United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
EMB Report 78-NHF-3
December 1979
Air
v>EPA Urea Manufacture
Emission Test Report
W. R. Grace & Company
Memphis, Tennessee
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REPORT ON PROCESS EMISSIONS TESTS
AT THE W. R. GRACE AND CO.
UREA MANUFACTURING FACILITY
IN MEMPHIS, TENNESSEE
Thomas M. Bibb
EPA Project Manager
Clyde E. Riley
EPA Technical Manager
EPA Contract #68-02-2820
Work Assignment #9
TRC Project #0988-E80-10
Prepared By:
Willard A. Wade'III, P.E., Project Manager
Reed W. Cass, Project Engineer
July 9, 1980
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TRC-Environmental Consultants, Inc.
Willard A. Wade III, P.E.
Project Manager
July 9, 1980
Note: Mention of trade names or commercial products in this publication
does not constitute endorsement or recommendation for use by the
Environmental Protection Agency.
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PREFACE
The work reported herein was performed by personnel from TRC Environmental
Consultants, Inc. (TRC), The GCA/Technology Division (GCA), W. R. Grace and
Co., Memphis, Tennessee, and the U.S. Environmental Protection Agency (EPA).
The scope of work, issued under EPA Contract No. 68-02-2820, Work
Assignment No. 9, was under the supervision of the TRC Project Manager, Mr.
Willard A. Wade, III. Mr. Reed W. Cass of TRC served as Project Engineer and
was responsible for summarizing the test and analytical data presented in this
report. Sample analysis was performed at the W. R. Grace and Co., Memphis,
Tennessee plant under the direction of Ms. Margaret M. Fox, and at the TRC
laboratory in Wethersfield, Connecticut under the direction of Mr. David F.
Dawson.
Mr. Mark L. Bornstein and Mr. Timothy L. Curtin of GCA were responsible
for monitoring the process operations during the emissions testing program.
GCA personnel were also responsible for preparing Section 3.0, Process
Description and Operations, and Appendix L of this report.
Personnel of W. R. Grace and Co. , Memphis, Tennessee whose assistance and
guidance contributed greatly to the success of this emission test program
include Mr. Norman E. Picquet, General Manager, and Mr. George T. Griesheimer,
Manager, Chemical Services Department.
Mr. Eric A. Noble, Office of Air Quality Planning and Standards,
Industrial Studies Branch, EPA, served as Test Process Project Engineer and
was responsible for coordinating the process operations monitoring.
Mr. Clyde E. Riley, Office of Air Quality Planning and Standards, Emission
Measurement Branch, EPA, served as Technical manager and was responsible for
coordinating the emission test program.
11
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TABLE OF CONTENTS
Preface ii
SECTION PAGE
1.0 INTRODUCTION 1
1.1 Background 1
1.2 Brief Process Description 3
1.3 Emissions Measurement Program 3
2.0 SUMMARY OF RESULTS 6
2.1 Prill Tower Scrubber Urea Collection Efficiencies . . 6
2.2 Prill Tower Emissions Test Results 8
2.3 Synthesis Tower Main Vent Emissions Test Results . . 25
2.4 Visible Emissions 27
2.5 Particle Size Tests 33
2.6 Volumetric Flowrates in the Prill Tower Scrubber
Inlets 33
2.7 Pressure Drops Across the Prill Tower Scrubbers ... 45
2.8 Analysis of the Scrubbing Liquor 45
2.9 Ambient Air Temperature and Relative Humidity .... 45
2.10 Process Product Sampling 50
3.0 PROCESS DESCRIPTION 52
3.1 Process Equipment 52
3.2 Emission Control Equipment 55
3.3 Production Rate Monitoring 56
3.4 Production and Control Equipment Monitoring 58
3.5 General Plant Operation 62
4.0 LOCATION OF SAMPLING POINTS 63
4.1 Prill Tower Scrubber Inlets 63
4.2 Scrubber A and C Outlets 68
4.3 Inlet Particle Sizing Locations 68
4.4 Urea Synthesis Tower Main Vent Sampling Location . . 70
4.5 Visible Emissions Observation Locations 70
4.6 Scrubber Pressure Drop Measurement Locations .... 75
4.7 Process Sample Collection Locations 75
4.8 Scrubber Liquor Collection Locations 75
4.9 Ambient Air Temperature and Relative Humidity .... 75
5.0 SAMPLING AND ANALYSIS METHODS 77
5.1 EPA Reference Methods Used in this Program 77
5.2 Urea Sampling and Analysis at the Prill Tower
Scrubbers 79
5.2.1 Sampling Methods 79
5.2.2 Sample Recovery and Preparation 82
5.2.3 Sample Analysis 82
ill
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TABLE OF CONTENTS (Continued)
SECTION PAGE
5.3 Ammonia Sampling and Analysis at the Prill Tower
Scrubbers 83
5.3.1 Sampling, Sampling Recovery and Preparation .... 83
5.3.2 Sample Analysis 83
5.4 Formaldehyde Sampling and Analysis at the Prill Tower
Scrubbers 85
5.5 Insoluble Particulate Sampling and Analysis at the
Prill Tower Scrubbers 85
5.6 Synthesis Tower Emissions Tests 85
5.6.1 Sampling and Analysis for Urea and Ammonia .... 85
5.6.2 Integrated Gaseous Bag Samples 87
5.7 Visible Emissions 87
5.8 Particle Size^Tests 89
5.9 Volumetric Flowrate Measurements in the Scrubber
Inlets 90
5.10 Pressure Drop Measurements Across Prill Tower
Scrubbers 91
5.11 Scrubber Liquor Sampling and Analysis 91
5.12 Ambient Air Temperature and Relative Humidity .... 92
5.13 Process Samples 92
IV
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LIST OF FIGURES
FIGURES PAGE
1-1 Process Flow Diagram
2-1 Six Minute Average Opacity Readings for Prill Tower
Scrubber C during Fertilizer Tests 28
2-2 Six Minute Average Opacity Readings for Prill Tower
Combined Scrubbers A-H during Fertilizer Tests . . 29
2-3 Six Minute Average Opacity Readings for Prill Tower
Scrubber A during Feed Tests 30
2-4 Six Minute Average Opacity Readings for Prill Tower
Scrubber C and Combined Scrubbers A-D during
Feed Tests 31
2-5 Cumulative Size Distributions of Particulate in
Scrubber A during Fertilizer Tests 36
2-6 Cumulative Size Distributions of Particulate in
Scrubber C during Fertilizer Tests 37
2-7 Cumulative Size Distributions of Particulate in
Scrubber A during Feed Tests 40
2-8 Cumulative Size Distributions of Particulate in
Scrubber C during Feed Tests ~.~.~ . . 41
3-1 Process Flow Diagram 53
4-1 Overhead View of Prill Tower 64
4-2 Schematic of Prill Tower and Typical Scrubber .... 65
4-3 Scrubbers A and C Inlet Sampling Locations 66
4-4 Scrubbers B, D, E, F, G and H Inlet Sampling
Locations 67
4-5 Scrubbers A and C Outlet Sampling Locations 69
4-6 Synthesis Tower Main Vent Sampling Location 71
4-7 Visible Emission Observer Locations (Ground Level). . 73
4-8 Visible Emission Observer Locations (Atop Prill
Tower) 74
4-9 Scrubber Liquor Sampling Points on Prill Tower ... 76
5-1 Modified EPA Particulate Sampling Train 80
5-2 Typical In-Stack Orifice and Nozzle Assembly .... 88
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LIST OF TABLES
PAGE
Summary of Urea Scrubbing Efficiency of
Scrubbers A and C During Emissions Testing .... 7
2-2a Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Entering and Exiting Prill Tower
Scrubber A on August 15-17, 1979 (English) .... 9
2-2b Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Entering and Exiting Prill Tower
Scrubber A on August 15-17, 1979 (Metric) 10
2-3a Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Entering and Exiting Prill Tower
Scrubber C on August 15-17, 1979 (English) .... 11
2-3b Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Entering and Exiting Prill Tower
Scrubber C on August 15-17, 1979 (Metric) 12
2-4a Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Entering and Exiting Prill Tower
Scrubber A on August 20-22, 1979 (English) .... 13
2-4b Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Entering and Exiting Prill Tower
Scrubber A on August 20-22, 1979 (Metric) 14
2-5a Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Entering and Exiting Prill Tower
Scrubber C on August 20-22, 1979 (English) .... 15
2-5b Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Entering and Exiting Prill Tower
Scrubber C on August 20-22, 1979 (Metric) 16
2-6 Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Entering the Prill Tower Scrubber A
on August 15-17, 1979 17
2-7 Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Exiting the Prill Tower Scrubber A
on August 15-17, 1979 18
2-8 Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Entering the Prill Tower Scrubber C
on August 15-17, 1979 19
2-9 Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Exiting the Prill Tower Scrubber C
on August 15-17, 1979 20
VI
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LIST OF TABLES (Continued)
TABLE • PAGE
2-10 Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Enter-ing the Prill Tower Scrubber A
on August 20-22, 1979 21
2-11 Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Exiting the Prill Tower Scrubber A
on August 20-22, 1979 22
2-12 Summary of Results of Urea, Ammonia and Formaldenyde
Tests on Gases Entering the Prill Tower Scrubber C
on August 20-22, 1979 23
2-13 Summary of Results of Urea, Ammonia and Formaldehyde
Tests on Gases Exiting the Prill Tower Scrubber C
on August 20-22, 1979 24
2-14 Summary of Results of Urea, Ammonia and Formaldehyde
Sampled at the Synthesis Tower Main Vent on
August 22, 1979 26
2-15 Visible Emission Observation Locations 32
2-16 Summary of Inlet Particle Sizing Test Results on
Scrubbers A and C During Fertilizer Grade Urea
Production 34
2-17 Summary of Inlet Particle Sizing Test Results on
Scrubbers A and C During Feed Grade'Urea
Production 38
2-18 Scrubber inlet Flowrates 42
2-19 Summary of Velocity Head (Inches Water) and Temperature
(°F) Measurements on Scrubber Inlets Not Tested
for Emissions 44
2-20 Summary of Scrubbers A and C Liquor Analysis Results
Fertilizer Grade Urea Production 46
2-21 Summary of Scrubbers A and C Liquor Analysis Results
Feed Grade Urea Production 47
2-22 Ambient Air Temperature and Relative Humidity
Measurements During Fertilizer Grade Urea
Production 48
2-23 Ambient Air Temperature and Relative Humidity
Measurements During Feed Grade Urea
Production 49
VII
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LIST OF TABLES (Continued)
TABLE PAGE
2-24 Summary of Bulk Density and Sieve Analyses on the
Unscreened Product Samples 51
3-1 Average Production Rates During Emission Tests ... 57
3-2 Relative Values of Operating Parameters During
Fertilizer Grade Prill Tower Emission Tests .... 59
3-3 Relative Values of Operating Parameters During
Feed Grade Prill Tower Emission Tests 60
3-4 Relative Values of Operating Parameters During
Synthesis Vent Emission Testing 61
4-1 Visible Emission Observation Locations 72
Vlll
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APPENDICES
A Urea, Ammonia and Formaldehyde Emission Test Results
A.I Prill Tower Scrubbers A and C Inlets - Fertilizer
A.2 Prill Tower Scrubbers A and C Outlets - Fertilizer
A.3 Prill Tower Scrubbers A and C Inlets - Feed
A.4 Prill Tower Scrubbers A and C Outlets - Feed
A.5 Example Equations and Sample Calculations
A.6 Urea Synthesis Tower Main Vent
B Field Data Sheets and Sampling Task Logs for Urea, Ammonia and
Formaldehyde Testing
B.I Prill Tower A and C Scrubber Inlets - Fertilizer
B.2 Prill Tower A and C Scrubber Outlets - Fertilizer
B.3 Prill Tower A and C Scrubber Inlets - Feed
B.4 Prill Tower A and C Scrubber Outlets - Feed
B.5 Urea Synthesis Tower Main Vent
C Visible Emissions Results
C.I Visible Emissions Summary Tables
C.2 Visible Emissions Recertification Certificate
C.3 Guidelines for EPA Method 9
C.4 Visible Emission Field Data Sheets
D Particle Size Tests
D.I Discussion of Particle Size Testing
D.2 Particle Size Field Data Sheets
D.3 Lab Weighing Data
Miscellaneous Field Data
E.I Scrubber Liquor Samples
E.2 Prill Tower Scrubber Pressure Drop
E.3 Ambient Air Temperature and Relative Humidity Measurements
E.4 Bulk Density and Sieve Analysis
Velocity Traverse Data for All Prill Tower Scrubbers
F.I Velocity Traverses - Fertilizer
F.2 Velocity Traverses - Feed
F.3 Summary Tables of Cyclonic Flow Angles
F.4 Single-Point Velocity Measurements on Scrubbers B, D, E, F, G, H
Cyclonic Flow Reference Documents
Daily Summary Logs
IX
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APPENDICES
(Continued)
I Sampling And Analytical Procedures
I.I Urea
1.2 Ammonia
1.3 Formaldehyde
1.4 In-stack Orifice Development
J Analytical Data
J.I Summary of Analytical Results
J.2 Summary of Analytical Procedures
J.3 Discussion of Methods and Results
J.4 Audit Samples
J.5 Cleanup Evaluation
J.6 Sample Recovery and Preservation
J.7 Laboratory Notebook
J.8 Water Gain Results: Impingers and Silica Gel
K Sampling Train Calibration .Data
K.I Orifice Calibrations
K.2 Nozzle Measurements
K.3 Pitot-Tube Calibrations
L Process Operations Log
M Project Participants
N Scope of Work
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1.0 INTRODUCTION
1.1 Background
Section 111 of the Clean Air Act of 1970 charges the Administrator of. the
(1
United States EnvironmentOiprotection Agency (EPA) with the responsibility of
establishing Federal standards of performance for new stationary sources which
may significantly contribute to air pollution. When promulgated, these
standards of performance for new stationary sources (SPNSS) are to reflect the
degree of emission limitation achievable through application of the best
demonstrated emission control technology. 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
W. R. Grace and Co. urea manufacturing plant in Memphis, Tennessee, as a site
for an emission test program. This plant produces feed and fertilizer grade
urea, and is considered to employ process and emission control technology
representative of modern urea solution formation and fluidized-bed prilling
processes.
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. Figure
1-1 shows a flow diagram of the complete urea production process. Emission
tests were performed during August 1979 on the inlets and outlets of two of
the eight prill tower scrubbers during production of both fertilizer and feed
grade urea. In addition, emission tests were performed on the main solution
formation vent on the synthesis tower during the production of feed grade urea.
-1-
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TO ATMOSPHERE
SCRUBBER LIQUOR FROM
1
1
NH3
CO,
AHW
3NIA RECOVERY SYSTEM
TO ATMOSPHERE
SOLUTION
PRODUCTION
SHAM PROGETTI
TniAi oprvri (
••••»
UREA
SURGE
TANK
OVERHEADS
MHHM
r
IS
ill
o
••*
IK
rf
1st STAGE
CONCENTRATOR
2nd STAGE -
rvApnoATnn
/^~
^_
DENOTES PRODUCT FLOW
MODIFIED JOY
TURBULAIRE SCRUBBER
(8 EACH)
I WET SCRUBBER I
PRODUCT I
r
CONVEYOR
FIGURE 1-1: PROCESS FLOW DIAGRAM, W.R. GRACE AND CO.,
MEMPHIS, TENNESSEE
098ft-001
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1.2 Brief Process Description
Urea is produced in a single production line by reacting ammonia and car-
bon dioxide using the Snamprogetti total recycle process. The urea solution
leaving the sythesis process proceeds to a two-stage evaporator where it is
concentrated to 99+ percent urea. A formaldehyde additive is added to prevent
caking of the product. The urea melt is pumped directly to the top of the
prill tower and then sprayed downward against an induced countercurrent of
air. As they fall, the melt droplets solidify. These solid prills are cooled
at the base of the tower by a fluidized bed cooler and are sent through a set
of sizing screens. Correctly sized prills are then conveyed to a bulk ware-
house for bagging or bulk-loading of trucks or railcars.
Eight impingement scrubbers (labelled A through H) located on the roof of
the prill tower control the air flow through the prill tower and fluidized-bed
cooler. The conveyor transfer points and bagging operation are controlled by
a wet scrubber and a baghouse, respectively.
1.3 Emissions Measurement Program
The emissions measurement program was primarily conducted August 13-22,
1979 at the W. R. Grace and Co., Memphis, Tennessee urea manufacturing plant.
In addition, visible emissions observations on the bagging operation baghouse
were performed on December 18, 1979. The measurement program consisted speci-
fically of the following:
Prill Tower Measurements (Fertilizer and Feed Grade)
1. Urea, ammonia, formaldehyde, and insoluble particulate in the inlet
and outlet gas streams of scrubbers A and C.
2. Particle size distributions in the inlet gas streams of scrubbers A
and C.
-3-
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3. Visible emissions from individual and combined scrubber outlets, ana
from the baghouse controlling the bagging operation.
4. Gas pressure drop across all scrubbers.
5. Urea, ammonia, formladehyde and solids content, temperature and pH of
the inlet and outlet liquors of scrubbers A and C.
6. Bulk density and sieve analysis of the prill tower unscreened product.
7. Volumetric flowrates of the scrubbers not tested for emissions.
8. Ambient air temperature and relative humidity during emission tests.
Urea Synthesis Tower Measurements (Feed Grade)
1. Urea, ammonia and insoluble particulate in the gas stream of the main
vent.
2. Oxygen and carbon dioxide content of the main vent gas stream, using
integrated gaseous bag samples.
TRC personnel were responsible for collecting the above emissions data.
Concurrently, GCA was responsible for monitoring and recording pertinent pro-
cess operation parameters. Concurrent test runs were conducted at the outlet
and inlet on scrubbers A and C. The chronology of these runs and other emis-
sions tests is contained in the Daily Summary Logs in Appendix H. Most inter-
ruptions (labelled as "stop" in the logs) that occurred during the scrubber
test runs were due to scrubber operational procedures or skipping over no-flow
points.
The following sections of this report present the results of the fertili-
zer grade and feed grade emissions tests (Section 2.0), process description
(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.
-4-
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Appendix J.5 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, ammonia and formaldehyde. The unexposed
impinger contents were then recovered, prepared and analyzed according to pro-
cedure in order to establish background/contamination levels resulting from
the sampling equipment itself.
Appendix J.4 contains the results of audit sample analyses. Urea stand-
ards were prepared by EPA and were then analyzed by TRC in accordance with EPA
instructions in order to assess the accuracy of the urea analysis procedure.
-5-
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2.0 SUMMARY OF RESULTS
This section presents summary tables of results and narrative on the
emissions testing conducted during the weeks of August 13-17 and August 20-24,
1979, at the W. R. Grace and Co. urea manufacturing facility in Memphis,
Tennessee. Testing was performed on gas and liquid streams entering and
exiting the prill tower scrubbers, and on the gas stream venting from the urea
synthesis tower. One additional day of visible emissions observations was
performed on December 18, 1979.
During the week of August 13-17, 1979, the plant was producing fertilizer
grade urea. The following week the plant was producing feed grade urea.
Urea concentrations were determined with the p-dimethylaminobenzaldehyde
colorimetric (with preliminary distrillation) analysis method. Two methods of
ammonia analysis were used throughout this testing program: the direct
Nessler method and the specific ion electrode method. The direct Nessler
analysis results are presented here as the primary ammonia data. Formaldehyde
concentrations were determined with the chromotropic acid method. All four
analysis methods are discussed in Section 5.0 and in Appendices I and J.
2.1 Prill Tower Scrubber Urea Collection Efficiencies
The calculated urea collection efficiencies for prill tower scrubbers A
and C are shown in Table 2-1. For scrubber A the fertilizer scrubber effici-
ency was consistently slightly higher than the feed scrubber efficiency. For
scrubber C, the opposite was true. Overall, the average combined scrubber
efficiencies were essentially the same for fertilizer and feed production
(85.6% and 86.6%, respectively).
-6-
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TABU- 2-1
SIMIARY or UREA SCRUBBING i;.rncn:.NCY or- SCRUBBERS A AMP c
DURING EMISSIONS Ti;ST[NG AT
W.R. GRACP. AM) CO., MBfllllS, TENNESSEE
Run Number
Product Grade
Run 1
Fertilizer
Feed
Run 2
Fertilizer
Feed
Run 3
Fertilizer
Feed
Average _^
Fertilizer Feed
D;it.c
08-15-79 08-20-79
08-16-79 '08-21-79
08-17-79 08-22-79
Scrubber Identification
Scrubber Efficiency
(Percent)
93.7 88.9 93.5 92.7
88.2 72.8 86.7 84.2 90.7 78.6 82.7 82.6 90.6 80.6 87.1 86.2
Average KEficiency
(Percent)
91.3
93.1
80.0
85.5
84.7
82.7
85.6
86.6
* These values do not represent exact averages of the individual run efficiencies. As noted on Tables 2-2 through 2-5, sample weights were averaged;
then from these average sample weights, average mass flow rates and efficiencies were calculated. Conversion factors and rounding met hex! s niay
yield minor discrepancies between average efficiencies calculated this way and averages calculated from the individual run efficiencies.
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2.2 Prill Tower Emissions Test Results
Tables 2-2 (Scrubber A) and 2-3 (Scrubber C) present the urea, ammonia ana
formaldehyde results for the fertilizer test runs. Tables 2-4 (Scrubber A)
and 2-5 (Scrubber C) present the same data for the feed test runs. Both inlet
and outlet data are on all these tables, and only the direct Nessler ammonia
data are shown. The average scrubbing efficiencies are as follows:
Collection Efficiencies (percent)
Fertilizer
Scrubber
A
B
Urea
90.6
80.6
Ammonia
0
0
Form.
96.6
93.2
Urea
87.1
86.2
Feed
Ammonia
53.3
46.1
Form.
76.6
73.1
Why the ammonia scrubbing efficiency for both scrubbers is less than zero for
the fertilizer test runs is not evident. The major differences between the
fertilizer and feed products are that the feed product is smaller in size and
more formaldehyde is -added to the feed production process. Ammonia stripping
by the scrubbing liquor was initially suspected. The scrubber liquor analysis
data (Section 2.9), however, show no evidence of ammonia stripping.
Tables 2-6 through 2-9 show the fertilizer data for both scrubbers, with
the individual inlet and outlet data on separate tables; Tables 2-10 through
2-13 show the feed data. The insoluble particulate data and the results of
both ammonia analysis methods are shown on these separated inlet and outlet
tables.
As is discussed in Sections 2.6 and 5.1, cyclonic flow was evident in all
the prill tower scrubber inlets; no cyclonic flow was evident in the outlets.
Maintaining isokinetic sampling under cyclonic flow conditions is difficult at
best. This difficulty is reflected in the calculated percent isokinetics (I)
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TABLE 2-2a (English)
SUNMARY OF RESULTS OF UREA, AT-MONIA AND FORMALDEIIYDE TESTS
OF GASES ENTERING AND EXITING PRILL TOWER SCRUBBER A
ON AUGUST 15-17 1979 AT W.R. GRACE AND CO., INC.
MEMPHIS, TENNESSEE
RUN NUMBER
DATE
IOCATION
VOLUME OF GAS SAMPLED (DSCF)a
STACK GAS FLOWRATE (DSCFM)5
STACK TEMPERATURE (°F)
PERCENT MOISTURE
PERCENT ISOKINETIC
PRODUCTION RATE (TONS/HOUR)
UREA DATA0
Total Sampling Weight (milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (percent)
AMMONIA DATAd
Total Sample Weight (milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (percent)
FORMALDEHYDE PATAe
Total Sample Weight (milligrams)
Grains/IXSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (percent)
Fertilizer 1
08-15-79
Inlet Outlet
Fertilizer 2
08-16-79
Inlet Outlet
Fcrtilizer 3
08-17-79
Inlet Outlet
Average'
0.
0
0.
1.31
000204
.1148
002 639
96
0.0578
0.
0
0.
i
0000082
.00437
0001005
0
0
1.92
.000285
0.168.3
.003675
96
0.0706
0.
0
0.
.9
0000102
.00529
0001155
0
0
1.75
.000281
0.1 «J9
.003712
9d .
C
0.
0
0.
.()
1.0761
00001 1 1
.00570
0001201)
Outlet
99.14
65630
113
2.382
108 .0
43.5
449
0.0699
39.35
0.905
93.7
182
0.0283
15.93
0.366
<0
109.2
62180
90
3.655
98.4
43.5
33.0
0.00465
2.478
0.0570
745
0.1051
56.01
1.287
104 . 1.
68880
112
1.881
106.4
45.8
622
0.0922
54.43
1.188
253
0.0375
22 . 1 4
0.483
106.4
60510
90
3.556
98.5
45.8
85.4
0.01236
6.410
0 . 1 399
88.2
821
0.1188
61.61
1.345
<0
95.94
70130
lib
1.844
97.8
45.5
502
0.0807
48.51
1.000
90.7
236
0.038(1
22.8-1
0.502
• 0
105.9
60530
89
3.677
98.1
45.5
59 . 7
0.008()8
4.503
0.0990
683
0.0993
51.51
1.132
99 . 7 1
(>.S27.0
111
2.031)
KM .1
44.9
52-1
O.IIK) I
47 . 13
1 .0511
224
0.0347
20.29
0.452
1(17.2
01073
90
3.1)33
98 . 3
44.9
59 . 4
II.IHI.S53
•1 . •)(>(>
0.0995
90. (,
750
0. 1077
So. 37
1.255
• I)
!.(><> O.OI>X2
0.11(111257 O.OOOU09S
O.ir.u3 (1.00513
0.003VI7 n.mini 142
a Dry standard cubic feet @ 68°F and 29.92 inches llg
b Dry standard cubic feet per minute
c p-dJmethylamino benzaldehyde colorimetric (with preliminary distillation) analysis method
d Direct Nessler analysis method.
e Chroinotropic acid analysis method
* Only sample weights from all three runs were averaged, and then mass flow rates and efficiencies were calculated from thosi- averar.i- s-implr
-------
TABLE 2-2b (Metric)
SUMMARY OF RESULTS OP UREA. AIWONIA, AND FORMALDEHYDE TESTS
ON GASES ENTERING AND EXITING PRILL TOWER SCRUBBER A
ON AUGUST 15-17, 1979 AT W.R. GRACE AND CO., NDiMPTTTsTTENNESSF.!;
o
I
Run Number
Date
Legation
Volume of Gas Sampled (Mm3 a).
Stack Gas Plow Rate (Nhi3/min )
Stack Temperature (°C)
Percent Moisture
Percent Isokinetic
Product ion Rate (Mg/llour)
Urea Data c
Total Sample Weight (Milligrams)
Grams/Nin3
Kg/Hour
Kg/Mg
Collection Efficiency (Percent)
Ammonia Data
Total Sample Weight (Milligrams)
Grams/Nin3
Kg/Hour
Kg/Mg
Collection Efficiency (Percent)
l:oniialdehyde IXita
Total Sample Weight (Milligrams)
Grams/Mm3
Kg/I lour
Kg/Mg
Collection Efficiency (Percent)
Fertilizer I
08-15-79
Inlet
2.8076
1860.1
45
2.382
108.0
39.46
449
0.1599
17.849
0.4525
93
182
0.06475
7.226
0.1830
Outlet
3.0925
1760.94
32
3.655
98.4
39.46
33.0
0.01064
1.124
0.0285
.7
745
0.24048
25.406
0.6435
Fertilizer 2
08-16-79
Inlet
2.9481
1950.7
44
1.881
106.4
41.55
622
0.2110
24.689
0.5940
88.
253
0.08580
in. 043
0.2415
Outlet
3.0133
1713.64
32
3.556
98.5
41.55
85.4
0.02828
2.907
0.06995
,2
821
0.27183
27.946
0.6725
Pert i 1 izer 3
Average *
08-17-79
Inlet
2.7170
1986.1
47
1.844
97.8
41.28
502
0.18465
22.004
0.5330
236
0.08695
in. 360
0.2510
Outlet
2.9991
1714.21
32
3.677
98 . 1
41 .28
59.7
O.OI98(i
2.043
0.0495
90 . 7
683
0.22721
23.365
0.56h
Inlet
2.8243
1932.3
46
2.036
1(11.1
4(1.73
524
0.18556
21.514
0.5280
224
0.07940
9. JIM
0.2260
Out let
3.035(1
1729.59
32
3.6.33
98 . 3
4(1.73
59.4
0. (II 95 2
2.02(.
0.04 '.IS
90.6
750
0.24643
.'5.51.9
li.()275
<0
1.31 0.0578
0.000467 0.0000188
0.05207 0.00198
0.001320 0.00005025
96.2
<0
1.92 0.0706
0.000652 0.0000233
0.07634 0.00240
0.001838 0.00005775
96.9
1.75
0.000643
0.07661
0.001856
0.0761
0.0000254
0.00261
0.00(106.33
96.6
1.66
0.00058S
O.M6KI.S
O.IHIII.7-1
0.06S2
ll.lll 1 7 38
(1.110233
II.IIIIIIO.S7I
96. (>
a Normal cubic meters P 20°C, 760 mm llg.
b Normal cubic meters per minute.
c p-diitiJthylamino bcnzaldehydc colorimetric (with preliminary distillation) analysis method.
d Direct Nessler Analysis method.
e Chromotropic Acid Analysis method.
* Only sample weights from all three runs were averaged, and then mass flow rates and efficiencies were calculated from these average sample wights.
-------
TABLB 2-3a (English)
SUMMARY OF RESULTS OF UREA, AWON1A AND FORMALDEHYDE TESTS
ON GASES ENTERING AND EXITING '1111- PRIM, TOWER SCRUBBER C
ON AUGUST 15-17, 1979 AT W.R.GRACE AND CO., INC.
MliMPIHS, TENNESSEE
RUN NUMBER
DATE
l.a:ATION
VOI.IM: OF GAS SAMPLED
STACK CAS FLOWRATE (DSCFM)b
SfACK TEMPERATURE (°F)
PERCENT MOISTURE
PERCENT ISOKINETIC
PRODUCTION RATE (TONS/I IOUR)
UREA DATAC
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (Percent)
ANMON1A f)ATAd
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Collection efficiency (Percent)
FORMALDEHYDE HATAe
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (Percent)
Fertilizer 1
Fertilizer 2
Fertilizer 3
Average*
08-15-79
Inlet
Outlet
101.1
62360
113
2.029
120.1
43.5
99.84
56220
86
3.314
99.8
43.5
135
0.0206
11.01
0.253
167
0.0258
12.41
0.285
<0
08-16-79
08-17-79
Inlet
Outlet
Inlet
Outlet
82.54
53660
111
1.395
121.3
45.8
98.08
56450
80
3.371
97.6
45.8
87.38
591150
116
1.371
114.3
45.5
109.4
62-110
82
4.012
'J8.5
45.5
127
0.0237
10.90
0.238
255
0.04004
19.37
0.423
173
0.0306
15.49
0.340
245
0.03449
18.45
0.405
0.849
0.041
0.0001296 0.0000063
0.06927
0.001592
0.003047
0.0000700
95.6
0.582
0.0001088
0.05004
0.001093
I
0.068
0.0000107
0.005165
0.0001128
39.7
0.790
0.00013%
0.07066
0.001553
93.
0.0625
0.0000088
0.004706
0.0001034
7,
90.34
5S3S7
113
i. 598
118.6
4-1.'.I
1(12.4
58360
83
3.56d
'.18.6
44.9
304
0.0464
24.80
0.570
37
0.00571
2.750
0.0632
88.9
217
0.04C6
18 . 67
0.408
67
0.01052
5.089
0.1111
72.8
275
0.0486
24 . 60
0.541
78 .6
70
0.00985
5.270
0.1158
265
0.0453
22.66
0.505
80
58
0.00872
4 .3(>3
0.0972
.6
145 222
(1.02-18 n.03339
12.11 10.70
0.276 0.372
••0
0.7-10 0.057
O.OOIH201 ll.ODlllill.Sd
0.(I(»o25 0.004287
O.OOI4O8 0.00009 5 !>
93 . 2
a Dry Standard Cubic Feet § 68 F and 29.92 inches llg.
b Dry Standard Cubic Feet per minute.
c p-dimethylamino benzaldehyde colorimetric (with preliminary distillation) analysis method.
cl Direct Nessler analysis method.
e Chromotropic acid analysis method.
* (Inly sample weights from all three runs were averaged, and then mass flow rates
and efficiencies were calculated from these averaged sample weights.
-------
TABLE 2-5h (Metric)
SUM4ARY OF RESULTS Ol: UREA, AM-DNTA AND FORMAI.DIiHYDI- TI-STS
ON CASES ENTERING AND MX I TING Till- PRILL TOWF.R SCRUBBER C
ON AUGUST 15-17, 1979 AT W.R. GRACE AND CO., MEMPHIS, TENNESSEE
N5
I
Run Number
Date
Location
Volume of Gas Sampled (Nm3 ).
Stack Gas Flow Rateo(Nm3/min ")
Stack Temperature ( C)
Percent Moisture
Percent Isokinetic
Production Rate (Mg/llour)
Urea Data c
Total Sample Weight (Milligrams)
Grams/Mm3
Kg/Hour
KB/MB
Collection Efficiency (Percent)
Ammonia Data
Total Sample Weight (Milligrams)
Granis/Nin3
Kg/Hour
KB/MB
Collection Efficiency (Percent)
Formaldehyde Data
Total Sample Weight (Milligrams)
Graiiis/Nm3
Kg/Hour
KB/MB
Collection Efficiency (Percent)
Fertilizer 1
08-15-79
Inlet
2.86315
1776.0
45
2.029
120.1
39.46
Outlet
2.82747
1592.2
30
3.314
99.8
39.46
Fertil
izer 2
08-16-79
Inlet
2.33753
1519.7
44
1.395
121.3
41.55
Outlet
2.77763
1601.2
27
3.371
97.6
41.55
Fertil
izer 3
Average *
08-17-79
Inlet
2.47460
1672.3
47
1.371
114.3
41.28
Outlet
3.09821
1767.5
28
4.012
98.5
41.28
Inlet
2.55S-I3
1652.7
•16
1 . 5'.m
HH.h
40.73
Out lot
2.8991)7
1652.7
28
3.5dd
!>H.t>
40.73
304
0.10617
11.249
0.285
37
0.01307
1.247
0.0316
88.9
217
0.09290
8.469
0.204
72.8
67
0.02407
2.308
0.0556
275
0.11120
11.159
0.271
70
0.022538
2 . 390
0.0579
78.6
265
0.103(iT>
10.279
0.253
58
0.01995
1 . 9" 9
O.O-ISd
80.6
135
0.04713
4.994
0.127
167
0.05903
5.629
0.1425
<0
0.849
0.0002965
0.031421
0.000796
0.041
0.0000144
0.001382
0.000035
127
0.05423
4.944
0.119
255
0.09161
8.786
0.2115
173
0.07002
7.026
0.170
245
0.07892
8.369
0.2025
0.582 0.068
0.0002489 0.0000245
0.022698 0.002343
0.000547 0.000056
88.9
145
O.H5(>7-I
5.629
0.138
O.llTdlll
7 .575
II. 1S(>
0.790
0.0003194
0.032051
0.000777
92,
0.0625
0.0000201
0.002135
0.000052
.8
0.7-10
M.OOOJ892
O.OJKdSl
0.000701
0.059
II .OIMIII197
0.001945
II. mil in. IK
92.8
a Normal cubic meters @ 20 C, 760 mm llg.
1) Normal cubic meters per minute.
c p-dimethylamino benzaldehyde colorimetric (with preliminary distillation) analysis method.
d Direct Nessler Analysis method.
e Chroino tropic Acid Analysis method.
* Only sample weights from all three runs were averaged, and then mass flow rates and efficiencies were calculated from these average sample heights.
-------
TABI.P. 2-4a (P.nglish)
SUNMARY OF'RF.SULTS op UREA, ANMONIA AND FORMAU>I;IIYDI- TI-STS
ON GASBS HNTI-RING AND EXITING PRII.I. TOWEK SOaJBIiER A
ON AUGUST 20-22, 1979, AT W.R. ORACH AND CO., "
Run Number
Date
Location
Volume of Gas Sampled (DSCP.a)
Stack Gas Plowrate (DSCIW )
Stack Temperature ( P)
Percent Moisture
Peixent Isokinetic
Production Rate (Tons/Hour)
Urea Data c
Total Sample Weight. (Milligrams)
Grains/DSC!1
Poiuids/llour
Pounds/Ton
Collection Efficiency (Percent)
Ammonia Data c
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (Percent)
Formaldehyde Data e
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (Percent)
Feed 1
08-20-79
Inlet Outlet
Peed 2
Peed 3
Average
08-21-79
08-22-70
Inlet
Outlet
Inlet
Outlet
Inlet
OutIrt
75.79
51720
189
2.731
106.0
47.2
380
0.0774
34.31
0.727
93
512
0.1043
46.24
0.980
53
0.409
0.0000833
0.0369
0.000782
73
90.18
49750
]()6
5.472
101.6
47.2
30.4
0.00519
2.213
0.0469
.5
293
0.05004
21.33
0.452
.9
0.133
0.0000227
0.00968
0.0002052
.8
77.72
51720
189
3.416
108.1
47.4
590
0.1172
51.96
1.096
86.7
570
0.1132
50.18
1.059
57.3
0.622
0.0001235
0.0547
0.001154
76.1
76.09
42270
103
5.291
100.9
47.4
94.0
0.01902
6.892
0.1454
292
0.05910
21.41
0.452
0.178
0.000360
0.01305
0.0002753
77.92
53010
182
2.509
106.6
45.9
534
0.1058
48.07
1.047
82.
636
0.1260
57.25
1.247
49.
0.644
0.0001275
0.0579
0.001261
78.
88.89
50390
97
5.377
98.9
45.9
111
0.01923
8.305
0. 1809
7
390
(1.06757
29.18
0.636
0
O.ldd
0.0(100:88
0.01212
0.0002706
5
77.14
5215H
184
2.885
106. 9
Hi. S
501
0. 10112
•14.79
0.957
574
0.1148
51.32
1.097
0.558
0.0001 12
O.OSOIKi
n.nnliiTn
85.05
r-!70
102
5. 380
100.5
4I..8
78.5
0.01421
5.782
0. 1236
87.1
325
0.05885
23.94
0.512
53.3
0. 159
0.000288
0.01 171
o.ooo25o3
7d. (i
a Dry standard cubic feet @ 68 F, 29.92 inches llg.
b Dry standard cubic feet per minute.
c p-diinethylamino benzaldeltyde colorimetric (with preliminary distillation) analysis method.
d Direct Nessler Analysis method.
e Chromotropic Acid Analysis method.
* Only sample weights from three runs were averaged, and then mass flow rates and efficiencies were calculated from these average sample ueighls.
-------
TABU: 2-4h (Metric)
SUMMARY OF RESULTS OF UREA, AMENTA AMI) FORMALDFJIYDE TESTS
ON GASES HNTERFNG AND EXITING Till; PRILL TOWER SCRUBBER A ON AtlQIST 20-22, 1970
-p-
I
Run Number
Date
Location
Voliune of Gas Sampled (Mm3 a).
Stack Cas Flow Hate (Nm3/min )
Stack Temperature (°C)
Percent Moisture
Percent Isokinetic
Production Rate (Mg/Hr)
Urea Data c
Total Sample Weight (Milligrams)
Grams/Niii3
Kg/llr
Kg/Mg
Collection Efficiency (Percent)
Ammonia Data
Total Sample Weight (Milligrams)
Grams/Mill3
Kg/llr
Kg/Mg
Collection Efficiency (Percent)
Fo niia 1 dchydc Da ta e
Total Sample Weight (Milligrams)
Grams/Mm3
Kg/llr
Kg/Mg
Collection Efficiency (Percent)
AT W.R. GRACE AND CO., MEMPHIS
Feed 1
08-20-79
Inlet
2.14637
1464.7
82.2
2.731
106.0
47.2
380
0.17710
15.563
0.3635
512
0.23865
20.974
0.4900
0.409
0.000191
0.01674
0.000391
Outlet
2.55390
1408.9
41.1
5.472
101.6
47.2
30.4
0.01188
1.0038
0.0235
93.5
293
0.11450
9.675
0.226
53.9
0.133
0.0000519
0.00439
0.000103
73.8
Feed 2
08-21-79
Inlet
2.20103
1464.7
87.2
3.416
108.1
47.4
590
0.26817
23.569
0.5480
86.7
570
0.25901
22.762
0.5295
57.3
0.622
0.000283 0
0.02481
0.000577 0
76.1
, TENNESSEE
Feed
3
Av<.«
T;IJ;C*
08-22-79
Outlet
2.15487
1197.1
39.4
5.291
100.9
47.4
94.0
0.04352
3.126
0.0727
292
0.13523
9.712
0.226
0.178
.0000824
0.00592
.000138
Inlet
2.20670
1501.2
83.3
2.509
106.6
45.9
534
0.24208
21.805
0.5235
82
636
0.28830
25.969
0.6235
49
0.644
0.000292
0.02626
0.000631
78
Outlet
2.51736
1427.0
36.1
5.377
98 . 9
•15.9
111
0.04400
3.767
0.0905
.7
390
0.15401
13.230
0.318
.0
o.loo
0.0000059
0.00503
0.000135
.5
Inlet
2.18400
1470. 9
84.4
2.885
10I..9
40.8
501
0.22927
20.317
0.4785
57-1
0.2o2o"
23.279
U.5485
0.55H
0.000250
(I. (12271
0.000535
(Hit let
2.40802
1344.4
38.9
5.380
100.5
10.8
78.5
0.03251
2.023
O.Od IN
87.1
325
0.1341.5
10.859
0.250
53.3
0. 159
o. 11000059
0.00531
(1.000125
"0.0
a Normal cubic meters @ 20 C, 760 mn llg.
h Normal cubic meters per minute.
c p-dimctliylninino benzaldehyde colorimetric (with preliminary distillation) analysis method.
d Direct Nessler Analysis method.
e Chromotropic Acid Analysis method.
* Only sample weights from all three runs were averaged and then mass flow rates and efficiencies KCT'C calculau-d from these aveniiie sample i-.eii;hl-
-------
Run Number
Date
Location
Volume of Gas Sampled (DSCF, a)
Stack Gas Flowrate o(USCFM )
Stack Temperature ( F)
Percent Moisture
Percent Isokinetic
Production Rate (Tons/Hour)
Urea Data C
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (Percent)
Ammonia Data
Total Sample Weight (Milligrams)
Grains/USCr
Pounds/Hour
Pounds/Ton
Collection Efficiency (Percent)
Formaldehyde Data
Total Sample Weight (Milligrams)
Graiiis/llSCF
Pounds/Hour
Pounds/Ton
Collection Efficiency (Percent)
TABLE 2-Sa (English)
SI&MARY OF RESULTS OF IIREA, AMMONIA AND FORMALDEHYDE TESTS
ON GASES ENTERING AND EXITING Till: PRILL TOWER SCRUBBER C
Feed I
08-20-79
Inlet
64.53
44150
184
3.041
105.7
47.2
411
0.0983
37.20
0.788
Outlet
83.59
46270
104
5.833
101.5
47.2
37
0.00682
2.703
0.0573
92.7
540
0.1291
48.86
1.035
322
0.05932
23.52
0.498
51.9
0.419 0.131
0.0001002 0.0000241
0.03792 0.009570
0.000803 0.0002028
74.7
R'. GRACE AND
l:eed
CO., MEMPHIS,
2
08-21-79
Inlet
69.63
48880
179
2.863
104.8
47.4
425
0.0942
39.47
0.833
84.
480
0.1064
44.58
0.941
53.
0.563
0.0001248
0.05229
0.001103
75.
Outlet
83.39
45160
103
6.388
103.8
47.4
87
0.01610
6.232
0.132
2
288
0.05330
20.63
0.435
8
0.182
0.0000337
0.013045
0.0002752
0
TENNESSEE
Feed 3
08-22-79
Inlet
68.85
46920
174
2.493
105.3
45.9
463
0.1038
41.75
0.910
82.6
483
0.1083
43.56
(1.949
31.8
Outlet
91.57
50470
99
6.160
102.0
45.9
100
0.01682
7.274
0.1585
408
0.068(i 2
29.68
0.647
0.440 0.168
0.0000986 0.11000283
0.03965 0.012221
O.OOOSd-l 0.0002662
69.2
Average*
67.67
46650
179
2.791'
105.3
4(>.8
433
0.0987
39.47
11.843
Hd.2
Sill
0.1 143
45.7(1
0.976
0.474
0.0001081
0.04322
0.000924
Out let
HI). IK
47300
(..127
102.4
46.8
0.0134
5.433
O.I 161
339
11.1160?
24.61
0.526
Dry standard cuhic feet @ 68 r, 29.92 inches Hg.
Dry standard cubic feet per minute.
a
1)
c p-dimethylamino benzaldehyde colorimetric (with preliminary distillation) analysis method.
d Direct Nessler Analysis method.
e Chromotropic Acid Analysis method.
* Only sample weights from all three runs were averaged, and then mass flow rates and efficiencies were calculated frun tin-si- avvnn;r
-------
TABLE 2-5h (Metric)
Run Number
Date
Locution
Volume of Gas Sampled (Nm3 a).
Stuck Gas Flowratc (Nm3/min )
Stack Temperature (°C)
Percent Moisture
Percent Isokinetic
Production Rate (Mg/llour)
Urea Data C
Total Sample Weight (Milligram)
Grams/Nm3
Kg/I I r
Kg/Mg
Collection Efficiency (Percent)
Auiiionia Data
Total Sample Weight (Milligram)
Grums/Nm3
Kg/Mr
Kg/Mg
Collection Efficiency (Percent)
Formaldehyde Data e
Total Sample Weight (Milligram)
Grams/Mm3
Kg/11 r
Kg/Mg
Collection Efficiency (Percent)
Feed 1
08-20-79
Inlet Outlet
1.827
1250.3
84.4
3.041
105.7
42.820
411
0.22492
16.874
0.394
92.7
2.367
1310.4
40
5.833
1.01.5
42.820
37
0.01560
1.226
0.0287
540
0.29539
22.163
0.518
51.9
322
0.13573
10.669
0.249
0.419
0.000229
0.017201
0.0004015
0.131
0.0000551
0.004341
0.0001OM
74.7
\NMONIA AND FORMALDEHYDE Tl
POWER SCRUBBER C ON AUGUST
CO., MEM11IIS, TENNESSEE
Feed 2
08-21-79
Inlet Outlet
1.972 2.362
1384.3 1278.9
81.7 39.4
2.863 6.388
104.8 103.8
43.001 43.001
425 87
0.21554 0.03684
17.904 2.827
0.417 0.0660
84.2
480 288
0.24345 0.12196
20.221 9.358
0.471 0.218
53.8
0.563 0.182
0.000286 0.0000771
0.023719 0.005917
0.0005515 0.0001376
75.0
•STS ON GASES
20-22, 1979 AT
Feed 3
08-22-79
Inlet
1.95(1
1328.8
78.9
2.493
105.3
41.640
463
0.23750
18.938
0.455
82.6
483
0.24780
19.759
0.475
31.8
0.440
0.000226 0
0.017985 (I
(1.0004320 0
69.2
Outlet
2.593
1429.3
37.2
6. 160
102.0
41.640
100
0.03849
3.299
0.0793
408
0.1570]
13.463
0.324
0.168
.0000648
.0055-13
.0001331
Average*
Inlet
1321. 1
81.7
2.799
105.3
42.457
Out let
2. 141
1339.5
3S.9
d.127
102.4
42.457
433 75
0.22584 O.(l30(i(i
17.901 2.164
0.422 0.0581
8d.2
501
0.2hi 53
20.730
0.488
339
(I. 13889
I I.1d3
0.2d3
0.4"4 O.ldO
(1.000247 0.0000(i5~
O.ol9d05 0.005278
0.0004li2 0.0001215
"3. I
u Nonnal cubic meters fl 20 C, 760 mm llg.
b Normal cubic meters per minute.
c p-dimethylumino benzaldehyde colorimetric (with preliminary distillation) analysis method.
d Direct Ncssler Analysis method.
e Chromotropic Acid Analysis method.
* Only sample weights from all three runs were averaged, and then muss flow rates and efficiencies were calculated from these avoru.r.e sample weights
-------
TABU- 2-6
SI&MARY OF RESULTS OF UREA, AIWONIA AND FOHMAI.DF.I1YDH TESTS
ON GASES ENTHIUNC. TTIK PR! 1.1. TOWER SCRUBBER A
ON AUGUST 15-17, 1979
AT W.R. CRACE AND CO., MEMPHIS, TENNESSEE
Run Number
Date
Volume of Gas Sampled (DSCF a)
Stack C.as Plowrate £USCFM h)
Stack Temperature ( F)
Percent Moisture
Percent Isokinetic
Production Rate (Tons/Hour)
Urea Data C
Total Sample Weight (Milligrams)
Crnins/nSCF
Pounds/Hour
Pounds/Ton
Ammonia Data
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Formaldehyde Data
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Insoluble Participate Data
Total Sample Weight (Milligrams)
Pounds/Hour
Fertilizer 1
08-15-79
99.14
65680
113
2.382
108.0
43., 5
449
0.0699
39.35
0.905
Fertilizer 2
08-16-79
104.1
68880
112
1.881
106.4
45.8
622
0.0922
54.43
1.188
Fertilizer 3
08-17-79
95.94
70130
116
1.844
97.8
45.5
502
0.0807
48.51
1 . 066
ON
182
0.0283
15.93
0.366
S1E
174
0.0271
15.26
0.351
1.31
0.000204
0.1148
0.002639
253
0.0375
22.14
0.483
sin
217
0.0322
19.01
0.415
DN
S1H
236 215
0.0380 0.0346
22.84 20.80
0.502 0.457
Average
99.71
68230
114
2.036
104.1
44.9
.524
0.0811
47.43
1.056
DN
224
0.0347
20.2'.)
11.452
sn:
2(12
0.0313
18.31
0.4HX
1.92
0.000285
0.1683
0.003675
0
0
1.75
0.000281
0.1689
0.003712
0
0
1 .<>
-------
TABU- 2-7
SUMMARY OF RKSUI.TS Ol: UREA, AMMONIA AND FORMALDEHYDE TESTS
ON fiASRS EX IT IN(; 1111: PRIM, TOWER SCRUBBER A
ON AUfllST 15-17, 1979
AT W.R. GRACE AND CO., MEMPHIS, TENNESSEE
l
M
CO
Rim Number
Date
Volume of Gas Sampled (DSCF a)
Stack Gas Flowrate (DSC1M b)
Stack Temperature ( F)
Percent Moisture
Percent Isokinetic
Production Rate (Tons/Hour)
Urea Data
Total Sample Weight (Milligrams)
Grai'ns/DSCF
Pounds/Hour
Pounds/Ton
Aiiniionia Data
Total Sample Weight (Milligrams)
Giviins/DSCF
Pounds/Hour
Pounds/Ton
Formaldehyde Data
f
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Insoluble ('articulate Data
Total Sample Weight (Milligrams)
Pounds/Hour
Fertilizer 1
(18-15-79
109.2
62180
90
3.655
98.4
43.5
33.0
0.00465
2.478
0.0570
nNd SIF. e
745 748
0.1051 0.1055
56.01 56.24
1.287 1.292
0.0578
0.0000082
0.00437
0.000101
0
0
Fertilizer 2
08-16-79
106.4
60510
90
3.556
98.5
45.8
85.4
0.01236
6.410
0.1399
DN SIF.
821 746
0.1188 0.1079
61.61 55.98
1.345 1.222
0.0706
0.0000102
0.00529
0.000116
0
0
Fertilizer 3
08-17-79
105.9
60530
89
3.677
98.1
45.5
59.7
0.00868
4 . 503
0.0990
DN SIF.
683 634
0.0993 0.0922
51.51 47.81
1.132 1.051
0.0761
0.0000111
0.0057(i
0.000127
0
0
Average
107.2
61073
90
3.633
98 . 3
44.9
59. -1
0.110853
4. -Id 5
0.099-1
DN S 1 1-;
750 7(19
0.1077 0.1018
56.37 53.29
1.255 1.18(.
0.0682
O.OOOII09S
0.00513
(1. 0001 1-1
(I
I)
a Dry standard cubic feet e 68 F, 29.92 inches llg.
I) Dry standard cubic feet per minute.
c p-dimethylamino benzaldehyde colorimetric (with preliminary distillation) analysis method.
d Direct Nessler Analysis method.
c Specific Ion Electrode Analysis method.
f Chromotropic Acid Analysis method.
-------
TABU; 2-8
SUMMARY Ol: RESULTS OF 1IRI-A. ANMONIA AND FORMALDEHYDE TESTS
(IN r,ASRS ENTERING THE PRILL TOWER SCRUBBER C
ON AUGUST 15-1.7, 1979
AT W.R. GRACE AND m., MF.MPIIIS, T-NNI-SSEE
Run Number
Date
Volume of Gas Sampled (I)SCF a)
Stack Gas Flowrate (USCI-M b)
Stack Temperature (°F)
Percent Moisture
Percent Isokinetic
Production Rate (Tons/Hour)
Urea Pata c
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Ammonia Data
Total Sample Weight (Milligrams)
Grains/DSC!-'
Pounds/Hour
1'ouiuls/Toii
Formaldehyde Data
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Insoluble Participate Data
Total Sample Weight (Milligrams)
Pounds/Hour
Fertilizer 1
08-15-79
101.1
62360
113
2.029
120.1
43.5
304
0.0464
24.80
0.570
DN
135
0.0206
11.01
0.253
SIP. c
132
0.0201
10.74
0.247
0.849
0.0001296
0.06927
0.001592
Fertilizer 2
08-16-79
82.54
53660
111
1.395
121.3
45.8
217
0.0406
18.67
0.408
DN
127
0.0237
10.90
0.238
S1E
113
0.0211
9.70
0.212
0.582
0.0001088
0.05004
0.001093
Fertilizer 3
08-17-79
87.38
59050
116
1.371
114.3
45.5
275
0.0486
24.60
0.541
DN
173
0.0306
15.49
0.340
Slli
155
0.0274
13.87
0.305
0,790
0.0001396
0.07066
0.001553
Average
911.34
58357
113
1.598
118.(i
44.9
2<>5
0,0453
22.66
0.505
DN
145
0.0248
12.41
0.276
SJE
I 33
0.0227
11.35
11.253
0.740
0.01101264
0.06323
I). 01) 14 08
a Dry standard cubic feet d 68 F, 29.92 inches llg.
b Dry standard cubic feet per minute.
c p-diniethylamino benzaldeliydc colorimetric (with preliminary distillation) analysis method.
d Direct Nessler analysis method.
e Specific Ion Electrode Analysis method.
f Chromotropic Acid Analysis method.
-------
TABU- 2-9
SUMMARY OP RESULTS 01- UREA, ANM1NIA AND FORMALDEHYDE TESTS
ON CASKS EXITING HIE PRILL TOWER SCRUBBER C
ON AUGUST 15-17, 1979
AT W.R. GRACE AND CO., MEMPHIS, TENNESSEE
o
I
Run Ninnhcr
Hate
Volinne of Gas Sampled (DSCF.;I)
Stack Gas Flowrate (IXSCFM b)
Stack Temperature ( I')
Percent Moisture
Percent Isokinetic
Production Rate (Tons/Hour)
Urea Data c
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Airanon i a Da ta
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
l-'oniinldchyde Data
Total Sample Weight (Milligrams)
Gr;iins/USi:i:
Pounds/Hour
Pounds/'l'on
Insoluble ['articulate Data
Total Sample Weight (Milligrams)
Pounds/I lour
Fertilizer 1
08-15-79
99.84
56220
86
3.314
99.8
43.5
37
0.00571
2.750
0.0632
DN
167
0.0258
12.41
0.285
175
0.0270
13.00
0.299
0.041
0.0000063
0.003047
0.000070
Fertilizer 2
08-16-79
98.08
56450
80
3.371
97.6
45.8
67
0.01052
5.089
0.1111
DN
255
0.0400
19.37
0.423
SIE
230
0.0361
17.47
0.382
0.068
0.0000107
0.005165
0.000113
Fertilizer 3
08-17-79
109.4
62410
82
4.012
98.5
45.5
70
0.00985
5.270
0.1158
245
0.0345
18.45
0.405
SI I-
232
9.0327
17.47
0.384
0.063
0.0000088
0.004706
0.000103
Average
KS2..I
58360
83
3.51.6
98. (,
44.9
58
0.00872
4.363
0.0972
UN
222
0.0334
16.70
0.372
sn;
2\2
1.0319
I 5. !>5
0.355
0.115?
0.000008(1
0.004287
0.00009(>
a Dry standard cubic feet 0 68 F, 29.92 inches llg.
I.) Dry standard cubic feet per minute.
c p-dimethylamino hcnzaldehyde colorimetric (with preliminary distillation") analysis method.
d Direct Ncssler analysis method.
e Specific Ion Electrode analysis method.
I" Chromotropic Acid analysis method.
-------
TABU-: 2-in
9IMWKY 0|; KI-Slll.TS OF HUM, AMONIA AND FORMA I. 11F.I IY Ill: TF.STS
ON. CASKS ENTERING TKF. PRTI.L TONHR SCRIIHHI-R A
~~ON AllfJ 1ST 20-22, 1079
AT W.R. CRACF. AND CO., MCMPIIIS, TI-NNF.SSF.F.
Run Number
Date
Volume of Gas Sampled (DSCF a)
Stack Gas Flowrate (IXSCFM I')
Stack Temperature ( F)
Percent Moisture
Percent Isokinetic
Production Rate (Tons/Hour)
Urea Data c
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Ammonia Data
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Feed 1
08-20-79
75.79
51720
180
2.731
106.0
47.2
380
0.0774
34.31
0.727
DN u
512
0.1043
46.24
0.98(1
Formaldehyde Data
f
467
0.0951
42.16
0.893
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Insoluble I'articulate Data
Total Sample Weight (Milligrams)
Pounds/Hour
0.409
0.0000833
0,0369
0.000782
0..04
Feed 2
08-21-79
77.72
51720
189
3.416
108.1
47.4
590
0.1172
51.96
1.096
DN
570
0.1132
50.18
1.059
SI I-
550
0.1092
48.41
1.021
Feed 3
08-22-79
77.92
53010
182
2.509
106.6
45.9
534
0.1058
48.07
1.047
DN
636
0.1260
57.25
1.247
SM!
609
0.1206
54.80
1.194
0.622
0.0001235
0.0547
0.001154
0.644
0.0001275
0.0579
0.001261
Avc'ragr
77. 14
52150
184
2.8«5
IOd.9
501
0.1002
44.79
0.957
DN
574
0.1148
51.32
1.097
SJJ:
542
11.1084
48.45
I .035
0.558
0.0001\2
0.05006
0.001070
a Dry standard cubic feet 0 68 F, 29.92 inches llg.
b Dry standard cubic feet per minute.
c p-dimethylamino benzaldehydc colorimetric (with prcliminary distillation) analysis method.
d Direct Nessler Analysis method.
e Specific Ion lilectrode Analysis method.
f Chromotropic Acid Analysis method.
-------
TABU: 2-11
SUNNARY Ol; RESULTS OH IIKKA, AMMONIA AND FORMAI.DIUIYDI- THSTS
-------
TAIU.H 2-12
SlflNARY OF RHSUITS OF IIRF.A, AMMONIA ANI) FORMAI.DFJIYnn TF.STS
ON GASHS ENTF.R1NG 'Mil; PRILL TOWI-R SCRIIBBHR C
ON Aim 1ST 20-22, 1979
AT W.R. GRACE AND CO., MBII1IIS, TF.NN1-SSHF:
I
l-o
UJ
Run Number
Date
Volume of Gas Sampled (DSCF a)
Stack Gas Flowrate (DSCfM h)
Stack Temperature
Percent Moisture
Percent Isokinetic
Production Rate (Tons/Hour)
Urea Data c
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Amiiionja Data
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Feed 1
08-20-79
64.53
44150
184
3.041
105.7
47.2
411
0.0983
37.20
0.788
DN
540
0.1291
48.86
1.035
Formaldehyde Data
f
Total Sample Weight (Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Insoluble Participate Data
Total Sample Weight (Milligrams)
Pounds/Hour
513
0.1227
46.43
0.984
0.419
0.0001002
0.03792
0.000803
1.30
<0.001
Feed
08-21-79
69.63
48880
179
2.863
104.8
47.4
425
0.0942
39.47
0.833
UN
480
0.1064
44.58
0.941
447
0.0991
41.52
0.876
0.563
0.0001248
0.05229
0.001103
Feed 3
08-22-79
68.85
46920
174
2.493
105.3
45.9
463
0.1038
41.75
0.910
DN
483
0.1085
43.56
0.949
S1F.
476
0.1067
42.91
0.935
0.44(1
0.0000986
0.03965
0.000864
Average
67.67
46650
179
2 799
105.3
46.8
433
0.0987
39.47
0.843
DN
501
0.1143
45.70
0.976
sii;
•179
0.1(192
43.66
0.933
0.474
(1.11001(181
11.11.1322
0.000924
a Dry standard cubic Feet e 68 F, 29.92 inches llg.
b Dry standard cubic feet per minute.
c p-dimethylamino bcnzaldehydc colorimetric (with preliminary distillation) analysis method.
d Direct Ncsslcr analysis method.
e Speci Tic Ion lilectrode Analysis method.
f Chroiuotropic Acid Analysis method.
-------
TABU: 2-13
SUMMARY OP RHSUI.TS OF IIRKA, AMMONIA AMI) FORMALDEHYDE TESTS
ON GASES UXfTING THE I'RII.L TOWER SCRUBBIER C
ON AUGUST 20-22, 1979
AT W.R. GRACE AND CO., MEMI11IS, TENNESSEE
I
t-O
Run Number
Date
Volume of Gas Sampled (I1SCF a)
Stack Gas Flowrate DSCBI h)
Stack Temperature (°F)
Percent: Moisture
Percent Isokineti.c
Product ion Rate (Tons/Hour)
Urea Data c
Total Sample Weight (Milligrams)
Grains/DSCF
I'ounds/llour
Pounds/Ton
Ammonia Data
Total Sample Weight (Milligrams)
Grains/DSCE
Pounds/Hour
Pounds/Ton
Formaldehyde Data
Total Sample Weight (Milligrams)
Grains/llSCr
Pounds/Hour
Pounds/Ton
Insoluble Participate Data
Total Sample Weight (Milligrams)
Pounds/Hour
Feed 1
08-20-79
83.59
46270
104
5.833
101.5
47.2
37
0.00682
2.703
(1.0573
DN
322
0.05932
23.52
0.498
SIE c
320
0.05895
23.37
0.495
0.131
0.0000241
0.009570
0.000203
Feed 2
08-21-79
83.39
, 45160
; 103
i 6.388
103.8
47.4
87
0.01610
6.232
0.1315
DN
288
0.05330
20.63
0.435
SIE
271
0.05015
19.41
0.409
0.182
0.0000337
0.013045
0.000275
Feed 3
08-22-79
91 ,57
50470
99
6.160
102.0
45.9
100
0.01682
7.274
0.1585
DN
408
0.06862
29.68
0.647
SIE
422
0.07097
30.70
0.669
0.168
0.0000283
0.012221
0.000266
Average
86.18
47300
102
6.127
102.4
46.8
75
0.013-18
5.462
0.1167
DN
339
0.06092
24.69
0.528
SIE
338
0.06074
2-1.6J
0.526
0.1611
0.0000288
0.011653
0.0(10249
a Dry standard cubic feet 0 68 F, 29.92 inches llg.
b Dry standard cubic feet per minute.
c p-dimcthylamino bcnzaldehyde colorimetric (with preliminary distillation) analysis method.
d Direct Ncssler analysis method.
e Specific Ion Electrode analysis method.
f Chroinotropic Acid analysis method.
-------
shown in Tables 2-2 through 2-6. For scrubbers A and C during both fertilizer
and feed grade tests, the calculated I averaged 99.9 percent at the outlets
and 108.7 percent at the inlets. The inlet isokinetics are consistently
higher than the outlet isokinetics, with the scrubber C fertilizer data (Table
2-3) most conspicuous {averaging 118.6 percent). These latter test runs also
exhibited the largest average cyclonic flow angles.
The differences between the scrubber A inlet and outlet flow rates during
the fertilizer and feed test runs (Tables 2-2 and 2-4) may also be due to the
inlet cyclonic flow.
2.3 Synthesis Tower Main Vent Emissions Test Results
Table 2-14 shows the results of the urea and ammonia test runs conducted
at the urea synthesis tower main vent. These test runs were performed on
August 22, 1979, during feed grade urea production. The urea concentrations
were at the threshold of detection. The results of the two ammonia analysis
methods agreed with each other within 5% in terms of total sample weight.
However, because of the large absolute amounts of ammonia in the gas stream
(about 70% of the dry gas stream was ammonia), the differences between calcu-
lated amounts of ammonia yield appreciable differences in calculated stack gas
volumetric flowrates. Thus, two sets of data are presented: one for direct
Nessler analysis results and one for specific ion electrode analysis results.
Integrated gaseous bag samples were collected during each particulate test
run at the synthesis tower vent. These samples were collected directly from
the vent stack using an Integrated Orsat Sampler. The samples were then ana-
lyzed for CO0 and O using the EPA Reference Method 3 Orsat analyzer
£• £
procedure. Results of these sample analyses are as follows:
-25-
-------
Run Number
Ammonia Analysis Method:
Volume of Gas Sampled (I)SCI: C)
Stack Gas Plowrate fDSCFM '-1)
Stack Temperature ( P)
Percent Moisture
Percent Isokmetic
Production Rate (Tons/Hour)
Q
Urea Data
Total Sample Weight (Milligrams)
r.rains/nSCF
Pounds/Hour
Pounds/Ton
Ammonia Data
Total Sample Weight (.Milligrams)
Grains/DSCF
Pounds/Hour
Pounds/Ton
Insoluble Particulate Data
Total Sample Weight (Milligrams)
Pounds/Hour
• TABI.K 2-14
SUNflARY OF RESULTS OP UREA AND AMMONIA TESTS
ON GASES SAMPLED AT 'IIIP. SYNTHESIS TOWER MAIN VENT
Run
m*
5.07
786.4
180
73.1
124.4
47.9
1.
SIE h
4.84
761.1
180
74.0
122.7
47.9
<28.2 <28.2
<0.0858 <0.0899
<0.578 <0.586
<0.0121 <0.0122
69439 64773
211.3 206.5
1424.0 1347.1
29.73 28.12
ON AUGUST 22, 1979
R. GRACF. AND CO., MEMPHIS, TENNESSE
Run 2
DN
5.10
742.4
181
74.1
132.6
47.9
<24.4
<0.0738
<0.470
< 0.0098
72296
218.7
1391.8
29.06
0
0
sin
5.17
747.8
181
73.8
133.4
47.9
<24.4
<0.0728
<0.467
<().0097
73836
220.4
1412.6
29.49
0
0
Run
DN
5.01
740.4
181
73.9
130.7
49.9
<23.2
<0.0715
<0.454
<0.0091
71218
219.3
1391.7
27.89
0.12
-------
Run No. Percent C02 Percent 02
1 10.6 11.8
2 33.2 9.2
3 14.0 11.0
The Run 2 data is the average of three samples. All data were recorded on the
synthesis tower field data sheets shown in Appendix B.
2.4 Visible Emissions
The opacity of the individual plumes from the outlets of scrubbers A and
C, and the opacity of the combined plumes from all operating scrubbers, were
monitored during the two week test period. Observations were made from ground
level and from atop the prill tower by certified smoke observers.
During the period of fertilizer grade urea production (August 15-17, 1979)
scrubber C and combined scrubbers A through H were monitored. The six-minute
average opacities ranged from 10% to 40% for scrubber C and from 10% to 35%
for combined scrubbers A through H. These data are shown graphically in
Figures 2-1 and 2-2.
During the period of feed grade urea production (August 20-22, 1979)
scrubbers A and C and combined scrubbers A through D were monitored. The
six-minute average opacities ranged from 3% to 30% for scrubber A, from 6% to
33% for scrubber C, and from 6% to 19% for combined scrubbers A through D.
These data are shown graphically in Figure 2-3 and 2-4.
The opacity of the plume from the bagging operation baghouse was monitored
December 18, 1979. The highest six-minute opacity was 1%; overall the opacity
averaged zero percent. These data were not graphed and are presented in tabu-
lar form in Appendix C along with all visible emissions data.
A description of all visible emission observations locations is shown in
Table 2-15.
-27-
-------
NJ
00
I
o
DC.
CO
X
CO
o
u_
>-
O-
o
e>
2
UJ
-------
ui
o
UI
O-
1/7
X
I—I
to
OL
O
o
Q-
O
C3
40
35
30
25
20
15
10
Jl
c*>
O
ro
O
O
ro
i
in
CM
in
in
ro
t—i
i
o
ID
ro
cn
J
N
o
Lf>
O
cr\
o
i
o
CO
LT)
IT)
O
I
O
o
LT>
cr>
ir>
in
ur>
un
8-16-79
8-17-79
*OBSERVER LOCATIONS ARE CIRCLED
FIGURE 2-2: SIX MINUTE AVERAGE OPACITY READINGS FOR PRILL TOWER
COMBINED SCRUBBERS A-H DURING FERTILIZER TESTS
AT W. R. GRACE AND CO., MEMPHIS, TENNESSEE
0988-003
-------
OJ
o
I
to
ui
x
o:
o
o
Q-
O
1
30
25
20
15
10
0
O
o
LO
IT)
o
1
r
CNJOO
<—10
I I
en in
en en
oo
i i
cno
en r-.
o —i
.—< i—i
<3- CM
CM CO
i-lO
COCTl
oo
OJ
CNJ
ID
ro
en
O
i
O
ro
en
o
en
CM
o
CM
O
en
O
o
CM
8-20-79
-8-21-79
8-22-79
*OBSERVER LOCATIONS ARE CIRCLED
FIGURE 2-3: SIX MINUTE AVERAGE OPACITY READINGS FOR PRILL TOWER
SCRUBBER A DURING FEED TESTS
AT W. R. GRACE AND CO., MEMPHIS, TENNESSEE
0988-004
-------
Jb
P"
LU
Si 30
a.
UJ
i 25
i |
s:
X
K 20
QC
£
£
2 15
a.
0
UJ
CD
g 10
>
T-O
ro O
O r-l
i— 1 r— 1
1 1
^-t-
r-l CM C^ O
I—I
1
LO
CO
r^ C
i
CM f
3
>
>
•-H CM
-------
TABLE 2-15
VISIBLE EMISSION OBSERVATION LOCATIONS
AT W.R. GRACE AND CO., MEMPHIS, TENNESSEE
Observer
Location
A
B
C
D
E
F
G
H
I
J
Distance To
Discharge
Point (Feet)
450
40
450
450
450
40
400
500
400
5-15
Height
Above Ground
(Feet)
0
200
0
0
0
200
0
0
0
0
Direction From
Discharge
Point
SE
SSE
E
SE
SSW
E
SW
s
ESS
S
Discharge
Description
Prill Tower
1 1
I!
M
1 1
1 I
II
1 1
1 1
Bag House
-32-
-------
2.5 Particle Size Tests
Particle size distribution tests were performed on the inlet gas stream of
both scrubbers A and C during each of the emission test runs. The tests were
performed with an Anderson cascade impactor with pre-impactor at a single
average flow point in each duct.
The results for the fertilizer tests are summarized in Table 2-16 and are
shown as cumulative size distribution curves in Figures 2-5 (scrubber A) and
2-6 (scrubber C) . The feed test results are shown in Taole 2-17 and Figures
2-7 and 2-8. All particle size field and laboratory data are contained in
Appendix D.
2.6 Volumetric Flowrates in the Prill Tower Scrubber Inlets
Velocity traverses were performed at scrubber inlets B, D, E, F, G and H
immediately before and immediately after each fertilizer emissions test run;
similar velocity traverses were made at scrubber inlets B and D before and
after each feed test run. The calculated flowrates resulting from these velo-
city traverses and from the scrubbers A and C emission tests are shown in
Table 2-18.
Cyclonic flow caused by the axial flow fans in each duct was evident to
some degtee in all eight scrubber inlets. The cyclonic flow angles were
measured at each traverse point in inlets B, D, E, F, G and H before the velo-
city traverses and in inlets A and C before the emission tests. The average
-33-
-------
TABU: 2-16
SUHMARY OF lNI,fiT PARTICLE SIZING TfiST RESULTS
ON SCRUBBERS A § C
DURING FERTILIZER GRADE URFA PRODUCTION
AT W.R. GRACE AND CO., MEMPHIS, TENNESSEE
Test Number
Sampling
Location
Test
Date
Test
Time
('articulate
Concentration
GR/DSCF
Aerodynamic
Size Range
pin
Mass In
Size Range
Percent
Cumulative
Percent
A Inlet
08-14-79
1252
0.040
>13.3
9.17-13.3
6.22-9.17
4.24-6.22
2.72-4.24
1.36-2.72
0.84-1., 36
0.57-0.84
<0.57
48.5
3.4
3.2
2.3
13,8
4.0
7.3
6.6
10,9
51 .5
48.1
<14.9
42.6
28.8
24.8
17.5
1(1.0
A Inlet
08-15-79
0955
0.034
>I4.5
10.0-14..5
6.8-10,0
4.63-6.8
2.97-4.63
1.5-2.97
0.93-1.5
0.63-0.93
<0.63
24.9
9 2
1 8
12.8
6.4
10.7
0
20,9
13.3
75.1
65. 9
<)4 1
51.3
•14.9
34 .2
34 .2
13.3
A Inlet
08-15-79
1126
0.039
>I5.3
10.6-15.3
7.16-10,6
4.89-7,16
3.14-4,89
1.58-3,14
0.98-1,58
0.67-0,98
<0.67
17,2
3.0
11.5
7.9
17,1
3.0
21 .4
14.7
4.2
82 8
7!) 8
68 3
60.4
43.3
40 3
18,9
4.2
-------
TABU: 2-16 (Cent.)
SUMMARY OF INU-r PARTICLFi SIZING TI-ST RI-SUI.TS
ON SCRtlBBKRS A f, C
HIRING FERTILIZER GRADE UREA PRODUCTION
AT W.R. GRACF. AN11 CO., MEMPHIS, TENNESSEE
Test Number
Sumpling
Location
Test
Date
Test
Time
Particulnte
Concentration
Gr/IXSCF
Aerodynamic
Size Uanj;e
inn
Mass In
Size Ranyc
Percent
Gumihit ivi
I'eivcMit
C Inlet
08-16-79
1122
0.022
>12.3
8.5-12.3
5.76-8.5
3.92-5.76
2.52-3.92
1.26-2.52
0.78-1.26
0.53-0.78
<0.53
49.0
0.0
0.4
3.0
1.2
11.5
19.5
10.8
4.6
51 .0
51.0
50.(,
47. h
4(>.-l
3-1.9
15.4
I
to
t-n
I
C Inlet
08-16-79
1543
0.027
>12.2
8.4-12.2
5.69-8.4
3.88-5.69
2.49-3.88
1,25-2.49
0.77-1..25
0.52-0.77
<0.52
21.2
I)
1.4
2.5
3.1
22.8
22.2
21.2
5,6
78.8
78.S
77 4
74 .9
71.S
49.0
21..8
5.6
C Inlet
08-17-79
1430
0.013
>13.0
8.93-13.0
6.05-8.93
4.13-6.05
2..65-4.13
1.33-2.65
0.82-1.33
0.56-0,82
<0.5d
66.5
3.7
0.0
0..0
1.5
0.0
15,0
6. 0
7.3
33.5
J'.l.K
.".1.8
28.3
2K 3
1 3.3
, . .1
-------
10.0.
o
o
1.0
cr
0.1
LEGEND
TEST 1 FERTILIZER 8-14-79
TEST 2 FERTILIZER 8-15-79
TEST 3 FERTILIZER 8-15-79
10 15 20 30 40 50 60 70
PERCENT OF MASS < INDICATED SIZE
80 85 90
FIGURE 2-5: CUMULATIVE SIZE DISTRIBUTIONS OF PARTICULATE
IN SCRUBBER A DURING FERTILIZER TESTS AT
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
0988-006
-36-
-------
10.0.
3.
OS
Q
O
1.0
*-4
Or
0.1
LEGEND
- TEST 1 FERTILIZER 8-16-79
- TEST 2 FERTILIZER 8-16-79
- TEST 3 FERTILIZER 8-17-79
10 15 20 30 40 50 60 70
PERCENT OF MASS < INDICATED SIZE
80 85 90
FIGURE 2-6:
CUMULATIVE SIZE DISTRIBUTIONS OF PARTICULATE
IN SCRUBBER C DURING FERTILIZER TESTS AT
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
-37-
0988-007
-------
TABLE 2-17
SWMARY OF INLET PARTICLE SIZING TEST RESULTS
ON SCRUBBERS A f, C
DURING FEED CRAM; UUEA PRODUG'ION
AT W.R. GRACE AND CO., MEMPHIS, TENNESSEE
Test Number
Sampling
location
Test
Date
Test
Time
Paniculate
Concentration
Cr/I)SCF
Aerodynamic
Size Range
inn
Mass In
Size Range
Percent
C.iuiinlal ivc
Percent
A Inlet
08-21-79
1605
0.031
>15.9
10.9-15.9
7.4-10.9
5.05-7.4
3.24-5.05
1.63-3.24
1.00-1.63
0.69-1.00
<0.69
88.6
0.0
0.0
0.0
0.0
5.3
6.1
0..0
0.0
I
• OJ
00
I
A Fnlet
08-22-79
0935
0.054
>16.3
11.2-16.3
7.0-11.2
5.18-7.60
3.33-5.18
1.67-3.33
1.03-1.67
0.71-1.03
<0.71
8-1.4
0.1
0..0
7.9
0.0
1.9
0.0
0.0
5.7
15.5
15.5
7.6
7.6
5.7
5.7
5.7
A Inlet
08-22-79
1430
0.020
>14,7
10.1-14.7
6.87-10,1
4.68-6.87
3.0-4.68
KS-3.0
0.93-1,5
0.63-0.93
<0.,63
98 .1
0..0
0.0
0.0
0.0
0.0
0.0
0,0
1.9
-------
TABU: 2-17 (Cont.)
SIJNMARY OF 1NI.1-T PARTICLE SIZING TEST RnSlll.TS
ON SCRUBBERS A f, C
DURING FEED GRADE. IIREA PRODUCTION
AT W.R. GRACE AN1) CXI., MEMPHIS, TENNESSEE
Test Niunlier
Sam)) ling
Location
Test
Date
Test
Time
Particulate
Concentration
Gr/DSCF
Aerodynamic
Si ze Range
inn
Mass In
Size Range
Percent
Ci initiative
Percent
C Inlet
08-20-79
1555
0.048
10.4-15.1
7.04-10.4
4.8-7.04
3.08-4.8
1.54-3.08
0.95-1.54
0.65-0.95
<0.65
71.8
0
6.0
3.5
4.')
3.4
5,0
0
5.4
28.2
28.2
"*2 ^
18.7
13.8
1(1.4.
5.4
5.4
C Inlet
08-21-79
1018
0.084
>13.40
9.22-13.4
6.25-9.22
4.26-6.25
2.73-4.26
1.36-2.73
0.84-1.36
0.57-0.84
<0..57
36.0
5..4
11.9
8.7
5.7
7.2
7.6
7,0
10.5
64.0
58. (.
46 7
38 .11
32.3
25.1
17.5
10.5
C Inlet
08-22-79
0935
0.052
11.5-16.7
7.81-11.5
5.32-7.81
3.42-5.32
1.72-3.42
1.07 1.72
0.73 1.07
<0.73
78.3
0.0
0.7
9.4
0.0
6.8
0.0
0..0
4 .8
21.7
21.7
21.0
11.6
4.8
•1.8
4.8
-------
10.0.
o
o
o
o
Q£
UJ
0.1
LEGEND-
- TEST 1 FEED 8-21-79
- TEST 2 FEED 8-22-79
- TEST 3 FEED 8-22-79
10 15 20 30 40 50 60 70
PERCENT OF MASS < INDICATED SIZE
80 85 90
FIGURE 2-7: CUMULATIVE SIZE DISTRIBUTIONS OF PARTICULATE
IN SCRUBBER A DURING FEED TESTS AT
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
-40-
0988-008
-------
10.0.
o
CJ
o
g
1.0
0.1
LEGEND
TEST 1 FEED 8-20-79
TEST 2 FEED 8-21-79
TEST 3 FEED 8-22-79
10 15 20 30 40 50 60 70
PERCENT OF MASS < INDICATED SIZE
80 85 90
FIGURE 2-8: CUMULATIVE SIZE DISTRIBUTIONS OF PARTICULATE
IN SCRUBBER C DURING FEED TESTS AT
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
0988-009
-41-
-------
TABU- 2-18
SCRUBRUR INUTF FLOWRATES* AT W.R. CRACK AND (X)., MEMPHIS, TENNESSEE
FERTILIZER
PEEP.
Scrubber Time
A During
R Before.3
After D
Average
C During
D Before
After
Average
1
•P- E Before
? After
Average
l: Be fore
After
Average
(! Before
After
Average
II Before
After
Average
I
65680
59150
54980
57065
62360
57970
57250
575TO"
65330
60010
52570
60950
59480
50115
72230
68450
70310
56410
56210
563TO
2
68880
50320
56890
53605
53660
48350
54370
5B50"
59000
60900
59950
61890
61030
5TT50
69990
70180
70085
58540
60140
59310
3
70130
44760
50720
47740
59050
51 330
51780
5T555
60900
58610
59755
62130
57810
59971)
69230
64820
57025
58540
55330
56935
Average
68230
51410
54197
5280T
58357
52550
54467
5T5TW
61743
59840
5079!
61657
59440
60548
70483
67817
59T5IT
57830
57227
57518"
1 2 3
51720 51720 53010
34600 34910 39190
34200 36890 39760
34400 35900 39475
44150 48880 46920
49140 46060 4574(1
45690 44870 463(10
474T5" T5155 35o!o~
Average
52150
36233
369 fid
36592
46650
46980
45620
3(7TmT
Total
492000
478000
472000
481000
17BIIOO
182000
185000
18JOIKI
a Flowrates calculated from velocity traverses perfomied before the indicated nins at scnihbcrs A and ('..
b l:lowratcs calculated from velocity traverses performed after the indicated runs at scrubbers A and ('..
c Sinn of averages, rounded to the nearest 1000 DSCI-II.
* Dry standard cubic feet per minute @ 68°F, 29.92 inches llg.
-------
flow angles measured at each inlet (averaged over all traverse points) are as
follows:
Average Flow Angle (degrees)
Fertilizer Runs Feed Runs
Scrubber ill ill
A 11.9 11.0 11.0 13.0 11.9 12.0
B 11.0 2.9 1.5 4.0 LI.3 2.0
C 15.0 24.4 22.5 14.0 13.5 9.0
D 7.4 2.9 4.3 10.4 6.0 9.0
E 12.2 15.7 18.4
F 21.0 2.5 2.4
G 16.0 14.9 12.3
H 13.8 11.3 11.2
The flowrates shown in Table 2-18 were calculated with the cyclonic flow
angles taken into account, as described in Section 5.1 and Appendix G.
During each emission test run, single point velocity head ( Ap) and tem-
perature (T) measurements were taken approximately every 15 minutes in inlets
B, D, E, F, G and H (fertilizer tests) and in inlets B and D (feed tests) .
This was done in order to have some measure of the consistency of flow in
these inlets during the emission tests. Averages of these data, along with
average Ap and T values from the complete before and after velocity traverses,
are shown in Table 2-19. These single-point measurements were made with ac-
count given to cyclonic flow angles.
All velocity traverse and single-point data are shown in Appendix F.
-43-
-------
TABLfi 2-19
S1JWIARY OP VKIjOCITY Iff-AD (INdlliS WAT1-R) AN1) TttirroATURF. (°F)
MFASURTMUNTS ON SCRUBBHR INLETS NOT Tl-STH) J:OR FMTSSIONS
AT W.R. GRACE AND CO., MIM11IIS, Tl-NNESSni:
Tliis table is claimed confidential by W.R. Grace and Co.
See Confidential Addendum: Contact F.ric Noble, EPA,
(919) 541-5213
-------
2.7 Pressure Drops Across the Prill Tower Scrubbers
This section is claimed confidential by W. R. Grace and Co. See confi-
dential addendum: contact Eric Noble, EPA, (919) 541-5213.
2.8 Analysis of the Scrubbing Liquor
The scrubbing liquor entering and exiting the A and C scrubbers was
sampled approximately every 30 minutes during each emission test run. Half-
liter samples were taken from the common liquor-stream inlet and from the two
separate liquor-stream outlets. The liquor temperature was measured immedi-
ately after the sample was collected, and when the sample reached room temper-
ature the pH was measured and recorded. After each emission test run, the
liquor samples taken during that run were combined into three composite
samples (one inlet and two outlet samples). These composite samples were then
analyzed for urea, ammonia, formaldehyde and undissolved solids. A summary of
these data is shown in Tables 2-20 (fertilizer test runs) and 2-21 (feed test
runs). The temperature and pH data for each individual scrubber liquor sample
are shown in Appendix E.
2.9 Ambient Air Temperature and Relative Humidity Measurements
The temperature and relative humidity of the ambient air were measured
periodically at the base of the prill tower during each emission test run.
These data are presented in Table 2-22 (fertilizer test runs) and 2-23 (feed
test runs).
-45-
-------
TABI.R 2-20
SUMMARY OP SCRUHBERS A AND C LIQUOR ANALYSIS RI-SUI.TS
FERTILIZGR GRAPH URKA PROHUCTION
W.R. GRACP. AN!) CO., MIWHIIS, TI-NNESSEF.
lliis table is claimed confidential by W.R. Grace and Co.
See Confidential Addendum: Contact Hric Noble, EPA,
(919) 541-5213
-------
TABLE 2-21
SUWARY OF SCRURBI-RS A AND C LIQUOR ANALYSIS RESULTS
FEED GRADE UREA PRODUCTION
W.R. GMCE AND CO., MMMllirS, TPJJ
Tliis table is claimcKl confidential by W.R. Grace and Co.
See Confidential Addendum: Contact Eric Noble, EPA
(919) 541-5213
I
-C-
-------
TABLE 2-22
.AMBIENT AIR TEMPERATURE AND RELATIVE HUMIDITY
MEASUREMENTS DURING FERTILIZER GRADE UREA PRODUCTION
AT W.R. GRACE AND CO., MEMPHIS, TENNESSEE
Relative
Run Number Date Time Wet Bulb ( F) Dry Bulb (°F) Humidity (%)
1 08-15-79 1000 71 77 74
1134 72 80 68
1529 72 82 61
1620 73 82 65
1657 73 81 68.5
1749 70 76 74
1843 68 74 74
Average 71 79 69
2 08-16-79 1125 63 75 51
1250 64 76 51
1330 63 78 43
1400 65 82 39
1500 64 82 36
1600 65 80 44
Average 64 79 46
3 08-17-79 1141 66 78 53
1200 66 79 50
1236 65 80 44
1307 66 80 41
1337 65 82 39
1407 63 82 33
1440 65 83 36.5
1500 67 83 42.5
Average 65 81 43
-48-
-------
TABLE 2-25
AMBIENT AIR TEMPERATURE AND RELATIVE HUMIDITY
MEASUREMENTS DURING FEED GRADE UREA PRODUCTION
AT W.R. GRACE AND CO., MEMPHIS, TENNESSEE
Run Number Date Time Wet Bulb (°F) Dry Bulb (°F)
Relative
Humidity (°»)
08-20-79
1103
1236
1305
1337
1404
1435
1505
1535
1605
Average
76
78
78
78
79
78
78
76
76
84
84
88
88
89
87
89
89
86
69
76
64
64
64.5
66.5
61
54.5
63
65
08-21-79
0945
1020
1105
1135
1205
1235
1305
1335
1405
1435
Average
76
76
76
77
76
76
77
77
77
78
77
84
84
85
86
85
86
87
89
89
89
86
69
69
66
66
66
63
63.5
57.5
57.5
61
64
08-22-79
0853
0940
1005
1050
1115
1206
1234
1304
1334
1428
1505
1523
Average
71
71
72
72
73
72
73
74
74
73
74
73
78
78
78
80
81
82
82
82
85
85
84
83
82
75
71
71
68
64.5
65
61
65
59.5
59.5
59
65.5
66
-49-
-------
2.10 Process Product Sampling
Samples of the prill tower unscreened product were taken by TRC personnel
during each emission test run. Bulk density and sieve analyses were then
performed on these samples in the W. R. Grace and Co. laboratory. The results
of these analyses are shown in Table 2-24.
Chemical analyses of samples of the urea melt and solid product were per-
formed by W. R. Grace and Co. personnel at the plant laboratory. These analy-
sis results are considered confidential by W. R. Grace and Co. and are not
presented in this report.
-50-
-------
TABI,F. 2-24
SIMMARY OF BULK DENSITY AND SIF.VF. ANALYSIS
ON 1111- IINSCRI-I-NKD IWIMKT SAMI'l.liS
AT W.R. GRA(T, AND 00., MJM1IIS, TliNNl-SSIil-
Percent Total Mass
Fertilizer
Date :
Time :
Run Number :
Sieve No.
8
10
12
14
16
20
30
50
Pan
Bulk Density (R/CC)
08-15-79
1820
1
24.6
-
59.0
13.7
1.6
0.6
0.2
0.2
0.1
0.730
08-16-79
1619
2
8.5
-
77.5
11.9
1.2
-
0.65
0.05
0.75
0.750
08-16-79
1720
2
7,0
-
74.6
14.8
1.7
1.0
0.5
0.2
0.1 .
0.750
08-17-79
1510
3
12.4
41.0
35.3
10.1
0.7
0.2
0.0
0.0
0.1
Average
0.754 0.746
08-20-79
1615
J_
0.7
0.32
1.75
6.47
15.45
43.04
25.90
6.33
0.025
0.760
Feed
08-21-79
1345
2
0.35
0.15
0.97
4.34
12.23
41.83
31.27
8.62
0.22
0.780
08-22-79
1250
3
1.97
0.47
1.32
5.49
14.32
42.23
27.85
6.14
0.20
Average
0.770 0.770
Bulk Density (lbs/ftj)
45.6
46.7
46.7
46.7
46.4
47.22
48.19
47.75
-------
3.0 PROCESS DESCRIPTION
Emissions measurements were made at the W. R. Grace and Co. Agricultural
Chemicals Group Facility in Memphis, Tennessee, . in order to obtain data neces-
sary to develop a new source performance standard for the urea industry. This
plant is considered to employ process and emission control technology repre-
sentative of modern urea solution formation and fluidized bed prilling proces-
ses.
Figure 3-1 presents a flow diagram of the solution formation and prill
tower operations and indicates the location of process sampling locations
(S1-S5) and emission test points (T1-T5). Emissions tests were designed to
characterize and quantify uncontrolled emissions from the solids production
and cooling (prill tower) processes, and to determine emission control equip-
ment efficiencies. During the emissions tests, conducted August 13-22, 1979,
process parameters pertinent to the operation of the various process streams
were monitored in order to determine if the process was operating at represen-
tative steady-state conditions. Detailed information on this process monitor-
ing is contained in Appendix L.
3.1 Process Equipment
There is one urea production line at this facility. Urea is produced by
reacting ammonia and carbon dioxide using the Snamprogetti total recycle pro-
cess built by C and I Gridler. The plant first started operation in October
1975. The . . . Note 1 ... urea solution leaving the synthesis process pro-
ceeds to a two-stage vacuum evaporator where it is concentrated to 99+ percent
urea. A formaldehyde additive is injected . . . Note 2 ... to prevent cak-
ing of the product.
Note 1 - See Item 1, Confidential Addendum, contact Eric Noble, EPA, (919)541-5213.
Note 2 - See Item 1, Confidential Addendum, contact Eric Noble, EPA, (919)541-5213.
-52-
-------
io ATHOSPIIERE
SCRUBBER LIQUOR FRON
AmmiA RECOVER? SVSUN
Nil,
CO,
SOLUTION
PRODUCTION
SHAH PROGETTI
TOTAL RECYCLE
UREA
SURGE
TANK/?
DENOTES PRODUCT FLOW
OVERHEADS
lit STAGE
CONCENTRATOR
MODIFIED JOY
TURDULAIRE SCRUBDER
(8 EACH)
BULK
LOAOINO
I BAGHDUSE I
BAGGINO
SCREENS
CONVEYOR
FIGURE 3-1: PROCESS FLOW DIAGRAM, W. R. GRACE AND CO.,
MEMPHIS, TENNESSEE
098R-010
-------
The urea melt is pumped directly to the top of the prill tower. There are
. . . Note 3 ... fittings at the top of the tower for either feed or fertil-
izer grade spray plates depending upon the grade being produced . . . Note 4 .
. . the only difference between the two grades is the size of the prills (the
feed grade being smaller) and the amount of additive injected. The number of
plates in use is determined by the desired production rate and the ambient
weather conditions. The maximum design production rate for the prill tower is
. . . Note 5 ... for either feed or fertilizer grade.
This prill tower employs a fluidized bed cooler near the base of the
tower, eliminating the need for a separate piece of cooling equipment. The
product leaving the fluidized bed cooler proceeds to a set of sizing screens.
One set is used for fertilizer grade and another set is used for feed grade.
The off-size material is conveyed to a dissolving tank and combined with the
prill tower scrubber liquor blowdown. The contents of the dissolving tank are
recycled to the process.
The correctly sized product prills are conveyed to a bulk warehouse. The
conveyor transfer points are controlled by a wet scrubber. The product is
temporarily stored in large piles on the warehouse floor. Front end loaders
move the urea to another conveyor belt which transports the prills to ...
Note 6 ... screens to remove . . . Note 7 ... material. The urea can be
either bagged in corner fill bagging machines or bulk shipped via truck or
railcar. A baghouse controls the particulate emissions from the bagging oper-
ation. The baghouse was built by General Resource Corporation and controls
about 141.6 cubic meters (500 cf) of air per minute with approximately 99.9
Note 3 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 4 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 5 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 6 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 7 - See Item 1(. Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
-54-
-------
percent particulate removal. Emission rates from this operation are estimated
at 0.00091 kg (0.002 Ibs) per hour at a velocity of 25.3 meters (83 feet) per
second, while bagging 9432 kg {20800 Ibs) per hour. Material collected by the
baghouse is redissolved and sent back to the process.
3.2 Emission Control Equipment
There are no major emission points from the urea synthesis and concentra-
tion steps since these are total recycle operations. The overheads from the
two stages of concentration are totally condensed and returned to the synthe-
sis operation. The major constituent of emissions is clean steam which is
used to keep the pressure safety valves free. Other emissions to the atmos-
phere include air, used to stabilize the CO feed stock; and a small amount
of ammonia vented from various sources, including the urea surge tank, dilute
carbamate tank, carbamate condenser, and aqua solution cooler.
On the roof of the prill tower, eight modified Joy Turbulaire Type "D"
impingement scrubbers control the total air flow through the prill tower and
the fluidized bed. The number of scrubbers in use at any one time depends
upon factors such as the feed rate of urea melt, desired prill size, and ambi-
ent temperature and humidity . . . Note 8 ...
The eight scrubbers were installed when the plant was built as originally
designed. Each scrubber used two fans in series, rated at 149200 watts (200
horsepower) each. In addition, a packed bed was installed to help control
ammonia emissions. As a result of stack emission tests after the plant
started operation, the units were redesigned so that only one fan was required
for each scrubber. This redesign was performed in conjunction with the
elimination of the packed bed . . . Note 9 ...
Note 8 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 9 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
-55-
-------
Scrubber liquor used for the Joy scrubbers comes from the ammonia recovery
strippers . . . Note 10 ... A bleed stream is taken from the scrubber liquor
holding tank on top of the tower and is concentrated to 50 percent by the
addition of off-size urea prills from the product screens. This stream is
recycled back to the concentrator.
3.3 Production Rate Monitoring
In order to determine whether the production line was operating at repre-
sentative steady-state conditions during testing, various process and control
equipment operating parameters were monitored . . . Note 11 ...
During testing of the prill tower, a radioactive source product counter
was used to measure the weight of the product leaving the screens . . . Note
12 ... Before the testing was started the product counter was calibrated by
filling a railcar directly and weighing the railcar before and after. The
weight difference was compared with the product counter readings and a cali-
bration factor was calculated . . . Note 13 ... Table 3-1 presents average
production rates for the prill tower during fertilizer grade and feed grade
tests.
During testing of the urea synthesis and concentration operations, the
flowrate of the urea solution to the concentrators was monitored and record-
ed. A urea surge tank is located between the synthesis and concentration
steps. This surge tank was maintained at a constant level, thus allowing the
use of the flow meter to relate the synthesis production rate to the concen-
tration production flow. Both the NH and CO feed rates to the
Note 10 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 11 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 12 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 13 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
-56-
-------
TABLE 3-1
AVERAGE PRODUCTION RATES
DURING EMISSIONS TESTS
AT W.R. GRACE AND CO., MEMPHIS, TENNESSEE
Process
Test
Production Rate
Tons/Hr Mg/Hr**
Prill Tower- Inlets $ Outlets to A § C Scrubbers Test No. 1 43.5 39.4
Fertilizer Inlets $ Outlets to A 5 C Scrubbers Test No. 2 45.8 41.6
Inlets § Outlets to A f, C Scrubbers Test No. 3 45.5 41.5
Inlet to A Scrubber Particle Size Test No. 1 57.2* 51.9
Inlet to A Scrubber Particle Size Test No. 2 45.5 41.3
Inlet to A Scrubber Particle Size Test No. 3 45.8 41.5
Inlet to C Scrubber Particle Size Test No. 1 48.3 43.8
Inlet to C Scrubber Particle Size Test No. 2 46.9 42.5
Inlet to C Scrubber Particle Size Test No. 3 45.8 41.5
Prill Tower-
Feed
Inlets 5 Outlets to A 5 C Scrubbers Test No.
Inlets $ Outlets to A 5 C Scrubbers Test No.
Inlets § Outlets to A § C Scrubbers Test
Inlet to A Scrubber Particle Size Test No.
Inlet to A Scrubber Particle Size Test No.
Inlet to A Scrubber Particle Size Test No.
Inlet to C Scrubber Particle Size Test No.
Inlet to C Scrubber Particle Size Test No.
Inlet to C Scrubber Particle Size Test No.
>. 1
i. 2
>. 3
1
2
3
1
2
3
47.2
47.4
45.9
46.4
45.3
46.5
44.7
46.9
46.8
42.8
43.0
41.6
42.1
41.1
42.2
40.5
42.5
42.4
Synthesis
Tower
Synthesis § Concentration Test No. 1
Synthesis § Concentration Test No. 2
Synthesis § Concentration Test No. 3
47.9
47.9
49.9
43.4
43.4
45.3
* Although the production rate data indicated this production rate, this value is
questionable.
grams per hour.
-57-
-------
synthesis process were also monitored to provide a check on the urea solution
flow meter . . . Note 14 ... The average production rates for each synthesis
and concentration test are shown in Table 3-1 also.
3.4 Production and Control Equipment Monitoring
In addition to the production rate determinations mentioned above, other
parameters were also monitored. During testing of the prill tower and its
scrubber emissions, spray header pressure, temperature of the melt after the
second evaporator, flowrate of the first concentrator, evaporator level, flow
rate of formaldehyde additive, density of the scrubber liquor in the holding
tank, and the level in the tank between the synthesis and concentration opera-
tions were monitored and recorded . . . Note 15 ...
Other synthesis and concentration operations parameters monitored and
recorded were: the ammonia feed rate and pressure; the carbon dioxide feed
rate, pressure, and temperature; the reactor skin and top temperatures; the
urea surge tank level and temperature; the dilute carbamate tank pressure; the
carbamate condenser pressure; aqua solution cooler pressure; and the percent
oxygen in the carbon dioxide feed . . . Note 16 ...
Due to the confidential nature of the monitored parameters, averages and
standard deviations cannot be presented. Instead, relative averages and
relative standard deviations expressed as percents are shown in Tables 3-2,
3-3 and 3-4. A value of one hundred percent represents the exact average of
all the values of that parameter for that series of tests. Standard
deviations were not calculated for particle size tests due to the limited
number of readings (three or less) . . . Note 17 ...
Note 14 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 15 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 16 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
Note 17 - See Item 1, Confidential Addendum, Contact Eric Noble, EPA, (919)541-5213.
-58-
-------
TABU- 3-2
RELATIVE VAUJES OF OPERATING PARAMETERS
DURING FERTILIZER GRADE PRILL TOWER EMISSION TESTS
(EXI'ltKSSED AS PERCENT 01- THE AVERAGE)*
I
ui
VO
Parameter
Spray Header Pressure
Melt Temperature
Plow to 1st Concentrator
Evaporator Level
Additive Flow Rate
S. (I.** of Scrubber Liquor
Urea Surge Tank Level
Unscreened Product Temperature
Scrubber Efficiency Tests
Test No. 1
AVG.
94
100
100
98
84
100
71
98
Std.
Dev.
300
0.00
182
45
80
0.00
149
101
Test No. 2
AVG.
93
100
99
94
90
100
84
101
Std.
Dev.
0.00
135
59
151
112
0.00
44
114
Test No. 3
AVG.
93
100
99
101
125
100
157
101
Std.
Dev.
0.00
165
59
104
108
300
106
85
Particle Size Tests
Inlet to A Scrubber
Test
1
133
99
-
93
-
100
52
-
Test
2
100
100
102
95
92
100
75
-
Test
3
100
100
102
95
92
100
75
-
Inlet to C Scrubber
Test
1
101
100
100
98
102
100
54
-
Test
2
93
100
99
101)
82
101)
122.
.
Test
3
93
liil
99
• 127
133
100
209
-
Speci fie Gravity
The numbers presented in this Table were derived by averaging all the values from all three of the fertilizer grade tests and
dividing that number into the average for a particular test. Standard deviations were not calculated for particle size tests
due to the limited number of readings (three or less).
-------
TABLE 3-3
REUTIvn VALUES OP OPERATING PARAMETERS
DURING FEED GRADE PRILL TOWER EMISSION TESTS
(EXPRESSED AS PERCENT OF Tin- AVERAGE)*
1 I
cr>
O
Parameter
Spray Head Pressure
Melt Temperature
Flow to 1st Concentrator
Evaporator Level
Additive Flow Rate
S. G.** of Scrubber Liquor
Urea Surge Tank Level
Unscreened Product Temperature
Scrubber Efficiency Tests
Test No. 1
AVG.
101
100
103
90
92
100
169
103
Std.
Dev.
129
98
102
93
188
0.00
0.00
30
Test No. 2
AVG.
97
100
99
95
107
100
149
102
Std.
Dev.
147
105
130
102
46
300
148
100
Test No. 3
AVG.
101
100
99
95
99
100
21
95
Std.
Dev.
24
98
68
105
65
0.00
152
170
Particle Size Tests
Inlet to A Scrubber
Test
1
97
100
99
89
106
100
169
-
Test
2
99
100
99
85
100
100
15
-
Test
3
111
100
99
137
100
100
4-1
-
Inlet to C Scrubber
Test
1
95
inn
IH2
90
89
1(10
1 69
-
Test
t
89
11)0
99
83
1(17
KID
139
-
Test
!S
111'.!
Hill
>i'i
1 id
99
Inn
:ii
-
** Specific Gravity
* The numbers presented in tin's table were derived by averaging all the values from all three of the feed grade tests and dividing that number
into the average of a particular test. Standard deviations were not calculated for particle size tests due to the limited number of readings
(three or less!.
-------
TABI.F. 3-4
RELATIVE VALUES OF 01'F.RATING PARAMETERS
DURING SYNTHESIS VTiWr I-MTSSION TESTING
(EXPRESSED AS PERCENT OF THE AVERAGE)*
Parameter
N1I3 Peed Rate
C02 Feed Rate
Nllj Pressure to Reactor
002 I'ressure to Reactor
Reactor Skin Temperature
Reactor Top Temperature
Urea Surge Tank Temperature
Urea Surge Tank Level
Flow to 1st Concentrator
Dilute Carharaate Tank Pressure
Carhamate Condenser Pressure
Aqua Solution Cooler Pressure
\ 02 in C02 Feed
C02 Feed Temperature
Test 1
AVG.
10J
99
103
98
100
100
100
56
98
96
100
100
94
99
Std.
Dev.
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
100
0.00
0.00
0.00
0.00
Test 2
AVG.
99 .
100
98
101
100
100
100
111
98
99
100
100
107
100
Std.
Dev.
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
88
0.00
0.00
300
0.00
Test 3
AVG.
100
101
99
101
100
100
100
133
104
105
100
100
99
100
Std.
Dev.
300
300
300
0.00
0.00
0,00
0.00
0.01)
300
112
0.00
0.00
0.00
11.0(1
* Note: The numbers presented in this table are derived by averaging all the values from all three of the synthesis vent test;
and dividing that number into the average for a particular test.
-------
3.5 General Plant Operation
Overall, the entire urea plant operated smoothly, as the data in Taoles
3-1 through 3-4 indicate. However, just before the first fertilizer grade
particulate test on the inlets and outlets to scrubbers A and C, the fan belts
on scrubber C broke causing a one hour and fifteen minute delay in starting
the test. In addition to the fan belts problem, some of the CO compres-
sors went down occassionally for short periods of time, but not during synthe-
sis tower tests. During the third test of the synthesis vent, the feed rate
of the urea melt to the concentrators had to be slightly increased in order to
maintain the level in the urea surge tank. None of these problems should
affect the test results.
-62-
-------
4.0 LOCATION OF SAMPLING POINTS
This section presents descriptions of the sampling locations used during
the emissions testing program conducted at the w. R. Grace and Co. urea manu-
facturing plant in Memphis, Tennessee during August and December 1979. Figure
4-1 shows an overhead schematic of the prill tower and adjacent facilities.
Figure 4-2 shows a cross-sectional schematic of the prill tower ana one of the
eight identical scrubbers atop the prill tower.
4.1 Prill Tower Scrubber Inlets
The scrubber A and scrubber C inlet sampling sites were each located in
59 3/8 inch I.D. vertical sections of steel duct. A schematic of these iden-
tical inlets, including traverse point locations, is present in Figure 4-3.
Two four-inch pipe flange sampling ports positioned 90 degrees apart were
located 77 inches (1.3 duct diameters) downstream from the top of the inside
of the prill tower; the nearest disturbance downstream from the ports was a
contraction beginning 38 1/2 inches (0.7 duct diameters) from the ports.
The inlet sampling locations did not meet the "eight and two diameters"
criterion as described in EPA Method 1; hence 24 sampling points were used on
each of the two traverse axes, for a total of 48 sampling points. Figure 4-3
shows a cross-sectional view of the duct at the sampling location and the
exact distance of each traverse point from the outside flange edge.
The scrubber A and scrubber C inlets were tested for particulate, while
scrubber inlets B, D, E, F, G and H (each identical to the A and C inlets)
were monitored only for temperature and gas velocity. Consequently, for these
six inlets only 14 sampling points were used on each traverse axis, for a
total of 28 sampling points for each inlet as specified by EPA Method 1.
These points were located as shown in Figure 4-4, which shows a cross-
-63-
-------
O
1—BAGGING TRANSFER
CONVEYOR
—BAGHOUSE FOR
BAGGING OPERATION
CONTROL
ROOM
TEMPERATURE AND
RELATIVE HUMIDITY
MEASUREMENT
LOCATION
PRODUCT TRANSFER-
CONVEYOR
O O
NOTE: EMISSIONS TESTS PERFORMED
ON SCRUBBERS A AND C
O
FIGURE 4-1
OVERHEAD VIEW OF PRILL TOWER AT
W. R. GRACE AND CO. ,
MEMPHIS, TENNESSEE
-64-
0988-011-001
-------
CLEAN AIR OUT
EL. 241'-Q"
•STACK EXTENSION
EL. 216'
VALVE OFF DURING -
TESTING *~y
TO EVAPORATOR AND
RECYCLE AS MOLTEN UREA
IRRIGATION PUMP J
_Q11 25 H. P. EACH *£^{
L. 199'-6"
186 '-0'J
MOL
i
TEN
UREA
x
a
-1
ii illll
\
f
>
*••
%
y
f
1 1 1 ii i
/
\
OVERHEAD
•* — WATER WASH
WATER SPRAY
J~ LEADS
iJ^N
t:^r\ \
vJh
v
ELECTRICAL AND FAN ROOM
FAN .,„•»
PRILLING ROOM SAMPUNG PORT-*
DAMPER^
FLOOR OFJPRILL ROOM 1 1
SPRAY HEADS-*;A _.A f&
.W*..» .•-•*•.•. ...tVA
-»
\
: ••
: t*
" C
— (
I""*
1
r \
y
mm
Xft
O
\
>—
H-
/
k
4
DUST LADDEN AIR — '
50'
^
r38"
-T t
T 9'-6'
1
— 59" I.D
FIGURE 4-2: SCHEMATIC OF PRILL TOWER AND TYPICAL SCRUBBER AT
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
0988-012-001
-65-
-------
I
ON
ON
TRAVERSE POINT
NUMBER
1
t.
3
4
5
6
7
8
9
10
11
1?
13
14
15
16
17
18
19
20
21
22
23
24
TRAVERSE POINT
LOCATION FROM
OUTSIDE OF
NIPPLE (INCHES)
5
5-7/8
7-1/4
8-5/8
10-1/4
11-3/4
13-1/2
15-1/2
17-5/8
20
23
27-1/2
39-1/2
43-7/8
47
49-3/8
51-1/2
53-1/2
55-1/4
56-3/4
58-3/8
59-3/4
61-1/8
62
FIGURE 4-3:
FLOOR-
PRILL TOWER
PRILL TOWER
SCRUBBER
INLET PORTS
38.5"
6'
77"
59-3/8"
63-3/8"
NORTHEAST (A)
SOUTH (C)
900
SOUTHEAST (A)
WEST (C)
SCRUBBERS A AND C INLET SAMPLING LOCATIONS (BOTH IDENTICAL)
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
n9«R-ni3-noi
-------
TRAVERSE POINT
NUMBER
1
2
3
4
5
6
7
8
9
10
11
12
13
14
TRAVERSE POINT
LOCATION FROM
OUTSIDE OF
NIPPLE (INCHES)
5.1
7.4
9.8
12.6
15.9
19.9
25.6
41.4
47.1
51.1
54.4
57.2
59.6
61.9
FLOOR-
PRILL TOWER
PRILL TOWER
SCRUBBER
INLET PORTS
38.5"
6'
T
77"
59-3/8"
Mill Hill » t» 4- • «lll
63-3/8"
900
FIGURE 4-4: SCRUBBERS B,D,E,F,G,H INLET SAMPLING LOCATIONS (ALL IDENTICAL)
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
0988-014
-------
sectional view of a duct at the sampling location and lists the exact distance
of each traverse point from the outside flange edge.
4.2 Scrubber A and C Outlets
After passing the inlet test section, the prill tower dust-laden gases are
drawn through a fan which discharges to the scrubber. The cleaned gases are
then exhausted to the atmosphere through a mist pad. A stack extension
approximately 10 feet in height was added so that a reasonable sampling trav-
erse plane could be established free from interferences from the mist pad and
the wind.
The A and C scrubber outlet stacks were 144 inches in internal diameter
and were fitted with two 1-3/4 inch pipe flange sampling ports positioned
90° apart. The sampling ports were located 2 feet 6 inches (0.2 duct diam-
eters) downstream from the mist pad, and 8 feet 3 inches (0.7 duct diameters)
upstream from the top of the stack extension.
The outlet sampling locations did not meet the "eight and two diameters"
criterion as outlined in EPA Method 1; hence 24 sampling points were chosen
for each traverse axis for a total of 48 sampling points at each outlet.
These points were located as detailed in Figure 4-5, which shows the cross-
sectional view of the duct at the sampling location and lists the exact dis-
tance of each traverse point from the outside flange edge.
4.3 Inlet Particle Sizing Locations
Particle sizing tests were performed in both the scrubber A and the scrub-
ber C inlet gas streams. An in-stack cascade impactor was positioned in the
duct through a port used for the particulate emissions tests. The impactor
nozzle was positioned for each run at a point of average velocity as deter-
-68-
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TO ATMOSPHERE
I
ON
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)
3-3/8
6-3/8
9-5/8
13-1/8
16-7/8
20-3/4
24-7/8
29-5/8
34-7/8
40-7/8
48-1/4
59
88-1/2
99-1/4
106-5/8
112-5/8
117-7/8
122-5/8
126-3/4
130-5/8
134-3/8
137-7/8
141-1/8
144-1/8
STACK _
EXTENSION
PRILL TOWER
SCRUBBER
OUTLET PORTS
8'-3'
MIST PAD
2'-6'
12'
IMU Mill « l« 4- HH im»t«l
12' - 1-3/4"
NORTHEAST (A)
WEST (C)
90°
SOUTHEAST (A)
NORTH (C)
FIGURE 4-5: SCRUBBERS A AND C OUTLET SAMPLING LOCATIONS (BOTH IDENTICAL)
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
09HH-01&-001
-------
mined by preliminary velocity traverses performed before each particle size
test run. The impactor nozzle was rotated directly into the gas stream at an
angle determined by the cyclonic flow angle traverses.
The specific sampling ports and points used during the particle size test
runs were as follows {see Figure 4-3):
Scrubber Inlet Fertilizer Test Runs Feed Test Runs
4.4
A
C
Urea
I
SE-11
S-5
Synthesis Tower Main Vent
2
NE-8
S-5
Sampling
2
NE-8
S-5
Location
1
SE-3
S-22
2
NE-8
S-20
_3
NE-12
W-15
The synthesis tower vent sampling location was in a 29-inch I.D. vertical
section of steel duct containing one four-inch pipe flange sampling port.
This port location met the "eight and two diameters" criterion which would
have allowed, in this case, a total of 12 sampling points over two traverses.
However, because of the physical limitations incurred by the use of an in-
stack orifice, only the back half of the one traverse could be sampled for a
total of 3 sampling points. These points were located as shown in Figure 4-6.
4.5 Visible Emissions Observation Locations
The white plumes exiting the prill tower scrubber stacks were observed
from nine different locations. These locations were chosen to conform with
EPA Reference Method 9 requirements and to allow observation of both individ-
ual and combined scrubber plumes. The plume from the baghouse on top of the
bagging operation warehouse was observed from within 15 feet of the baghouse
outlet. These locations are described in Table 4-1 and shown in Figures 4-7
and 4-8.
-70-
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TO ATMOSPHERE
TRAVERSE POINT
NUMBER
1
2
3
POINTS!?
SAMPLED! j!
TRAVERSE POINT
LOCATION FROM
OUTSIDE OF
NIPPLE (INCHES)
5-1/4
8-1/4
12-1/2
24-3/8
28-3/4
31-3/4
o
GREATER THAN
2 STACK DIA.
GREATER THAN
8 STACK DIA.
ONLY BACK HALF WAS
SAMPLED DUE TO IN-
STACK ORIFICE
FIGURE 4-6: LOCATION OF SOLUTION TOWER TEST PORTS AND POINTS AT
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
0988-016
-------
TABLE 4-1
VISIBLE EMISSION OBSERVATION LOCATIONS
AT W.R. GRACE AND CO., MEMPHIS, TENNESSEE
Distance To
Height
Direction From
Observer
Location
A
B
C
D
E
F
G
H
I
J
Discharge
Point (Feet)
450
40
450
450
450
40
400
500
400
5-15
Above Ground
(Feet)
0
200
0
0
0
200
0
0
0
0
Discharge
Point
SE
SSE
E
SE
SSW
E
SW
S
ESS
S
Discharge
Description
Prill Tower
IT
II
II
II
II
It
II
II
Bag House
-72-
-------
A,D
co
I
GATE
BULK
WAREHOUSE
*J
WAREHOUSE
E
z
=
n
i
=
a
(\
\i
|
CO
• i
RILM
OWER/
:=3
a
NTROL
*OOM
i
i
i
!
1
1
i
:
i
i
i
i
* OBSERVER LOCATIONS (see Table 4-1 for descriptions)
NOT TO SCALE
*H
AMMONIA
PLANT
*E
*G
1
LAB 1
FIGURE 4-7: VISIBLE EMISSION OBSERVER LOCATIONS
MEMPHIS, TENNESSEE
0988-017
-------
TOP VIEW OF PRILL TOWER
POSITION B OBSERVING STACK C
POSITION F OBSERVING STACK A
SCRUBBER
C
o
/ SCRUBBER V
ELEVATOR
SHAFT
N
* OBSERVER LOCATIONS
(see Table 4-1 for descriptions)
FIGURE 4-8: VISIBLE EMISSION OBSERVER LOCATIONS AT
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
0988-01R
-------
The plumes were all 'observed against partly cloudy or clear blue skies.
The urea synthesis tower vent plume continuously mingled with some of the
scrubber plumes so that separate opacity readings for the vent plume were not
possible.
4.6 Scrubber Pressure Drop Measurement Locations
Pressure drops across the eight prill tower scrubbers were measured with a
verticle U-tube water manometer connected across the venturi throat of each
scrubber.
4.7 Process Sample Collection Locations
The unscreened solid product samples were collected during both fertilizer
and feed grade tests. The samples were collected at the bottom of the prill
tower, as the product fell onto the vibrator screens. Samples of the synthe-
sis solution and urea melt were also taken directly from their associated pro-
cesses.
4.8 Scrubber Liquor Collection Locations
Scrubber liquor samples were collected from the streams entering and exit-
ing the prill tower A and C scrubbers. The samples were collected at three
locations as shown in Figure 4-9. Outlet samples were collected from the sep-
arate return pipes adjacent to scrubbers A and C. The inlet samples were col-
lected from one tap on the common sump feeding all of the scrubbers.
4.9 Ambient Air Temperature and Relative Humidity Measurement Location
Ambient air temperature and relative humidity measurements were taken at
the base of the prill tower during each emission test run. Figure 4-1 shows
the location of this measurement point.
-75-
-------
TOP VIEW OF PRILL TOWER
CTi
I
ELEVATOR
SHAFT
LEGEND
* OUTLET
0 INLET SUMP
FIGURE 4-9: SCRUBBER LIQUOR SAMPLING POINTS ON THE PRILL TOWER AT
W. R. GRACE AND CO., MEMPHIS, TENNESSEE
0988-019
-------
5.0 SAMPLING AND ANALYSIS METHODS
This section presents general description of sampling and analysis
procedures employed during the emissions testing program conducted at the
W. R. Grace and Co., Memphis, Tennessee urea manufacturing facility during
August 13-22, 1979. Details of sampling and analysis procedures are contained
in Appendices I and J.
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 Sta-
tionary Sources", Appendix A, Federal Register, Volume 42, No. 160, Thursday,
August 18, 1977, pp 41755 ff.
o 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 ana local flow
disturbances. In addition, this method discusses the pitot-nulling
technique used to establish the degree of cyclonic flow in a duct.
o Method 2 - Determination of Stack Gas Velocity and Volumetric Flowrate
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.
o Method 3 - Gas Analysis for CO2, C>2/ Excess Air and Dry Molecular Weight
This method describes the extraction of a grab or integrated gas
sample from a stack and the analysis of that sample for CC>2 and
02 with an Orsat analyzer.
o 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 conden-
sation impingers. The assembly and operation of the required sampling
train is specified.
-77-
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o Method 5 - Determination of Particulate Emissions from Stationary
Sources
This method specifies the isokinetic sampling of participate matter
from a gas stream utilizing techniques introduced in the above four
methods. Sample collection and recovery, sampling train cleaning ana
calibration, and gas stream flowrate calculation procedures are spec-
ified.
o Method 9 - Visual Determination of the Opacity of Emissions from
Stationary Sources
This method describes how trained observers are to determine the opa-
city of emissions. The duration and frequency of observations, ori-
entation of the observer with respect to the source, sun and back-
ground, methods of data recording and calculation, and qualifications
of observers are specified.
Presently, methods of cyclonic flow measurement and interpretation are
largely in their formative stages. As noted in Section 2.6, some degree of
cyclonic flow was evident in all eight scrubber inlets, caused by the axial
flow fans in these ducts. The alignment approach^ ' was used during the
inlet sampling tests to properly account for the effects of cyclonic flow, as
follows:
1. A preliminary traverse was performed at each inlet before every test
to establish the flow angles at each traverse point. The pitot-
nulling technique, as detailed in EPA Reference Method 1, was used to
measure the flow angles.
2. During particulate or velocity traverses the probe tip was rotated
according to the flow angles at each traverse point, so that the
probe tip faced directly into the gas flow. The flow angle was
recorded on the field data sheets along with all other pertinent data.
3. During the particulate traverses, the sampling time at each traverse
point was weighted by the cosine of the flow angle at that point.
These sampling times are noted on the field data sheets.
4. The cosine of the flow angle was applied to the velocity equations
used to calculate the flowrate in the scrubber inlets.(2)
"Evaluation of Particulate Sampling Methods for Cyclonic Flow," Westlin,
P.R., et al., OAQPS, ESED, EMB, TSS, August 2, 1979.
2 Source Sampling Reference Method, prepared by Entropy Environmentalists,
Inc., for USEPA, November, 1977.
-78-
-------
Angular flow in ducts is a complex phenomenon for which the measurement
and analysis technique described above, as well as other proposed techniques,
are only an approximation to what is actually occuring in a duct. For
example, angle measurement by pitot-nulling is convenient, utilizing equipment
already part of the particulate sampling train. However, only one component
of the 3-dimensional flow vector is measured in this way, and whether or not
this measured component is a significant component of the flow vector is not
always known. Further work is needed to develop an accurate angular flow
determination method that is readily adaptable to source sampling in the field.
5.2 Urea Sampling and Analysis at the Prill Tower Scrubbers
5.2.1 Sampling Methods
Urea, ammonia and formaldehyde in the inlet and outlet gas stream of the
prill tower scrubbers A and C were sampled at points located in accordance
with the relationship, detailed by EPA Method 1, of the sampling ports to up-
stream and downstream flow disturbances. The velocity of the duct gas was
measured using S-type pitot tubes constructed and calibrated in accordance
with EPA Method 2. Cyclonic flow in the scrubber inlets was handled as
described above in Section 5.1.
The sampling train used on this sampling program is shown in Figure 5-1
and is a modification of the standard EPA Method 5 particulate sampling
train. The modifications used were: altered impinger sequence, absence of a
filter and use of a teflon line.
The sampling train shown in Figure 5-1 consists of a nozzle, probe, teflon
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 con-
nected to a 5/8-inch stainless steel glass-lined probe wrapped with nichrome
-79-
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STACK HALL
THERMOMETER
i
00
o
I
LEGEND
1 - NOZZLE 7
2 • PRODE 0
3 - TEFLON LINE 9
4 - ICE OATH 10
5 - FLEXABLE5 LINE 11
6 - VACUUM GAGE 12
NEEDLE VALVE
PUMP
DRY GAS METER
ORIFICE
PITOT TUDE ft INCLINED MANOMETER
POTENTIOMETER
FIGURE 5-1:
MODIFIED EPA PARTICULATE SAMPLING TRAIN
AUGUST 18,1977, FEDERAL REGISTER
0980-020
-------
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 two impingers con-
tained deionized, distilled water (100 mis each). The next two impingers con-
tained IN H2so4 (100 mis each). The fifth impinger was empty, and the
sixth contained 200 grams of indicating silica gel. Leaving the last impin-
ger, the sample stream flowed through flexible tubing, a vacuum gauge, neeule
valve, pump, and a dry gas meter. A calibrated orifice and inclined manometer
completed the train. The stack velocity pressure was measured using a pitot
tube and inclined manometer. Stack temperature was monitored with a thermo-
couple attached to the probe and connected to a potentiometer. A nomograph
was used to quickly determine the orifice pressure drop required for any pitot
velocity pressure and stack temperature in order to maintain isokinetic samp-
ling conditions.
The probe temperature was maintained at about 10°F above the duct gas
temperature (if the gas temperature did not exceed approximately 160°F) in
order to prevent condensation within the probe. Where the gas temperature
exceeded 160°F, the probe was maintained at 160°F.
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, orifice pressure drop and, at the
scruober inlets, the flow angle.
The only significant problem encountered during the sampling tests was the
necessity of interrupting sampling runs while the fans in the scrubber inlet
ducts were washed. These interruptions occurred frequently because of the
heavy particulate load accumulated by the fans.
-81-
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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 connecting
glassware were rinsed with deionized, distilled water and brushed (three
times). Samples were put in glass jars with teflon-lined caps, as follows:
Jar ttl - contents of the nozzle, probe, flexible teflon line, first two
impingers, their connecting glassware, and their deionizea, dis-
tilled water wash.
Jar 12 - contents of the third, fourth and fifth impingers, their con-
necting glassware, and their IN ^504 solution rinse.
Jar 13 - silica gel from the sixth impinger.
The contents of the first jar were filtered using a tared Buchner funnel
filter and a vacuum filtration apparatus in order to remove all traces of
undissolved material. The funnel filter was then stored in a labelled petri
dish and returned to the TRC chemical laboratory. A portion of the filtrate
was set aside untreated for analysis for formaldehyde content. To the other
portion, a small amount of sulfuric acid was added to bring the pH to less
than 6; this portion was in turn divided into two portions for the urea and
ammonia analyses.
5.2.3 Sample Analysis
The acid impinger samples (jar #2) and the acidified portion of the water
impinger samples (jar #1) were analyzed for urea at the TRC laboratories.
Prior to shipment to TRC, the samples were distilled at the W. R. Grace and
Co. laboratory in order to remove any ammonia. At TRC the samples were ana-
lyzed with the p-dimethylaminobenzaldehyde colorimetric method within 20 days
of sample collection. Preliminary distillation to remove ammonia was per-
formed because ammonia is a known interference in this analysis.
-82-
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One problem was encountered during these analyses. At the beginning of
the urea analyses it was noted that the acid impinger samples (from jar »2)
were yielding negative absorbances. The TRC chemist reasoned that since the
acid impinger samples were preserved with IN H so. and the water impin-
ger samples were preserved with H2S04 at a concentration of only 2
ml/liter, the sulfuric acid may be a negative interference. A test of this
hypothesis with distilled water blanks showed that H So. did indeed
cause negative interference. Based on this information, the urea analyses
were then performed with standards prepared with the same H SO concen-
tration as the samples. Complete details of the urea analyses are contained
in Appendix J.
5.3 Ammonia Sampling and Analysis at the Prill Tower Scrubbers
5.3.1 Sampling, Sample Recovery and Preparation
The same samples collected, recovered and prepared as described in Section
5.2.1 and 5.2.2 were analyzed for ammonia as well as urea.
5.3.2 Sample Analysis
The acid impinger samples and the acidified portions of the water impinger
samples were analyzed for ammonia using two methods: specific ion electrode
(SIE) method and direct Nessler method.
The SIE analyses were performed at the W. R. Grace and Co. laboratory
within 48 hours of sample collection. An Orion model 95-10 ammonia electrode
was used in accordance with the electrode manufacturer's procedures. This
method is extremely specific for ammonia and is subject to few, if any, inter-
ferences.
-------
The Nessler analysis method ^ ^ was performed at the TKC laboratory
within 20 days of sample collection. This is a colorimetric method subject to
turbidity interference from a variety of species. In addition, aelays in
sample analysis may allow dissolved ammonia to diffuse out of solution, yield-
ing reduced ammonia concentrations. Alternatively, delays in sample analysis
may result in some species, like urea, breaking down or converting to ammonia
and yielding falsely high ammonia concentrations.
These two ammonia methods yielded results that agree closely with each
other, but a consistent difference is evident. The following is a summary of
the ammonia sample catches:
Average Ammonia Sample Weight (mg)
Sample Location
A inlet
A outlet
C inlet
C outlet
Syn. Tower 70984 67794
For all fertilizer tests at the A and C scrubbers, the direct Nessler (DN)
results averaged 7.6% higher than the specific ion electrode (SIE) results.
For all feed tests (excluding the synthesis tower), the DN results averaged
2.8% higher that the SIE results. One factor involved here may be the time
Fertilizer
DN
224
750
145
222
SIE
202
709
133
212
Feed
DN
574
325
501
339
SIE
542
324
479
338
Standard Methods of Water and Wastewater Analysis, 14th Edition, 1975, p
412 ff.
-84-
-------
elapsed between sample collection and sample analysis. The SIE analyses were
performed within 48 hours after sample collection, while the DN analyses were
performed up to 20 days after sample collection. Some conversion of urea to
ammonia may have occurred in the samples waiting for DN analysis. Since the
feed tests were performed one week after the fertilizer tests, less urea
conversion occurred in the feed samples.
5.4 Formaldehyde Sampling and Analysis at the Prill Tower ScruDbers
The same samples collected, recovered and prepared as described in Section
5.2.1 and 5.2.2 were analyzed for formaldehyde as well as urea and ammonia.
The untreated portions of the water impinger samples were analyzed for formal-
dehyde at the TRC laboratory within 20 days of sample collection using the
chromotropic acid colorimetric analysis method.
5.5 Insoluble Particulate Sampling and Analysis at the Prill Tower Scrubbers
The water impinger samples (collected as described in Section 5.2.1) were
analyzed for insoluble particulate (undissolved solids) as follows. The con-
tents of jar #1 were suction-filtered using a previously desiccated, tared
glass fiber filter, Buchner funnel and vacuum system, as described in Section
5.2.2. The filter was then placed in a petri dish and brought to TRC. In the
TRC Laboratory, the filters were desiccated and weighed to a constant weight.
This analysis took place within 20 days of sample collection.
5.6 Synthesis Tower Emissions Tests
5.6.1 Sampling and Analysis for Urea and Ammonia
Emissions tests at the urea synthesis tower main vent were performed in a
manner similar to that described in Section 5.2, with the following modifica-
tions to the sampling train and sampling method:
-85-
-------
1. An in-stack orifice was used to permit isokinetic sampling of the
vent gas stream which had a moisture content greater than 50%. The
in-stack orifice measures the sample stream flowrate in the probe at
the same moisture and temperature conditions as in the stack.
2. -Only three traverse points were used because of the physical limita-
tions imposed by the in-stack orifice.
3. Two extra impingers were added to allow for more complete sample
collection. Impingers 1-3 each contained 100 ml of distilled,
deionized water; impingers 4-6 each contained 100 ml of ION
H2SO4; impinger 7 was empty, and impinger 8 contained 200 grams
of silica gel. The empty impinger was placed immediately in front of
the 8th impinger to act as a demister to prevent too rapid saturation
of the silica gel.
The ION H2S04 was used in two of tne three test runs. In the third
test run, 5N H2SO. was used. The reason for this was that the ION solu-
tions had to be substantially diluted in order to respond to the specific ion
electrode ammonia analysis. With this analysis method, as the sample is
diluted the sensitivity of the electrode decreases.
A procedure similar to that described for the prill tower scrubbers in
Section 5.2 and 5.3 was followed for the synthesis tower sample recovery and
preparation. The contents of the sample jars were:
Jar #1 - contents of the first 3 impingers and the distilled water wash
of the nozzle, probe, teflon line and impinger connecting glass-
ware.
Jar 12 - contents of impingers 4, 5, 6, and 7 and the concentrated acid
rinse of these impingers and their connecting glassware.
Jar #3 - silica gel from impinger 8.
The contents of jars #1 and 12 were analyzed for urea, ammonia and insoluble
particulate as described in Sections 5.2, 5.3 and 5.5, respectively.
-86-
-------
The in-stack orifice was calibrated in the field at W. R. Grace and Co.
prior to the synthesis tower tests. The purpose of the calibration was to
determine a value for the coefficient B in the following equation:
Ah = (B) (AP)
where Ah = pressure drop across the orifice (inches water)
AP = velocity pressure (inches water).
With B determined, a nomograph was used to establish isokinetic flow in the
sampling train: for a given measured Ap in the stack, the pressure drop Ah
across the orifice was adjusted to the proper value.
A typical in-stack orifice assembly is shown in Figure 5-2. A detailed
description of the in-stack orifice calibration is contained in Appendix K.
5.6.2 Integrated Gaseous Bag Samples
Integrated gaseous bag samples were collected from the synthesis tower
main vent during each of the urea particulate test runs at this location.
Samples were drawn directly from the gas stream with an Integrated Orsat
Sampler. The bag samples were analyzed for CO and 0 at the W. R.
Grace and Co. laboratory within one hour of sample collection using an EPA
Method 3 Orsat analyzer.
5.7 Visible Emissions
The visible emission measurements of the prill tower scrubber plumes were
conducted by two certified visual emission observers in accordance with EPA
Reference Method 9, These measurements were taken from two general loca-
tions: one observer was atop the prill tower directly across from either the
A or C scrubber outlet; the other observer was on the ground, observing either
the same scrubber plume concurrently with the first observer or observing com-
-87-
-------
TO SAMPLING TRAIN
i
00
00
ADAPTORS
MANOMETER
TAPS
TIP
FIGURE 5-2: TYPICAL IN-STACK ORIFICE AND NOZZLE ASSEMBLY
0988-021
-------
bined plumes from all operating scrubbers. Observations of a given plume
lasted from one-half hour to about two hours, and within an observation period
readings were taken and recorded at 15-second intervals.
Visible emission measurements of the baghouse plume were conducted over a
period of five hours by a single certified observer positioned within 15 feet
of the baghouse outlet atop the bagging operation warehouse.
Visible emission measurements of the synthesis tower main vent plume were
specified in the original work assignment. These measurements were subse-
quently cancelled by the EPA technical manager because the vent plume mixed
with the scrubber plumes.
I
5.8 Particle Size Tests
Particle size tests were performed at the inlets to scrubbers A and C
using an Anderson cascade impactor with a pre-impactor. The impactor was
operated in its in-stack mode in accordance with the manufacturer's procedures.
Prior to the initiation of sampling, the impactor was leak tested and
placed in the duct for 20 minutes to allow it to heat to duct temperature in
order to prevent condensation. Sampling began immediately upon rotation of
the nozzle into the flow stream, taking into account the observed cyclonic
flow angle. Sampling was performed isokinetically from a single average flow
point that was predetermined from velocity traverses performed prior to each
particle size test run. Each of the fertilizer tests lasted 30 minutes; each
of the feed tests lasted 15 minutes.
The impactor was loaded -before each test run with pre-weighed glass fiber
collection substrates. Upon completion of a test run, the substrates were
removed in a secluded, clean area and placed in petri dishes and sealed. The
cyclone preseparator contents were brushed into a tared sample jar and
-89-
-------
sealed. These samples were brought to TRC and were weighed on an analytical
balance to 0.1 mg in a constant humidity environment.
5.9 Volumetric Flowrate Measurements in the Scrubber Inlets
Velocity traverses were performed in the inlets of scrubbers B, D, E, F,
G, and H before and after each fertilizer emission test run, and in the inlets
of scrubbers B and D before and after each feed emissions test run. Two per-
pendicular traverses were performed at each inlet during each velocity test,
with velocity head and stack gas temperature monitored at each sampling
point. The probe was rotated in accordance with the observed cyclonic flow
angle at each point; cyclonic flow angles were measured at each sampling point
prior to each "before" velocity test. From these data volumetric flowrates
were calculated in accordance with the alignment approach for cyclonic flow
calculations, as noted in Section 5.1.
During each fertilizer emission test run, single-point velocity head and
temperature measurements were taken approximately every 15 minutes at each of
these six scrubber inlets. Similar measurements were made at inlets B and D
during the feed emission test runs. These single average-flow points were
determined from preliminary velocity traverses, including the "before" trav-
erses. The appropriate cyclonic flow angle was applied with these single-
point measurements.
In order to compute the volumetric flowrates of each of these six inlets,
assumptions on the values of two parameters were made, based on the results of
the complete tests performed on scrubbers A and C. The duct static pressure
was assumed to be -2.0 inches of water for fertilizer and feed tests; the per-
cent moisture was asssumed to be 1.8% for the fertilizer tests, and 2.9% for
the feed tests. With these assumptions other necessary parameter values were
-90-
-------
calculated and, with the measured velocity head, temperature and cyclonic flow
angles, the flowrates were calculated.
5.10 Pressure Drop Measurements Across Prill Tower Scrubbers
Pressure drop measurements were taken across all eight prill tower scrub-
bers during the fertilizer tests and across scrubbers A through D curing the
feed tests. Measurements were taken .approximately every 15 minutes during
each test run using a vertical U-tube water manometer connected to pressure
taps across the throat of the scrubber venturi.
After the first fertilizer test run, the pressure drop across some of the
scrubbers was adjusted to obtain a more constant value across all the scrub-
bers. This adjustment was made by modifying the liquor level in each scrubber.
5.11 Scrubber Liquor Sampling and Analysis
Samples were taken from the common liquor stream going to scrubbers A and
C and from the separate streams returning from each of these two scrubbers.
Half-liter aliquots of the scrubber liquor were collected approximately every
30 minutes during each test run. The sample temperature was measured immedi-
ately after collection, and the pH was measured in the W. R. Grace and Co.
laboratory as soon as the sample reached room temperature. The individual
samples were then combined to form three composite samples for each test run
(one inlet sample and two outlet samples). These composite samples were then
vacuum-filtered through a tared glass-fiber filter. Each filtrate sample was
divided into two portions: to one portion concentrated sulfuric acid was
added to bring the pH to less than 6; the second portion remained untreated.
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The untreated portions were analyzed for urea and formaldehyde as
described in Sections 5.2 and 5.4, respectively. Formaldehyde analyses were
performed on samples from only one fertilizer test run and one feed test run.
The acidified portions were anlayzed for ammonia by the specific ion
electrode and direct Nezzler methods as described in Section 5.3 above. The
filter was desiccated and weighed to determined undissolved solids as
described in Section 5.5 above.
5.12 Ambient Air Temperature and Relative Humidity
Ambient air temperature and relative humidity were recorded periodically
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, and
psychrometric tables were then used to compute relative humidity from these
measurements.
5.13 Process Samples
One grab sample of the unscreened solid urea product was collected by TRC
personnel at the hopper inlets to the vibrating screen during each emission
test run. Bulk density and sieve analyses were then performed on these
samples at the W. R. Grace and Co. laboratory within two hours of sample col-
lection.
The bulk density was determined with a tared graduated cylinder and a
platform balance. The sample was passed through a riffle and then poured into
the graduated cylinder until it overflowed. The sample was then leveled with
the top of the cylinder, and the cylinder and contents were weighed.
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The particle size of the product was estimated by means of a sieve ana-
lysis. A small amount (about 250 grams) of sample was weighed to the nearest
0.01 gram. This sample was then poured into the top sieve ana then shaken
through the stack of sieves. After shaking, each sieve was weighed to deter-
mine the amount of material retained by it.
Samples of the urea process solution were taken by W. R. Grace and Co.
personnel from various locations in the process. Chemical analyses were per-
formed on these samples and on the solid product by W. R. Grace and Co. who
requested that the analysis results remain confidential.
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