1.9
2.2
1.4
1.2
1.4
1.4
1.4
1.3
-c
2.3
1.7
1.8
1.3
1.8
2.7
3.1
300 TPD
Raw recorder readings (arbitrary units)
data read from control room
and not adjusted (see
-------
1. Production Rate - Production of prills at Reichhold's plant is moni-
tored by an Ohmart gamma ray absorption unit located on a conveyor
between the prill tower and the rotary drum cooler. Calibration of
the unit, usually done at weekly intervals, is accomplished by passing
calibration plates of known gamma ray absorbency through the device
and then setting the control room instruments accordingly. Production
is logged by both a strip chart recorder and on magnetic disk by a
minicomputer. Reichhold personnel provided EPA with computer print-
outs of production (at 3 to 5 minute intervals) for each test period
except for one day when this printout was not available. For this
day, production data recorded in the control room was used.
Reichhold personnel examined the Ohmart data during the tests and
expressed concern that the recorded production appeared higher than
was indicated by other plant parameters. At the conclusion of the
test, Reichhold provided correction factors for each day which ranged
from 85 percent to 100 percent of recorded production. These correc-
tion factors were based on mass balances of the entire urea plant.
These correction factors have been applied to the data in Tables 3-2
through 3-7 and are recorded at the bottom of each table. A summary
of the corrected production rates is shown in Table 3-4.
2. C02 Feed - The C02 feed to the urea reactor was monitored as an
indicator of normal operation of the synthesis section of the plant.
This parameter was monitored for changes only. Data recorded is the
raw chart recorder values and has not been converted to actual flow-
rates.
3. NH3 Feed - Same comments as above.
4. Prill Temperature - The temperature of the prills leaving the tower
prior to the cooler was monitored with a temperature probe located on
a conveyor near the production rate monitor. This data was recorded
as an indicator of normal cooling function and melt temperature in the
prill tower.
5. Crystallizer Level No. 1 - According to plant personnel, the crystal-
lizer and centrifuges are two of the more troublesome components in
the urea production chain. Since any anomaly in the crystallizer
operation could directly effect the crystals fed to the prill tower,
this parameter was monitored. Only relative changes were of interest;
thus, the numbers have not been converted to actual units.
6. Crystallizer Level No. 2 - This monitor also measures the level in the
crystallizer.
7. Centrifuge Power - The crystallizer centrifuge motor current was moni-
tored as an indicator of changes in urea crystal flowrate prior to the
prill tower.
8. Melt Trough Level No. 1 - Two steam-jacketed crystal melters feed two
melt troughs which gravity-feed the spray heads. Melt trough levels
tend to fluctuate considerably as spray heads build up deposits and
-52-
-------
clog. The trough levels were monitored in case a major upset caused
prill production to drop significantly.
9. Melt Trough Level No. 2 - Same comments as above.
3.3.2 Emission Control System Monitoring
The emission control system was monitored to insure the CHEAF scrubber and
associated preconditioning system was operating normally during the tests.
Additionally, the data provide a characterization of normal control equipment
operation that can be used to assess factors such as power requirements and
water use.
Two groups of parameters directly associated with the emission control
system were monitored during the emissions tests. The first group concerns
the operation of the Downcomer and preconditioning system. The second group
concerns the operation of the CHEAP scrubber.
Seven parameters associated with the Downcomer preconditioner system, and
eight parameters associated with the CHEAF scrubber, were monitored and re-
i
corded during the emissions tests. The Downcomer parameters monitored were:
1. Sump Level - A float recorder in the Downcomer sump was monitored to
insure proper liquor inflows and outflows.
2. Sump Slowdown - Liquor flows out of the Downcomer sump and precondi-
tioning loop to other parts of the plant. This flow was monitored to
insure the preconditioning system was interacting normally with the
rest of the plant. This parameter was monitored for relative changes
only. Data values shown are raw chart recorder readings.
3. Preconditioner Flowrate - A flowmeter reading was available for one
portion of the preconditioning system. It was monitored to insure the
preconditioning sprays were operating normally. These readings are
given in terms of standardized values since the plant considers this
information confidential.
4. Preconditioning Temperature No. 1 - Temperature measurements were
available at two points in the preconditioning system and were record-
ed as an indicator of normal preconditioner operation. These measure-
ments are given in terms of standardized values since the plant
considers this information confidential.
-53-
-------
5. Preconditioner Temperature No. 2 - Same comments as above.
6. Prill Tower Exit Temperature No. 1 - The prill tower exhausts through
four ports. These ports are ducted into two manifolds before being
joined to the common Downcomer, and each manifold is equipped with a
temperature sensor. Manifold temperatures were monitored for abnormal
and sudden temperature variations.
7. Prill Tower Exit Temperature No. 2 - Same comments as above.
Preconditioning system data recorded during the emissions tests are summarized
in Tables 3-8 through 3-13.
The CHEAP scrubber operating parameters monitored were:
1. Pressure Drop - The total pressure drop from the CHEAP inlet to a
position prior to the fan but after the demister was monitored. Since
pressure drop has a direct effect on scrubber efficiency, this reading
served as an important indicator of proper scrubber operation. Read-
ings taken in the control room were generated electrically using pres-
sure transducers. U-tube water manometer readings were also taken
during the emissions tests and are presented in Section 2.4 of this
report.
2. Liquor Flowrate - The flow of scrubber liquor to the CHEAP sprays is
measured with a flowmeter. Since an adequate and uninterrupted supply
of liquor to the filter mat is vital for proper scrubber operation,
this parameter was monitored for unusual variations.
3. Sump Level - The sump directly feeds the CHEAP sprays. The sump
liquor level was used as an indicator of normal inflow and outflow.
4. Fan Current - The current to the fan motor is an indicator of normal
airflow through the entire prill tower-scrubber system. The current
meter in the control room was monitored. This meter measures one
phase of the three-phase current used by the fan motor.
5. Spray Temperature - The CHEAP spray temperature was recorded during
the tests and serves to indicate normal interior temperatures in the
CHEAP.
\
6. Inlet Temperature - A temperature sensor located at the top of the
CHEAP filter section serves to identify any changes in the prill tower
and preconditioning system which might affect the scrubber performance.
7. Outlet Temperature - The sensor for this parameter is located just
prior to the fan. With this reading it is possible to determine
normal temperature differences across the filter mat and demister.
8. Stack Temperature - The sensor for this parameter is located in the
ductwork leading from the fan housing to the outlet stack and is used
to indicate approximate gas stream outlet temperatures.
-54-
-------
TABLE 3-8
PRECONDITIONER OPERATING PARAMETERS
(4/15/80, Series A, Run 1)
i
Ul
Ul
I
Time
11:22
11:38
12:00
12:11
12:16
12:30
12:45
12:59
13:15
13:29
13:44
13:59
14:14
14:32
14:48
14:59
15:15
15:29
15:46
15:59
16:14
16:34
16:45
16:59
17:16
17:30
17:36
Sump
Level
55
54
54
Start
52
53
54
54
53
53
54
53
54
54
54
53
53
53
54
54
54
53
54
54
53
54
Test
Sump
Slowdown
12.0
12.0
12.0
Test
12.0
12.0
12.0
12.0
12.0
12.0
12.3
12.3
12.3
12.3
12.3
12.3
12.3
12.3
12.3
12.3
12.3
12.0
12.3
11.8
12.1
12.5
Ended
Precond.
Flowrate
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
Precond.
Temp 11
-.02
0
0
0
0
0
0
-.01
-.01
-.01
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
Precond .
Temp 12
0
-.01
-.01
0
.01
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
Prill Tower
Exit Temp fl
111
109
110
109
108
110
110
110
111
108
112
111
107
108
109
109
110
109
109
109
110
108
110
110
108
Prill Tower
Exit Temp #2
107
107
108
106
108
108
109
108
110
112
110
110
115
115
117
118
118
118
120
117
117
119
118
114
118
Raw recorder readings (arbitrary units)
Values shown have been standardized (see text)
-------
TABLE 3-9
PRECONDITIONER OPERATING PARAMETERS
(4/16/80, Series A, Run 2)
i
01
Time
9:00
9:15
9:24
9:29
9:59
10:29
11:01
11:29
12:01
12:20
12:59
13:00
13:34
14:02
14:29
15:09
15:37
16:04
16:30
16:57
17:35
18:00
18:17
a Raw
Sump
Level
(%)
70
70
Start
69
69
68
68
68
67
Test
Test
64
63
62
61
61
61
60
60
60
60
61
Test
3
Sump
Slowdown
12.2
12.2
Test
12.3
12.3
12.2
11.5
12.3
12.2
Interrupted
Restarted
12.1
11.5
12.3
12.3
12.3
12.3
12.3
11.0
11.2
11.1
11.2
Ended
b
Precond.
Flowrate
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
b
Precond .
Temp 11
-.01
-.01
-.01
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
b
Precond.
Temp 12
.01
0
0
0
0
0
0
0
0
0
0
0
0
0
0
-.01
-.01
-.01
0
Prill Tower
Exit Temp 11
(°F)
103
104
104
106
107
107
109
109
113
114
113
114
116
116
113
110
108
105
105
Prill Tower
EXit Temp 12
(°F)
103
103
104
105
107
106
108
109
111
112
112
113
114
114
117
113
112
111
111
recorder readings (arbitrary units)
b Values shown have been standardized (see
text)
-------
TABLE 3-10
PRECONDITIONER OPERATING PARAMETERS
(4/17/80, Series A, Run 3)
I
Ln
Time
8:22
8:30
9:17
10:00
10:42
11:10
11:40
12:03
12:16
12:37
13:00
13:36
14:06
14:36
15:09
15:30
15:44
Sump
Level
54
Start
54
53
53
53
54
53
Test
Test
54
54
54
54
51
54
Test
a b
Sump Precond.
Slowdown Flowrate
12.2
Test
12.2
12.3
11.5
11.2
11.3
11.2
Interrupted
Restarted
11.2
11.2
11.0
11.1
11.4
11.4
Ended
0
0
0
0
0
0
0
0
0
0
0
0
0
Precond. Precond.
Temp 11 Temp 12
0
-.01
-.01
0
0
0
0
.01
.01
0
-.01
-.01
-.01
.01
0
0
0
0
-.01
0
0
0
0
0
0
0
Prill Tower
Exit Temp 11
104
103
104
103
104
104
104
105
105
107
107
108
108
Prill Tower
Exit Temp 42
101
98
100
99
101
100
101
104
104
106
106
106
106
Raw recorder readings (arbitrary units)
Values shown have been standardized (see text)
-------
TABLE 3-11
PRECONDITIONER OPERATING PARAMETERS
(4/18/80, Series B, Run 1)
00
Time
8:11
8:23
9:14
9:31
10:00
10:29
10:59
11:30
12:29
13:00
13:37
13:59
14:29
15:00
15:28
15:35
Sump
Level
64
Test
65
64
64
63
63
64
64.
64
62
61
61
62
62
Test
Sump
Slowdown
11.2
Started
11.2
11.3
11.3
11.2
11.3
11.3
11.2
11.0
11.2
11.6
11.2
11.2
11.1
Ended
Precond.
Flowrate
.01
-.01
-.02
0
-.02
.01
.02
.02
.01
-.01
.02
.02
-.02
-.03
P r econd . P r econd .
Temp 11 Temp 12
.01
.01
.01
.01
0
0
-.01
-.01
-.01
-.01
0
0
0
0
.01
.01
0
0
0
0
0
0
0
-.01
0
0
0
0
Prill Tower
Exit Temp fl
104
105
107
106
105
106
108
109
111
111
110
110
112
113
Prill Tower
ExitQTemp §2
101
103
105
104
104
105
107
110
111
110
110
110
111
112
Raw recorder readings (arbitrary units)
Values shown have been
-------
TABLE 3-12
PRECONDITIONER OPERATING PARAMETERS
(4/21/80, Series B, Run 2)
vo
I
Time
7:58
8:58
9:28
9:57
10:24
10:53
11:29
12:30
13:04
13:31
14:04
14:30
15:00
15:28
15:47
Sump
Level
52
Start
54
54
53
52
52
51
48
50
51
48
51
50
50
50
Test
Sump
Slowdown
11.3
Test
11.2
11.2
11.4
11.2
11.2
11.2
11.1
11.2
11.2
11.2
11.2
11.2
11.2
11.0
Ended
Precond.
Flowrate
-.16
.17
-.09
-.01
-.01
.02
.01
.02
-.03
.02
.01
-.01
.02
-.01
.01
Precond. Precond.
Temp #1 Temp 12
0
-.02
-.01
0
0
0
0
0
.01
0
0
0
.01
0
0
-.01
.01
0
0
0
0
0
0
0
0
0
0
0
0
0
Prill Tower
Exit Temp #1
92
94
94
96
97
98
99
100
101
100
101
100
100
101
100
Prill Tower
Exit Temp «2
91
93
94
96
99
100
102
103
104
102
102
103
104
104
104
Raw recorder readings (arbitrary units)
Values shown have been standardized (see text)
-------
TABLE 3-13
PRECONDITIONER OPERATING PARAMETERS
(4/22/80, Series B, Run 3)
o
Time
7:55
8:31
8:36
8:40
8:50
8:55
9:14
9:30
9:50
10:03
10:40
10:58
11:27
12:40
13:00
13:29
14:01
14:30
15:00
15:30
15:35
Sump
Level
64
62
Test
Test
Test
56
56
56
56
56
53
52
50
51
48
52
49
50
50
50
Test
Sump
Slowdown
11.2
11.2
' Star ted
Interrupted
Restarted
11.2
11.4
11.2
11.0
11.5
11.2
11.2
11.2
11.1
11.7
11.1
11.1
11.2
11.1
11.3
Ended
Precond.
Flowrate
-.13
-.23
-.04
-.01
-.01
.11
.11
.20
.20
.18
-.03
-.06
-.06
-.04
-.04
-.06
-.05
Precond. Precond.
Temp 11 Temp 12
0
.10
0
0
0
-.04
-.05
-.04
-.04
-.04
.01
0
0
0
0
0
0
0
0
0
0
b
0
0
0
.01
.03
0
.01
0
0
0
0
0
Prill Tower
Exit Temp 11
94
100
98
98
98
98
99
100
101
102
105
105
103
102
104
104
104
Prill Tower
Exit Temp |2
96
98
97
97
98
98
99
100
101
102
104
105
105
105
106
107
107
Raw recorder readings (arbitrary units)
Values shown have been standardized (see text)
-------
CHEAP scrubber system data recorded during the emissions test are summarized
in Tables 3-14 through 3-19.
3.4 Summary of Plant Operations
The plant functioned smoothly throughout the 6 days of testing. Three
minor test interruptions (described below) were identified by personnel moni-
toring the production process:
1. 4/16/80, 1220 - Both melt troughs experienced high levels due to spray
head plugging. The testing crew was instructed to discontinue testing
until the heads were cleaned. Almost immediately after shutdown, the
heads were cleaned and the trough levels began to drop. The test was
restarted at 1259.
2. 4/17/80, 1216 - Spray head plugging reoccurred and testing was inter-
rupted from 1216 to 1237. Subsequently it was decided that unless
trough levels remained high for a significant period, a testing inter-
ruption was unnecessary.
3. 4/22/80, 0840 - The bubbler level indicator in the CHEAP sump clogged
and the sump was pumped down. The sump tends to collect an oily film
from pump packings and this film floats on the surface of the sump.
This oil was pumped onto the CHEAP filter and caused the pressure drop
to increase. In order to maintain a pressure drop reasonably consis-
tent with previous runs, the baffle plate was adjusted. The bubbler
was cleaned and testing resumed at 0850.
Overall, the prill tower and CHEAP scrubber were operating normally during
the entire testing period.
-61-
-------
TABLE 3-14
CHEAP OPERATING PARAMETERS
(4/15/80, Series A, Run 1)
I
ON
ho
Time
11:22
11:38
12:00
12:11
12:16
12:30
12:45
12:59
13:15
13:29
13:44
13:59
14:14
14:32
14:48
14:59
15:15
15:29
15:46
15:59
16:14
16:34
16:45
16:59
17:16
17:30
17:36
Pressur
Drop
(in W.G
15.5
16.0
16.0
Test
16.0
16.0
16.0
15.8
15.8
15.5
15.8
15.5
15.3
15.6
15.3
15.7
15.4
15.5
15.3
15.5
15.5
15.6
15.5
15.5
15.3
15.5
Test
e Liquor
Flowrate
.) (GPM)
225
225
225
Started
228
225
225
225
225
228
228
225
225
228
225
228
225
225
228
225
228
225
225
225
228
225
Ended
Sump
Level
(in)
43.2
43.2
43.8
44.4
44.4
43.2
43.2
44.4
43.8
44.
44.
44.
44.
43.
44.
44.
44.
43.8
43.2
44.4
43.8
43.8
44.4
44.4
43.8
Fan
Current
(amps)
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
44
Spray
Temp
(°F?
94
94
94
96
94
94
95
94
95
95
95
96
96
95
96
96
96
96
96
96
96
96
97
96
96
Inlet
Temp
(°F?
95
94
96
95
95
95
96
95
96
95
96
96
97
96
96
96
97
96
96
96
96
96
97
96
96
Outlet
Temp
(°F)
94
95
94
94
94
95
95
94
95
95
95
95
95
95
95
95
96
96
96
95
96
96
96
95
95
Stack
Temp
(°F)
106
106
102
104
105
105
105
105
106
106
106
106
106
106
106
106
107
106
106
106
106
106
106
106
106
-------
TABLE 3-15
CHEAP OPERATING PARAMETERS
(4/16/80, Series A, Run 2)
LO
I
Time
9:00
9:15
9:24
9:29
9:59
10:29
11:01
11:29
12:01
12:20
12:59
13:00
13:34
14:02
14:29
15:05
15:37
16:04
16:30
16:57
17:35
18:00
18:17
Pressure Liquor
Drop Flowrate
(in W.G.) (GPM)
12.5
12.7
Test
12.3
12.4
12.5
12.5
12.5
12.5
Test
Test
12.3
12.3
12.3
12.3
12.1
12.3
12.1
12.2
12.3
12.2
12.1
Test
228
228
Started
228
225
225
228
228
228
Interrupted
Restarted
228
228
228
228
228
228
228
228
228
228
228
Ended
Sump
Level
(in)
43.2
43.8
44.4
44.4
43.8
43.8
43.8
43.8
44.4
44.4
44.4
43.8
43.2
43.8
44.4
43.8
43.8
44.4
44.4
Fan
Current
(amps)
46
47
47
46
46
46
46
46
46
46
46
46
46
46
46
46
44
46
46
Spray
Temp
<°F)
94
94
93
93
93
93
94
95
95
95
95
95
96
96
96
95
95
94
95
Inlet
Temp
<°F>
94
94
94
94
94
94
95
95
95
96
95
95
96
96
96
95
95
94
95
Outlet
Temp
<°F)
94
94
94
94
94
94
94
95
95
95
95
95
96
96
95
95
95
94
95
Stack
Temp
<°F)
104
103
103
104
103
104 .
105
105
105
105
105
105
106
105
106
105
105
104
104
-------
TABLE 3-16
CHEAP OPERATING PARAMETERS
(4/17/80, Series A, Run 3)
Time
8:22
8:30
9:17
10:00
10:42
11:10
11:40
12:03
12:16
12:37
13:00
13:36
14:06
14:36
15:09
15:30
15:44
Pressure Liquor
Drop Flowrate
(in W.G.) (GPM)
12.5
Test
12.5
12.5
12.3
12.5
12.5
12.5
Test
Test
12.5
12.2
12.3
12.5
12.3
12.3
Test
228
Started
228
228
228
228
230
230
Interrupted
Restarted
230
230
230
233
230
230
Ended
Sump
Level
(in)
43.8
43.2
45.0
43.8
43.9
44.4
43.8
43.8
43.8
44.4
44.4
44.4
43.8
Fan
Current
(amps)
46
46
47
46
46
47
46
46
46
46
46
46
46
Spray
Temp
<°F)
93
92
92
92
92
93
92
93
93
94
94
94
94
Inlet
Temp
(°F)
94
93
93
93
93
93
94
93
93
94
94
94
94
Outlet
Temp
(0F?
93
92
93
92
93
93
92
93
93
94
93
93
94
Stack
Temp
(°F)
102
102
102
102
102
102
102
102
102
103
103
103
103
-------
TABLE 3-17
CHEAP OPERATING PARAMETERS
(4/18/80, Series B, Run 1)
Ul
Time
8:11
8:23
9:14
9:31
10:00
10:29
10:59
11:30
12:29
13:00
13:37
13:59
14:29
15:00
15:28
15:35
Pressure Liquor
Drop Flowrate
(in W.G.) (GPM)
12.1
Test
12.1
12.1
12.0
12.0
12.4
12.1
11.9
12.3
12.0
12.2
11.9
12.1
11.9
Test
235
Started
233
235
235
235
235
235
235
235
235
235
235
235
235
Ended
Sump
Level
(in)
44.4
44.4
44.4
44.4
44.4
44.4
44.4
44.4
44.4
44.4
44.4
44.4
44.4
44.4
Fan
Current
(amps)
46
46
46
46
46
46
46
46
46
46
46
46
46
46
Spray
Temp
<°F)
94
95
95
95
94
95
95
96
96
95
96
96
96
96
Inlet
Temp
<°F)
95
95
95
95
95
95
96
97
96
96
96
97
97
97
Outlet
Temp
<°F)
94
94
95
94
94
95
95
96
95
95
95
96
96
96
Stack
Temp
<°F)
104
104
105
104
104
104
104
105
105
105
105
105
106
106
-------
TABLE 3-18
CHEAP OPERATING PARAMETERS
(4/21/80, Series B, Run 2)
Time
7:58
8:58
9:28
9:57
10:24
10:53
11:29
12:30
13:04
13:31
14:04
14:30
15:00
15:28
15:47
• Pres
Drop
(in
12
Te
12
12
12
12
12
12
12
12
12
12
12
12
12
12
Te
SUl
W.C
.4
st
.4
.4
.4
.4
.5
.4
.3
.4
.4
.5
.4
.5
.5
.4
st
re Liquor Sumj
Flowrate Lev*
;.) (GPM) (in)
235 44.-!
Started
235 44.
235 44.
235 44.
235 44.
235 43.
235 44.
233 44.
235 44.
235 44. <
235 44. <
235 44.4
235 44. <
235 44. <
235 44. ^
Ended
) Fan
>1 Current
(amps)
1 46
46
46
46
47
46
46
46
46
1 46
1 46
1 46
1 46
1 46
1 46
Spray
Temp
(°F)
89
91
91
91
91
91
92
92
92
92
92
92
92
92
92
Inlet
Temp
<°P)
89
91
91
91
91
91
92
91
92
92
92
91
91
92
92
Outlet
Temp
(°F)
89
91
91
91
91
92
92
92
92
92
92
92
92
92
92
Stack
Temp
(°F)
99
101
101
101
101
102
102
102
102
102
102
102
102
102
102
-------
TABLE 3-19
CHEAP OPERATING PARAMETERS
(4/22/80, Series B, Run 3)
i
o\
Time
7:55
8:31
8:36
8:40
8:50
8:55
9:14
9:30
9:50
10:03
10:40
10:58
11:27
12:40
13:00
13:29
14:01
14:30
15:00
15:30
15:35
Pressure Liquor
Drop Flowrate
(in W.G.) (GPM)
12.5
13.0
Test
Test
Test
12.9
12.4
12.2
12.2
12.7
12.5
12.5
12.5
12.2
12.3
12.3
12.2
12.3
12.3
12.4
Test
238
225
Started
Interrupted
Restarted
228
235
235
233
235
235
235
235
235
235
235
235
235
235
235
Ended
Sump
Level
(in)
48.6
27.6
39.0
39.0
39.0
39.0
38.4
39.0
39.0
39.0
39.0
39.0
39.0
39.0
39.0
39.0
39.0
Fan
Current
(amps)
46
46
45
45
45
46
45
46
45
45
45
45
46
46
46
46
46
Spray
Temp
<°F)
92
95
93
93
93
93
93
94
94
95
95
95
94
94
94
94
94
Inlet
Temp
(°F)
93
94
93
92
94
93
94
93
95
96
95
95
94
94
94
94
94
Outlet
Temp
(°F)
92
94
93
93
93
93
94
93
95
95
95
95
94
94
94
94
94
Stack
Temp
<°F)
102
105
103
103
103
103
104
104
105
105
105
105
104
105
104
105
113
-------
4.0 LOCATION OF SAMPLING PORTS AND POINTS
This section presents descriptions of the sampling locations used during
the emissions testing program conducted on the prill tower CHEAP scrubber at
the Reichhold Chemicals, Inc., urea manufacturing plant in St. Helens, Oregon
during April 1980. Figure 4-1 shows a profile schematic of the CHEAP scrubber.
4.1 CHEAP Inlet (Downcomer)
The Downcomer inlet sampling site was located in a 75-inch ID vertical
section of a stainless steel duct. A schematic of the Downcomer inlet,
including exact traverse point locations, is presented in Figure 4-2.
The two flanges from the middle preconditioning sprayers, which were posi-
tioned 90 degrees apart in a horizontal plane, were used for the sampling
ports. These ports were located 21 feet 6 inches (3.4 duct diameters) up-
stream from the lower preconditioning sprayers and 20 feet 3 inches (3.2 duct
diameters) downstream from the upper preconditioning sprayers.
This inlet sampling location did not meet the "eight and two diameters"
criterion as prescribed in EPA Method 1; hence 24 sampling points were used on
each of the two traverse axes, for a total of 48 sampling points.
4.2 CHEAP Outlet
From the inlet testing location the prill tower gases are drawn through
the CHEAP scrubber and entrainment separator by a 400 horsepower induced draft
fan. The gases are then exhausted to the atmosphere through an 80 foot stack.
The 95 inch ID outlet stack was fitted with two 4-1/2" pipe flange samp-
ling ports positioned 90 degrees apart in a horizontal plane. The sampling
ports were located 9 feet 6 inches (1.2 duct diameters) upstream from the top
of the stack and 30 feet 6 inches (4.9 duct diameters) downstream from where
the short extension duct from the ID fan enters the outlet stack.
-68-
-------
CTi
ID
I
PRILL TOWER
21'-4" O.D.
A
PRECONDITIONING
SPRAYS
^ DOWNCOMER
'-0" O.D.
VARIABLE FLOW CHEAF
EXHAUST STACK
8'-0" O.D.
ENTRAINMENT
SEPARATOR ~~7
/ \
J.
A
~—~^ J
t
r-*V
f K ^
:fl=0-fl-Jl
•»-
=fr-
^v
b
400
HP-
FAN
rf\ « "|
_ 1 1
FIGURE 4-1: SCHEMATIC OF PRILL TOWER CHEAF SCRUBBER AT
REICHHOLD CHEMICALS. INC., ST. HELENS, OREGON
LJ
•RECIRCULATION SUMP
0988-008
-------
o
I
TRAVERSE POINT
NUMBER
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
TRAVERSE POINT
LOCATION FROM
OUTSIDE OF
NIPPLE (INCHES)
8.00
9.40
11.13
12.95
14.86
16.90
19.10
21.55
24.25
27.40
31.23
36.85
52.53
57.78
61.60
64.75
67.45
69.93
72.10
73.98
76.08
77.88
79.60
81.00
UPPER _
SPRAYERS
LOWER .
SPRAYERS
FLOW
i\\\ \i\\\\
in i
TO
CHEAP
FIGURE 4-2: CHEAF INLET (DOWNCOMER) SAMPLING LOCATION REICHHOLD CHEMICALS, INC.,ST. HELENS, OREGON
0988-001
-------
The outlet sampling location did not meet the "eight and two diameters"
criterion of EPA Method 1. Twenty sampling points were chosen for each
traverse axis, for a total of 40 sampling points. A schematic of the CHEAP
outlet, including exact traverse point locations, is presented in Figure 4-3.
4.3 Inlet Particle Sizing Locations
Three particle sizing tests were performed on the CHEAP inlet (Downcomer)
gas stream. A Sierra Series 226 in-stack cascade impactor was positioned in a
sampling port used for the urea emissions tests. During each test run the
impactor nozzle was positioned at a point of average velocity as determined by
preliminary velocity traverses performed before each particle size test run.
All three particle sizing tests were performed at Fort 1 Point 10.
4.4 Visible Emissions Observation Locations
The white plume exiting the CHEAP scrubber was observed from three loca-
tions chosen to conform with EPA Reference Method 9 guidelines. The three
observer locations are shown in Figure 4-4 and are described below.
Distance to Height Above Direction
Observer Discharge Point
Location (Feet)
A 300
B 300
C 200
4.5 Scrubber Liquor Collection
Ground
(Feet)
40
0
0
Locations
From Discharge
Point
E
SSE
ESE
Discharge
Description
CHEAP Outlet
CHEAP Outlet
CHEAP Outlet
Scrubber liquor samples were collected during the Series A and the Series
B emissions tests. (Series A: simultaneous inlet and outlet testing, with
preconditioning sprayers off; Series B: outlet testing only, with the precon-
ditioning sprayers on.) During Series A and B, liquor samples were collected
-71-
-------
TRAVERSE POINT
NUMBER
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
TRAVERSE POINT
LOCATION FROM
OUTSIDE OF
NIPPLE (INCHES)
5.75
8.25
10.86
13.71
16.75
20.17
23.90
28.25
33.50
41.40
62.64
70.43
75.75
80.12
83.80
87.24
90.24
93.13
95.79
98.26
TO ATMOSPHERE
1.0. FAN
95" [MHHIHIIIIH —I— uiniinniiiuii I NEST
NORTH
FIGURE 4-3: CHEAF OUTLET SAMPLING LOCATION REICHHOLD CHEMICALS, INC., ST., HELENS, OREGON
0988-002
-------
LEGEND
* OBSERVER LOCATIONS
• AMBIENT AIR MEASUREMENTS LOCATION
PRILL TOWER
CHEAF ENTRAPMENT
SCRUBBER SEPARATOR
OUTLET
STACK
BULK STORAGE
WAREHOUSE
BULK STORAGE
WAREHOUSE
AMMONIA
STORAGE
TANKS
FRONT
GATE
AMMONIUM
NITRATE
STORAGE
TANKS
FIGURE 4-4: VISIBLE EMISSIONS OBSERVER LOCATIONS
REICHHOLD CHEMICALS, .INC. ,ST. HELENS, OREGON
-73-
0988-003
-------
by TRC personnel from the following locations:
common samples from the solution formation lower sprays and downcomer
sump;
samples from the CHEAP sump.
During Series B, liquor samples were collected by Reichhold personnel from the
following locations:
• common samples from upper sprays from the strippers and middle sprays
from crystallizers;
• scrubber bottom;
• hot well to sump.
4.6 Ambient Air Temperature and Relative Humidity Measurement Location
Ambient air temperature and relative humidity measurements were taken at
the base of the CHEAP scrubber outlet stack during each emission test. Figure
4-4. shows the location of this measurement point.
-74-
-------
5.0 SAMPLING AND ANALYSIS METHODS
This section presents general descriptions of sampling and analysis proce-
dures employed during the emissions testing program conducted at the Reichhold
Chemicals Inc., St. Helens, Oregon urea manufacturing facility during April
15-22, 1980. Details of sampling and analysis procedures are contained in
Appendices G and H.
5.1 EPA Reference Methods Used in This Program
The following EPA Reference Methods were used during this emission testing
program. These methods are taken from "Standards of Performance for New
Stationary Sources, Appendix A", Federal Register, Volume 42, No. 160, Thurs-
day, August 18, 1977, pp 41755 ff.
• Method 1 - Sample and Velocity Traverses for Stationary Sources
This method specifies the number and location of sampling points
within a duct, taking into account duct size and shape and local
flow disturbances.
• Method 2 - Determination of Stack Gas Velocity and Volumetric Flow-
rate
This method specifies the measurement of gas velocity and flowrate
using a pitot tube, manometer and temperature sensor. The physical
dimensions of the pitot tube and its spatial relationship to the
temperature sensor and any sample probe are also specified.
• Method 4 - Determination of Moisture Content in Stack Gases
This method describes the extraction of a gas sample from a stack
and the removal and measurement of the moisture in that sample by
condensation impingers. The assembly and operation of the required
sampling train are specified.
• Method 9 - Visual Determination of the Opacity of Emissions from
Stationary Sources
This method describes how trained observers are to determine the
opacity of emissions. The duration and frequency of observations,
orientation of the observer with respect to the source, sun and
background, methods of data recording and calculation, and qualifi-
cations of observers are specified.
-75-
-------
The emissions tests and sample analyses were performed using EPA
Reference Method 28, Determination of Particulate (Urea) Emissions
from Urea Plants. This method incorporates modifications to EPA
Reference Method 5, Determination of Particulate Emissions from
Stationary Sources, that reflect the characteristics of urea and
urea sources. With Method 5 as a reference, Method 28 specifies
the isokinetic sampling of urea particulate from a gas stream
utilizing techniques introduced in Methods 1, 2, and 4. Sample
collection and recovery, sampling train cleaning and calibration,
and gas stream flowrate calculation procedures are specified.
Method 28 is shown in its entirety in Appendix G.
5.2 Urea Sampling and Analysis at the Cleanable High Efficiency Air Filter
Scrubber (CHEAP)
5.2.1 Sampling Methods
Urea in the inlet and outlet gas stream of the CHEAP scrubber were samp-
led at points located in accordance with EPA Method 1. The velocity of the
duct gas was measured using S-type pitot tubes constructed and calibrated in
accordance with EPA Method 2.
The sampling train used on this sampling program is shown in Figure 5-1
and is a modification to the particulate sampling train specified by EPA
Method 28. The modifications used were: altered impinger sequence, use of
a Teflon line, and the addition of a sixth impinger.
The sampling train shown in Figure 5-1 consists of a nozzle, probe, Tef-
lon line, six impingers, vacuum pump, dry gas meter, and an orifice flow
meter. The nozzle is stainless steel and of buttonhook shape. The nozzle
was connected to a 5/8-inch stainless steel glass-lined probe wrapped with
nichrome heating wire and jacketed. Following the probe, the gas stream
passed through a 3/8-inch I.D. Teflon line into an ice bath/impinger
system. The impinger system consisted of six impingers in series. The
first, third, fifth and sixth impingers were the Greenburg-Smith design,
modified by replacing the tip with a 1/2 inch glass tube extended to within
1/2 inch of the impinger's bottom. The second and fourth impingers were of
-76-
-------
STACK WALL
THERMOMETER
f
n
t
I
LEGEND
1 - NOZZLE 7
2 - PROBE 8
3 - TEFLON LINE 9
4 - ICE BATH 10
5 - FLEXIBLE LINE 11
6 - VACUUM GAGE 12
NEEDLE VALVE
PUMP
DRY GAS METER
ORIFICE
PITOT TUBE & INCLINED MANOMETER
POTENTIOMETER
FIGURE 5-1: MODIFIED EPA PARTICULATE SAMPLING TRAIN
-------
the regular design Greenburg-Smith units including tips with orifice plates
located within 1/2 inch of the bottom. The first two impingers contained
deionized, distilled water (100 mis each). The next two impingers contained
IN H.SO. (100 mis each) . The fifth impinger was empty, and the sixth
contained 200 grams of indicating silica gel. Leaving the last impinger,
the sample stream flowed through flexible tubing, a vacuum gauge, needle
valve, pump, and a dry gas meter. A calibrated orifice and inclined mano-
meter completed the train. The stack velocity pressure was measured using a
pitot tube and inclined manometer. Stack temperature was monitored by a
thermocouple attached to the probe and connected to a potentiometer. A
nomograph was used to determine the orifice pressure drop required to main-
tain isokinetic sampling conditions.
The probe temperature was maintained at about 10 F above the duct gas
temperature, in order to prevent condensation within the probe.
Test data recorded at each sampling point included test time, sampling
duration at each traverse point, pitot pressure, stack temperature, dry gas
meter volume and inlet-outlet temperature, probe temperature and orifice
pressure drop.
The sampling train was leak checked before and after each test run. The
sampling train calibration data is contained in Appendix I.
5.2.1.1 CHEAP Inlet
During Series A test run 1 each of the 48 traverse points was sampled
for 4 minutes yielding a total test time of 192 minutes. During test runs 2
and 3, each traverse point was sampled for three minutes for a total test
time of 144 minutes. The extended test time on test run 1 was due to an
oversight by the sampling train operator.
-78-
-------
5.2.1.2 CHEAP Outlet
For the Series A test run 1, each traverse point was sampled for 4
minutes and each port was traversed twice, for a total sample time of 320
minutes. In the analysis of the Series A test run 1 samples, the TRC chem-
ist determined that the urea concentrations were near the lower detectable
limit. Under the direction of the Technical Manager the Series A test run 2
total sampling time was increased to 480 minutes by traversing each port
three times. This technique yielded more than enough urea for analysis, so
for test run 3 the total sampling time was reduced to 400 minutes (5 minutes
per point and each port traversed twice). This sampling time was sufficient
to collect enough urea to measure, and the test run 3 procedure was main-
tained for the Series B tests as well.
5.2.2 Sample Recovery and Preparation
At the completion of each test run the train was leak checked. Then the
nozzle, probe, flexible Teflon line, first two impingers, and their connect-
ing glassware were rinsed with deionized, distilled water (three times).
The volume of the impinger contents were measured and the samples were put
in glass jars with Teflon-lined caps, as follows:
Jar #1 - Contents of the nozzle, probe, flexible Teflon line, first two
impingers, their connecting glassware, and the deionized, dis-
tilled water wash of these articles.
Jar #2 - Contents of the third and fourth impingers, their connecting
glassware, and their IN H2S04 solution rinse.
Jar 13 - Silica gel from the sixth impinger.
-79-
-------
5.2.3 Sample Analysis
5.2.3.1 Inlet
The inlet sample urea analyses were perfomed at the TRC laboratory with-
in 20 days of sample collection. Portions of both the acid impinger samples
(jar #2) and water impinger samples (jar #1) were analyzed for urea with the
p-dimethylaminobenzaldehyde (POAB) procedure. Ammonia was removed prior to
urea analyses by adding a buffer and adjusting the pH to >9.5 then boiling
the sample.
5.2.3.2 Outlet
On site urea analyses were performed on only the water impinger samples
(jar #1) from the six outlet test runs. These analyses were performed with
the PDAS method, with preliminary distillation for ammonia removal, within
24 hours of sample collection. Afterwards, both the water and acid impinger
samples were analyzed at the TRC lab for urea within 20 days of sample col-
lection by the PDAS method with preliminary distillation.
The initial on-site urea analysis of the Series A test run 1 water
impinger sample was performed according to the Method 28 procedure, and
yielded a urea concentration below the threshold of detection. The analysis
was repeated using a modification to the analysis procedure under the direc-
tion of the Technical Manager. The sample aliquot used for analysis was
increased from 100 ml as specified by Method 28 to 500 ml and then boiled
down to about 100 ml. A measurable (but still low) urea concentration was
thereby obtained. For the remaining outlet samples aliguots up to 700 ml
were used. In this way the amount of urea available for final analysis was
increased by up to a factor of seven and the sample absorbances were brought
into the working range of the calibration curves. Because two analyses were
-80-
-------
performed in the field on the Series A test run 1 sample, insufficient
sample volume remained for analysis of this sample at TRC.
No significant difference existed between the TRC analysis urea impinger
catches and the field analysis urea impinger catches. The average impinger
catches for each test series were as follows:
Average Impinger Catch (mg)
TRC Analysis Field Analysis
Series A (2 runs) 19.1 18.8
Series B (3 runs) 12.0 13.1
Average 14.8 15.4
The Series A run 1 data are not included in these averages because the field
analysis was very low (6 mg) due to the relatively short sampling time, and
no analysis at the TRC laboratory was possible (as discussed above).
5.3 Ammonia Sampling and Analysis at the Cleanable High Efficiency Air
Filter Scrubber (CHEAP)
5.3.1 Sampling and Sample Recovery
The same samples that were collected and recovered as described in
Sections 5.2.1 and 5.2.2 were analyzed for ammonia as well as urea.
5.3.1.1 Inlet
On-site ammonia analyses were performed on both water and acid impinger
samples with the Specific Ion Electrode (SIE) method within 48 hours of
sample collection. An Orion Model 95-10 ammonia electrode was used in
accordance with the electrode manufacturer's procedures.
-81-
-------
5.3.1.2 Outlet
On-site ammonia analyses were performed on portions of both the water
and acid impinger samples with the specific ion electrode (SIE) method with-
in 48 hours of sample collection.
At the TRC laboratory ammonia analyses were performed on portions of
the water and acid impinger samples by the direct nesslerization method
within 20 days after sample collection. The nessler analysis method is a
colormetric method subject to turbidity interference from a variety of
species. In addition, delays in sample analysis may allow dissolved ammonia
to diffuse out of solution, yielding reduced ammonia concentrations. Alter-
natively, delays in sample analysis may result in some species, like urea,
breaking down or converting to ammonia and yielding falsely high ammonia
concentrations.
Turbidity was not a problem during these nessler analyses. A compari-
son of the direct nessler (DM) ammonia sample weights to the SIE ammonia
sample weights does, however, show the DN results to be consistently, though
slightly, lower than the SIE results:
Average Ammonia Sample Weight (mg)
Test Series DN SIE (DN-SIE) x 100/SIE
A 1633 1675 -2.5%
B 1643 1799 -8.7%
Since the DN analyses were done after the SIE analyses, some ammonia diffu-
sion may have occured.
5.4 Visible Emissions
The visible emission measurements of the CHEAP scrubber outlet plume
was conducted by a certified visible emission observer in accordance with EPA
-82-
-------
Reference Method 9. These measurements were taken from two general loca-
tions during both the Series A and Series B test runs: atop an ammonium
nitrate holding tank and adjacent to the railroad tracks near the ammonia
storage tanks. Plume observations lasted approximately three hours, and
within an observation period readings were taken and recorded at 15 second
intervals. The background used for the observations were green trees on the
side of a mountain. Six-minute averages were calculated from the 15-second
observations.
5.5 Particle Size Tests
Particle size tests were performed at the CHEAP Downcomer (inlet) using
a Sierra Series 226 impactor with a cyclone preseparator. The impactor was
operated in its in-stack mode in accordance with the manufacturer's proce-
dures.
Prior to the initiation of sampling, the impactor was leak tested and
placed in the duct for 15 minutes to allow it to heat to duct temperature in
order to prevent condensation. Sampling began immediately upon rotation of
the nozzle into the gas stream. Sampling was performed isokinetically from
a single average flow point that was predetermined from velocity traverses
performed prior to each particle size test run. Test No. 1 was run for 7
minutes, Test No. 2 for 20 minutes, and Test No. 3 for 14 minutes. Origin-
ally the sampling periods were to have been 30 minutes each, but because of
the high loadings on the substrates isokinetic sampling was difficult to
maintain. When the required flow could no longer be maintained, sampling
was terminated.
The impactor was loaded before each test run with pre-weighed glass
-83-
-------
fiber collection substrates. Upon the completion of each test, the sub-
strates were removed in a secluded, clean area and placed in sealed petri
dishes. These samples were brought to TRC and were weighed on an analytical
balance to within 0.1 mg in a constant humidity environment.
5.6 Scrubber Liquor Sampling and Analysis
Scrubber liquor samples were collected approximately every hour during
each of the seven-hour test runs. Aliquots were collected from each of the
following locations:
Series A Test
combined
-combined
• combined
Lower sprays from solution formation.
Downcomer sump
CHEAP sump
Series B Test
Upper sprays from strippers
Middle sprays from crystallizers
Lower sprays from solution formation-
Downcomer sump
CHEAP sump
Scrubber bottom
Hot-Well-to-Sump
During Series A and B, TRC personnel collected the samples from the com-
bined lower sprays from solution formation and the Downcomer sump, and from
the CHEAP sump. During Series B, Reichhold personnel collected common samp-
les from the combined upper sprays from strippers and middle sprays from
crystallizers, and from the scrubber bottom and hot-well-to-sump.
The sample temperature was measured immediately after collection. Once
the sample reached room temperature (70 F) the pH was measured. Upon
completion of each test run, the aliquots collected during that run were
combined to form one composite sample for each location: Series A yielded
-84-
-------
two composite samples per run; Series B yielded three composite samples per
run. These composite samples were then vacuum-filtered through a tared
glass-fiber filter. Analyses for urea and undissolved solids were performed
as follows:
Urea - Sample filtrates were analyzed within 20 days after collec-
tion by the p-dimethylaminobenzaldehyde procedure in the
same manner as described in Section 5.2;
Solids - The funnel filter was desiccated and weighed to determine
undissolved solids.
TRC performed analyses on the TRC-collected liquor samples and on the scrub-
ber bottom and hot-well-to-sump samples provided by Reichhold.
5.7 Pressure Drop Measurements Across the CHEAP Scrubber
Pressure drop measurements were taken across the CHEAP scrubber during
the Series A and Series B test runs. Measurements were taken approximately
every 30 minutes during each test run using a vertical U-tube water mano-
meter connected to pressure taps across the throat of the scrubber.
5.8 Ambient Air Temperature and Relative Humidity
Ambient air temperature and relative humidity were recorded approximate-
ly every thirty minutes at the base of the prill tower during each emission
test run. Wet bulb and dry bulb temperature measurements were made with a
Bendix psychron; psychrometric tables were then used to compute relative
humidity from these measurements.
-85-
------- |