.f* ~? r&r* United States Environmental Protection Agency Office of Air Quality Planning and Standards Research Triangle Park NC 27711 EMB Report 83-CDR 10 April 1 984 Air Emission Test Report American Cyanamid Company Savannah, Georgia ------- NSPS DEVELOPMENT PARTICULATE AND PARTICLE SIZING EMISSIONS TESTING TITANIUM DIOXIDE SPRAY DRYER AND CALCINER SYSTEMS AMERICAN CYANAMID COMPANY SAVANNAH, GEORGIA FEBRUARY 9-16, 1984 Compiled by: ENTROPY Post Office Box 12291 Research Triangle Park, N. C. 27709 68-02-3852 Work Assignment No. 2 EMB Project No. 81 REG 8 Task Manager Dan Bivins Emission Measurement Branch Emissions Standards and Engineering Division OFFICE OF AIR QUALITY PLANNING AND STANDARDS OFFICE OF AIR, NOISE, AND RADIATION U. S. ENVIRONMENTAL PROTECTION AGENCY RESEARCH TRIANGLE PARK, N. C., 27711 ------- DISCLAIMER Although the research described in this report has been funded wholly or in part by the United States Environmental Protection Agency through Contract 68-02-3852 to Entropy, it has not been subject to the Agency's peer and administrative review and therefore does not necessarily reflect the views of the Agency, and no official endorsement should be inferred. ------- TABLE OF CONTENTS LIST OF TABLES v LIST OF FIGURES vii 1. INTRODUCTION 1-1 1.1 Background 1-1 1.2 Scope of the Project 1-1 1.3 American Cyanamid Testing Program 1-1 1.3.1 Source Applicability 1-1 1.3.2 Outline of Testing Program 1-2 1.4 Report Organization 1-2 2. SUMMARY AND DISCUSSION OF RESULTS 2-1 2.1 Introduction 2-1 2.2 Chloride Process 2-1 2.2.1 General 2-1 2.2.2 #312 Baghouse Inlet 2-1 2.2.3 #312 Baghouse Outlet 2-2 2.2.4 #322 Baghouse Outlet 2-2 2.2.5 Spray Dryers Stack 2-2 2.3 Sulfate Process . . 2-18 2.3.1 General 2-18 2.3.2 East and West I.D. Fan Outlets 2-18 2.3.3 East and West ESP Outlets 2-19 2.3.4 #2 Calciner Exhaust Stack 2-19 2.3.5 #2 Calciner Product Outlet 2-19 3. PROCESS DESCRIPTION AND OPERATION 3-1 3.1 Introduction 3-1 3.2 Pollutants/Sampling Points 3-1 3.2.1 Spray Dryers 3-1 3.2.1.1 . Particulate Mass and Particle Sizing 3-1 3.2.1.2 Visible Emissions 3-1 3.2.1.3 Feed and Product Samplers 3-1 3.2.2 Rotary Calciner #2 3-4 3.2.2.1 Particulate Mass and Particulate Sizing 3-4 3.2.2.2 Visible Emissions 3-4 (continued next page) ------- ii TABLE OP CONTENTS (continued) 3.3 Process Description 3-4 3.3.1 Spray Dryers 3-4 3.3.2 Rotary Calclner #2 3-8 3.4 Process Conditions During Testing. . . 3-8 3.4.1 Spray Dryers 3-8 3.4.2 Rotary Calciner #2 3-10 4. SAMPLING LOCATIONS 4-1 4.1 Applicability of Sampling Sites 4-1 4.2 Chloride Process Sampling Locations 4-1 4.2.1 #312 Spray Dryer Inlet 4-1 4.2.2 #312 Settling Chamber Product Outlet . 4-1 4.2.3 #312 Baghouse Inlet 4-1 4.2.4 #312 Baghouse Product Outlet 4-4 4.2.5 #312 Baghouse Outlet 4-4 4.2.6 #322 Spray Dryer Inlet 4-4 4.2.7 #322 Baghouse Product Outlet ..... 4-4 4.2.8 #322 Baghouse Outlet 4-6 4.2.9 #312 and #322 Exhaust Stack, Particulate Sampling .... 4-6 4.2.10 #312 and #322 Exhaust Stack, Visible Emissions 4-6 4.3 Sulfate Process #2 Calciner Sampling Locations 4-9 4.3.1 #2 Calciner Inlet 4-9 4.3.2 Water Spray Cooler Outlet 4-9 4.3.3 East Side I.D. Fan Outlet 4-9 4.3.4 East Side I.D. Fan Inlet 4-9 4.3.5 West Side I.D. Fan Outlet 4-9 4.3.6 West Side I.D. Fan Inlet 4-13 4.3.7 East and West Sides ESP Outlets 4-13 4.3.8 #2 Calciner Exhaust Stack, Particulate Sampling 4-13 4.3.9 #2 Calciner Exhaust Stack, Visible Emissions 4-17 4.3.10 #2 Calciner Product Outlet 4-17 (continued next page) ------- Ill TABLE OF CONTENTS (continued) 5. SAMPLING AND ANALYTICAL METHODS 5-1 5.1 Sampling Objectives 5-1 5.2 Particulate Emissions Testing 5-1 5.2.1 #312 Baghouse Inlet 5-1 5.2.2 #312 Baghouse Outlet 5-1 5.2.3 #322 Baghouse Outlet 5-1 5.2.4 East and West I.D. Fans Outlets 5-2 5.2.5 East and West I.D. Fans Inlets 5-2 5.2.6 East and West ESP Outlets 5-2 5.3 Sulfuric Acid Mist 5-2 5.4 Trace Metals Analysis 5-2 5.5 Sieve Analysis and Moisture Content 5-2 5.6 Plume Opacity 5-3 5.7 Fugitive Emissions 5-3 5.8 Particle Size Testing 5-3 6. QUALITY ASSURANCE 6-1 6.1 Introduction 6-1 6.2 Sampling Train Components 6-1 6.3 Preseparator and Cascade Impactors . 6-1 6.4 Sample Collection Substrates 6-1 6.5 Substrate Weighing 6-2 6.6 Sample Analysis 6-2 6.7 EPA Method 3 6-2 6.8 EPA Method 9 6-2 7. APPENDICES 7-1 7.1 Chloride Process Test Results and Example Calculations ... 1 7.1.1 #312 Spray Dryer Baghouse Inlet 2 7.1.2 #312 Spray Dryer Baghouse Outlet 25 7.1.3 #322 Spray Dryer Baghouse Outlet 39 7.1.4 #312 and #322 Spray Dryers Stack 59 (continued next page) ------- IV TABLE OF CONTENTS (continued) 7.2 Sulfate Process #2 Calciner Test Results and Example Calculations 63 7.2.1 #2 Calciner I.D. Fan Outlet (East) 64 7.2.2 #2 Calciner I.D. Fan Outlet (West) 84 7.2.3 #2 Calciner ESP Outlet (East) 105 7.2.4 #2 Calciner ESP Outlet (West) 108 7.2.5 #2 Calciner Stack Ill 7.3 Chloride Process Field Data 119 7.3.1 #312 Spray Dryer Baghouse Inlet 120 7.3.2 #312 Spray Dryer Baghouse Outlet 146 7.3.3 #322 Spray Dryer Baghouse Outlet 167 7.3.4 #312 and #322 Spray Dryers Stack 191 7.3.5 Visible Emissions, Method 9 205 7.4 Sulfate Process #2 Calciner Field Data 213 7.4.1 East I.D. Fan Inlet and Outlet . . . 214 7.4.2 West I.D. Fan Inlet and Outlet 235 7.4.3 #2 Calciner ESP Outlet (East) 255 7.4.4 #2 Calciner ESP Outlet (West) 264 7.4.5 #2 Calciner Stack 273 7.4.6 Visible Emissions . . . 287 7.5 Feed and Product Analytical Data 291 7.6 Sampling and Analytical Procedures 353 7.7 Calibration Data 407 7.8 Test Participants 480 7.9 Testing Protocol and Run/Sample Numbering Cross-Reference 481 ------- List of Tables Number Title Page 1-1 Test Schedule, Planned Vs. Actual 1-3 1-2 Test Log 1-4 Chloride Process 2-1 Particulate Emissions & Concentrations Summary 2-3 2-2 Collection Efficiencies Of Control Devices 2-4 Particulate Tests Summary of Results 2-3 #312 Spray Dryer Baghouse Inlet 2-5 2-4 #312 Spray Dryer Baghouse Outlet 2-6 2-5 #322 Spray Dryer Baghouse Outlet 2-7 2-6 Spray Dryers Stack 2-8 Summary of Particle Sizing Test Results 2-7 #312 Baghouse Inlet 2-9 2-8 #312 Baghouse Outlet 2-11 2-9 #322 Baghouse Outlet 2-13 Summary of Visible Emissions Observations 2-10 Spray Dryers Stack 2-15 2-11 Spray Dryers Stack 2-16 2-12 Spray Dryers Stack 2-17 Sulfate Process 2-13 Particulate Emissions and Concentrations Summary 2-20 2-14 Collection Efficiencies Of Control Devices 2-21 Particulate Tests Summary of Results 2-15 #2 Calciner, East I.D. Fan Outlet 2-22 2-16 #2 Calciner, West I.D. Fan Outlet 2-23 2-17 #2 Calciner, East ESP Outlet 2-24 2-18 #2 Calciner, West ESP Outlet 2-25 2-19 #2 Calciner Stack 2-26 ------- vi List of Tables (continued) Number Title Page Summary of Particle Sizing Test Results 2-20 East I.i). Fan Outlet 2-27 2-21 West I.D. Fan Outlet 2-29 Summary of Visible Emissions Observations 2-22 #2 Calciner Stack 2-31 2-23 #2 Calciner Stack 2-32 2-24 #2 Calciner Stack . 2-33 Nitrogen Oxides (as N0ฃ) Testing Summary 2-25 #2 Calciner Stack 2-34 1 Emission Tests Conducted at American Cyanamid Company 3-2 ------- vii List of Figures Number Title Page 1 Simplified Flow Diagram of Chloride Process 3-5 2 Simplified Flow Diagram of Sulfate Process 3-6 3 Flow Diagram for Emission Control System for Spray Dryers 3-7 4 Flow Diagram for Emission Control System for Rotary Calciner 3-9 4-1 Chloride Process and Sampling Points 4-2 4-2 #312 Baghouse Inlet Dimensions 4-3 4-3 #312 Baghouse Outlet Dimensions 4-5 4-4 #322 Baghouse Outlet Dimensions 4-7 4-5 Spray Dryers #312 and #322 Stack Dimensions 4-8 4-6 Sulfate Process and Sampling Points 4-10 4-7 #2 Calciner East and West Side I.D. Fan Outlets Dimensions 4-11 4-8 #2 Calciner East I.D. Fan Inlet Dimensions 4-12 4-9 #2 Calciner West I.D. Fan Inlet Dimensions 4-14 4-10 #2 Calciner East and West ESP Outlet Dimensions 4-15 4-11 #2 Calciner Exhaust Stack Dimensions 4-16 ------- 1-1 1. INTRODUCTION 1.1 Background. The Emission Measurement Branch (EMB) of the U.S. EPA is directing a project designed to generate support data for a possible New Source Performance Standards (NSPS) for calciners and dryers in the mineral industries. Process-related emission factors are being determined from the testing of controlled sources (for the various industries). 1.2 Scope of the Project. EMB is responsible for coordinating the efforts of Entropy to achieve the goals of the testing program. Entropy has been retained under EMB Contract No. 68-02-3852, Work Assignment No. 2 to conduct testing programs at designated industrial facilities. Entropy is to perform emission measurements at the recommended sampling locations, obtain process feed and product samples, and, in conjunction with Research Triangle Institute (RTI), conduct sample analyses as directed by the Industrial Studies Branch of EPA (ISB). As directed by the Industrial Studies Branch of EPA (ISB), Midwest Research Institute (MRI) will monitor process and operating conditions in order to designate suitable testing conditions for the respective processes and to provide a record of process and operational data during the testing. 1.3 American Cyanamld Testing Program. This report covers stationary source sampling performed at the American Cyanamid Company manufacturing plant in Savannah, Georgia on February 9-16, 1984. Bill Trees, Chris Gingrich, and Bill Roberts of American Cyanamid and Dan Bivins of EPA/EMB were present to coordinate the testing. Yogesh N. Doshi and Lynda D. Carney of MRI monitored the plant process and recorded operational data during the testing. 1.3.1 Source Applicability. American Cyanamid operates a titanium dioxide (T102) production facility which is representative of the TiOo pigment industry. The plant uses spray dryers and rotary calciners which are the two most difficult processes within the industry to control. In addition, T102 is believed to have the finest particle size distribution of materials in the industry and, consequently, would represent "worst case" conditions. Spray dryers are used in the chloride process to produce rutile pigment ------- 1-2 (used primarily in paints), while rotary calciners are used in the sulfate process to generate rutile pigment and anatase pigment (used in the paper industries). Emissions from the processes are controlled by two or more types of equipment in series. Settling chambers and baghouses are used primarily for product recovery, while cyclones, wet electrostatic precipitators, and scrubbers provide the additional emission control needed to meet state requirements. 1.3.2 Outline of Testing Program. Emission measurements were performed at the spray dryer system within the chloride process and at the calciner system within the sulfate process. Table 1-1 provides a comparison of the original testing plan and the actual tests performed; the testing program as performed is outlined in Table 1-2, which provides test dates, sampling locations, and test methods. 1.4 Report Organization. Immediately following is the "Summary of Results" section. Appendices 7.1 and 7.2 present the complete results of testing at the chloride and sulfate processes; field data can be found in Appendices 7.3 and 7.4. The two processes are described in the "Process Description and Operation" section, while Appendix 7.5 presents feed and product analytical data. The next section, "Sampling Locations," provides a comprehensive description and illustration for each location; "Sampling and Analytical Procedures" follows, describing the sampling strategy used. Descriptions of the equipment and procedures can be found in Appendix 7.6. The final section, "Quality Assurance," notes the procedures used to ensure the Integrity of the sampling program; Appendix 7.7 provides pertinent calibration data. Appendix 7.8 contains a listing of the Entropy test participants and their roles in the testing program. ------- 1-3 TABLE 1-1 TEST SCHEDULE Planned Vs. Actual Type of Sample Number of Samples Taken Planned Actual Chloride Process Spray Dryers System #312 Spray Dryer Spray Dryer Inlet Settling Chamber Product Outlet Baghouse Product Outlet Baghouse Inlet Baghouse Outlet #322 Spray Dryer Spray Dryer Inlet Baghouse Product Outlet Baghouse Outlet Exhaust Stack feed 3 product 3 product 3 particulate 3 particle size 6 particulate 3 particle size 6 feed 3 product 3 particulate 3 particle size 6 particulate 3 particle size 6 visible emissions 3 4 4 4 4 8 4 4 4 4 4 6 4 0 3 Sulfate Process #2 Calciner System Water Spray Cooler Outlet #2 Rotary Calciner Inlet East ID Fan Inlet East ID Fan Outlet West ID Fan Inlet West ID Fan Outlet East ESP Outlet West ESP Outlet #2 Calciner Exhaust Stack product 3 feed 3 velocity 0 particulate 3 particle size 6 velocity 0 particulate 3 particle size 6 particulate 3 particle size 6 particulate 3 particle size 6 particulate 3 particle size 6 nitrogen oxides 3 visible emissions 3 3 3 2 3 6 2 3 6 3 0 3 0 3 0 3 3 ------- 1-4 TABLE 1-2 TEST LOG CHLORIDE PROCESS Test 1, February 9, 1984 1312 Baghouse Inlet Particulate Particle Size #312 Baghouse Outlet Particulate Particle Size #322 Baghouse Outlet Particulate Particle Size Spray Dryer Stack Particulate Visible Emissions Run Number 1 S-l-A S-l-B S-1-B2* 4 S-4-A S-4-B 11:23 16:40 17:45 15:56 09:35 14:03 16:15 Finish Time 13:31 16:41 17:46 15:57 11:44 15:12 17:00 7** S-7-A S-7-B 09:35 15:45 15:21 10:58 15:46 15:22 10 10 09:40 09:35 11:46 11:35 Test 2, February 11, 1984 #312 Baghouse Inlet Particulate Particle Size #312 Baghouse Outlet Particulate Particle Size #322 Baghouse Outlet Particulate Particle Size Spray Dryer Stack Particulate Visible Emissions 2 S-2-A S-2-B 5 S-5 8 S-8-A S-8-B 11 11 09:05 12:40 13:19 09:05 09:30 09:00 10:50 11:55 09:00 09:02 10:40 12:41 13:20 12:26 13:00 10:08 10:51 11:56 12:31 11:02 * S-l-B was overloaded; S-1-B2 was performed on February 13 for replacement ** Run 7 consists of component runs 7A & 7B; refer to summary of results for details ------- 1-5 TABLE 1-2 (continued) TEST LOG - - CHLORIDE PROCESS - - Test 3, February 11, 1984 #312 Baghouse Inlet Particulate Particle Size #312 Baghouse Outlet Particulate Particle Size Particle Size QC //322 Baghouse Outlet Particulate Particle Size Spray Dryer Stack Particulate Visible Emissions Run Number 3 S-3-A* S-3-A2* S-3-B 6 S-6** Bl, Rl*** 9 S-9-A** S-9-B 12 12 Start Time 13:54 16:22 14:52 16:49 14:02 14:12 14:45 13:51 15:44 16:10 14:00 14:00 Finish Time 15:14 16:23 14:53 16:50 16:14 17:19 15:45 14:58 15:45 16:11 16:10 14:10 Test 4, February 16, 1984 #312 Baghouse Inlet Particulate #312 Baghouse Outlet Particulate #322 Baghouse Outlet Particulate Spray Dryer Stack Particulate Visible Emissions 28 09:45 11:47 29 09:45 11:49 30 09:46 10:52 31 09:50 12:02 31 10:05 12:06 * S-3-A was overloaded; S-3-A2 was performed on February 13 for replacement. ** S-6 catch weights were negligible; S-9-A catch was overloaded; neither run is tabulated in the results. *** Quality Control Reactivity Run Rl and Blank Run Bl performed February 13. (continued next page) ------- 1-6 TABLE 1-2 (continued) TEST LOG SULFATE PROCESS Test 1, February 14, 1984 Run Start Finish Number Time Time 92 Calciner East I.D. Fan Outlet Particulate 13 15:55 17:04 Particle Size S-13-A* 18:01 18:06 S-13-B 18:37 18:42 #2 Calciner West I.D. Fan Outlet Particulate 16 15:55 16:39 Particle Size S-16-A 18:34 18:39 S-16-B 19:00 19:05 #2 Calciner East ESP Outlet Particulate 19 15:50 16:58 #2 Calciner West ESP Outlet Particulate 22 15:50 16:54 92 Calciner Stack Particulate 25 15:54 17:00 Visible Emissions 25 15:49 16:49 Nitrogen Oxides 25 A-D 15:56 16:56 Test 2, February 15, 1984 #2 Calciner East I.D. Fan Outlet Particulate 14 09:35 12:04 Particle Size S-14-A 16:14 16:29 S-14-B 17:00 17:15 #2 Calciner East I.D. Fan Inlet Velocity Traverse V-14 13:05 13:45 #2 Calciner West I.D. Fan Outlet Particulate 17 11:15 12:00 Particle Size S-17-A 16:00 16:15 S-17-B 16:55 17:20 $2 Calciner West I.D. Fan Inlet Velocity Traverse V-17 12:30 13:00 * S-13-A was overloaded; therefore no results were tabulated. (continued next page) ------- 1-7 TABLE 1-2 (continued) TEST LOG SULFATE PROCESS Test 2, February 15, 1984 Run Start Finish Number Time Time #2 Calciner East ESP Outlet Participate 20 09:40 10:48 #2 Calciner West ESP Outlet Particulate 23 09:39 10:42 #2 Calciner Stack Particulate 26 09:39 10:56 Visible Emissions 26 09:35 10:35 Nitrogen Oxides 26 A-D 09:41 10:45 Test 3, February 15, 1984 //2 Calciner East I.D. Fan Outlet Particulate 15 14:13 14:50 Particle Size S-15-A 17:40 17:55 S-15-B 18:25 18:40 #2 Calciner East I.D. Fan Inlet Velocity Traverse V-15 16:00 16:30 #2 Calciner West I.D. Fan Outlet Particulate 18 14:14 15:15 Particle Size S-18-A 17:51 18:16 S-18-B 18:40 19:05 #2 Calciner West I.D. Fan Inlet Velocity Traverse V-18 16:40 17:15 #2 Calciner East ESP Outlet Particulate 21 14:15 15:33 #2 Calciner West ESP Outlet Particulate 24 14:14 16:22 #2 Calciner Stack Particulate 27 14:17 15:34 Visible Emission 27 14:16 15:16 Nitrogen Oxides 27 A-D 14:20 15:22 ------- 2-1 2. SUMMARY AND DISCUSSION OF RESULTS 2.1 Introduction. The testing of the two TiOฃ production systems are treated as two distinct sets of data. Chloride process-spray dryers system test results are discussed in Section 2.2, while the sulfate process- it 2 calciner system testing is discussed in Section 2.3. 2.2 Chloride Process. A summary of the parciculate emissions and concentrations at the chloride process sampling locations is presented in Table 2-1; efficiencies of the control devices are summarized in Table 2-2. Run-by-run data summaries of the particulate testing are provided by location in Tables 2-3 to 2-6; particle sizing data is tabulated in Tables 2-7 to 2-9. The average plume opacity was 9% (results for tests 1, 2, and 4 were 6%, 15%, and 5%, respectively); refer to Tables 2-10 to 2-12 for the tabulated results. 2.2.1 General. The results presented in Table 2-2 are reasonably consistent considering the nature of the process and the control equipment. Some of the variability in the data is probably due to variations in the production loads on the two spray dryers. It is recommended that the production data presented in Section 3 be reviewed in conjunction with the test results. The original test plan scheduled three test sets. However, a fourth test was performed because the production load during the first test set was slightly below the minimum desired load. Only particulate and opacity measurements were taken during the fourth test set; no particle size tests were performed. Because initial inspection of the test site revealed that there were no fugitive emissions, EMB and Entropy made a joint decision to cancel the scheduled Method 22 observations. When comparing flue gas flow rates between locations, it is important to note the increase in excess air due to leakage through the system. Due to leakage of excess air into the system, the flow rates increase significantly as the flue gases approach the stack. 2.2.2 #312 Baghouse Inlet. At the #312 Baghouse Inlet, each 24-minute test was performed such that the 24 minutes were distributed over the 120 minute outlet sampling period. The efficiency calculation therefore assumes ------- 2-2 that the 24-minute inlet tests are representative of the 120 minute testing Interval. The same Is true of the efficiency data presented for the Peterson Scrubber, I.e., the tests at the Spray Dryers Stack and at the #312 Baghouse Outlet lasted 120 minutes, whereas the tests at the #322 Baghouse outlet lasted 60 minutes. The original test plan scheduled three sets of particle size runs (three runs per set) at each location. During the sampling at the #312 Baghouse Inlet, It was observed that runs S-l-B and S-3-A were overloaded. Two additional runs, S-1-B2 and S-3-A2, were performed as replacements two days after the completion of the third test set. 2.2.3 #312 Baghouse Outlet. At the #312 Baghouse Outlet, four particle size runs were performed* Very small quantities of particulate were captured in the impactor during those runs because the flue gas particulate concentration was low; the catch for particle size run S-6 was negligible and is not tabulated at all in the results. Due to the limited catch and time constraints imposed by the plant and process operations, it appeared impractical, if not impossible, to secure a catch which would satisfy EMB requirements. Therefore, a joint decision was made by EMB and Entropy to discontinue particle size testing at this location. 2.2.4 #322 Baghouse Outlet. Due to the heavy particulate loading encountered at this location during Test 1, particulate run 7 was divided into two components which were performed, processed, and analyzed as two separate runs. Component run 7A was performed on 25% of the duct cross section (one port), while component run 7B was performed on 75% of the cross section (three ports); an equivalent run 7 was calculated from component data using appropriate weighting parameters for averaging selected parameters, particulate concentrations, etc. Since only the sampled duct areas of each component run are used in the emission rates and air flow rates calculations, the sum of component runs 7A and 7B represents the emissions and flows of the total cross section. Six particle size runs were performed at the #322 Baghouse Outlet; however, run S-9-A was overloaded and is not tabulated. 2.2.5 Spray Dryers Stack. No particle size runs were performed in the ------- 2-3 TABLE 2-1 PARTIGULATE EMISSIONS & CONCENTRATIONS SUMMARY Chloride Process Test Set 2 3 Emission Rates, Ib/hr: #312 Spray Dryer Baghouse Inlet, Runs 1-3 & 28 Outlet, Runs 4-6 & 29 #322 Spray Dryer Baghouse Outlet, Runs 7Eq-9 & 30 Spray Dryer Stack Runs 10-12 & 31 1,412 1,818 2,041 2,024 0.22 0.11 0.79 0.89 507.5 506.5 480.3 357.2 8.06 8.11 8.87 5.26 Average 1,824 0.50 462.9 7.58 Concentration, Gr/DSCF: #312 Spray Dryer Baghouse Inlet, Runs 1-3 & 28 Outlet, Runs 4-6 & 29 #322 Spray Dryer Baghouse Outlet, Runs 7Eq-9 & 30 Spray Dryer Stack Runs 10-12 & 31 20.7 0.0024 24.7 0.0011 28.1 0.0077 28.8 0.0091 4.19 4.09 3.86 2.91 0.023 0.027 0.029 0.020 25.6 0.0051 3.76 0.025 Emission Rates, kg/hr; #312 Spray Dryer Baghouse Inlet, Runs 1-3 & 28 Outlet, Runs 4-6 & 29 #322 Spray Dryer Baghouse Outlet, Runs 7Eq-9 & 30 Spray Dryer Stack Runs 10-12 & 31 640.7 824.6 925.7 918.1 827.3 0.10 0.052 0.36 0.40 0.23 230.3 229.8 217.8 162.0 210.0 3.65 3.68 4.02 2.38 3.43 Concentration, mg/DSCM; #312 Spray Dryer Baghouse Inlet, Runs 1-3 & 28 Outlet, Runs 4-6 & 29 #322 Spray Dryer Baghouse Outlet, Runs 7Eq-9 & 30 Spray Dryer Stack Runs 10-12 & 31 47,336 56,437 64,202 65,855 58,458 5.59 2.54 17.7 20.7 11.63 9,583 9,350 8,822 6,662 8,604 53.1 60.7 67.0 45.6 56.6 ------- 2-4 TABLE 2-2 COLLECTION EFFICIENCIES OF CONTROL DEVICES Chloride Process 1 2 3 4 Average //312 Spray Dryer Baghouse Emissions Elate, Ib/hr Inlet 1,412 1,818 2,041 2,024 1,824 Outlet 0.22 0.11 0.79 0.89 0.50 Collection Efficency, 99.98 99.99 99.96 99.96 99.97 Percent Peterson Scrubber Emissions Rate, Ib/hr Inlet* 507.7 506.6 481.1 358.1 463.4 Outlet 8.06 8.11 8.87 5.26 7.58 Collection Efficiency, 98.41 98.40 98.16 98.53 98.36 Percent * "Inlet" emissions are the sum of the #312 and #322 Baghouse Outlet emissions rates; "Outlet" emissions are those measured at the Spray Dryer Stack. ------- 2-5 TABLE 2-3 PARTICULATE TESTS SUMMARY OF RESULTS Chloride Process #312 Spray Dryer Baghouse Inlet 28 Run Date 02/09/84 02/11/84 02/11/84 02/16/84 Test Train Parameters; Volume of Dry Gas 16.345 11.408 10.849 10.469 Sampled, SCF* Percent Isokinetic 96.2 106.7 102.9 103.8 Stack Parameters; Temperature, Deg. F 298 299 299 302 Air Flow Rates SCFM*, Dry 7,966 8,599 8,485 8,205 ACFM, Wet 14,342 15,938 15,846 15,403 Method 5 Test Results; Catch, Milligrams 21,911.2 18,233.2 19,725.8 19,524.9 Concentration, Grains Per DSCF* 20.69 24.67 28.06 28.78 Milligrams Per DSCM 47,336 56,437 64,202 65,855 Emission Rate, Pounds Per Hour 1,412.5 1,818.0 2,040.8 2,024.1 Kilograms Per Hour 640.7 824.6 925.7 918.1 * 68 Deg. F. - 29.92 in. Hg. ------- 2-6 TABLE 2-4 PARTICULATE TESTS SUMMARY OF RESULTS Chloride Process #312 Spray Dryer Baghouse Outlet 29 Run Date Test Train Parameters: Volume of Dry Gas Sampled, SCF* Percent Isokinetic Stack Parameters: Temperature, Deg. F Air Flow Rates SCFM*, Dry ACFM, Wet Method 5 Test Results: Catch, Milligrams Concentration, Grains Per DSCF* Milligrams Per DSCM Emission Rate, Pounds Per Hour Kilograms Per Hour 02/09/84 83.379 106.7 260 10,711 17,985 13.2 0.0024 5.59 0.22 0.10 02/11/84 95.903 109.4 269 12,017 20,286 6.9 0.0011 2.54 0.11 0.052 02/11/84 96.103 110.4 271 11,936 20,282 48.2 0.0079 17.7 0.79 0.36 02/16/84 82.161 97.9 270 11,504 19,089 48.2 0.0091 20.7 0.89 0.40 * 68 Deg. F. - 29.92 in. Hg. ------- 2-7 TABLE 2-5 PARTICULATE TESTS SUMMARY OF RESULTS Chloride Process #322 Spray Dryer Baghouse Outlet Run Date Test Train Parameters; Volume of Dry Gas Sampled, SCF* Percent Isoklnetic Stack Parameters; Temperature, Deg. F Air Flow Rates SCFM*, Dry ACFM, Wet Method 5 Test Results; Catch, Milligrams Concentration, Grains Per DSCF* Milligrams Per DSCM Emission Rate, Pounds Per Hour Kilograms Per Hour 7Eq 8 106. 2060) 103.8 218 95.3 218 30 02/09/84 02/11/84 02/11/84 02/16/84 23.327(D 23.346 21.521 23.182 104.2 222 14,140(1) 14,462 14,532 14,311 21,848(1) 22,971 22,199 21,971 NA 6,181.6 5,376.9 4,373.7 4.19(3) 4.09 3.86 2.91 9,583(3) 9,350 8,822 6,662 507.5(1) 506.5 480.3 357.2 230.3(1) 229.8 217.8 162.0 * 68 Deg. F. - 29.92 in. Hg. (D Sum of 7A and 7B (2) Average of 7A and 7B (3) Average weighted by flow rate (7A & 7B) ------- 2-8 TABLE 2-6 PARTICULATE TESTS SUMMARY OF RESULTS Chloride Process Spray Dryers Stack 10 11 12 31 Run Date Test Train Parameters: Volume of Dry Gas Sampled, SCF* Percent Isokinetic Stack Parameters: Temperature, Deg. F Air Flow Rates SCFM*. Dry ACFM, Wet Method 5 Test Results: Catch, Milligrams Concentration, Grains Per DSCF* Milligrams Per DSCM Emission Rate, Pounds Per Hour Kilograms Per Hour 02/09/84 115.727 106.8 124 40,507 . 51,013 174.0 0.023 53.1 8.1 3.65 02/11/84 95.630 100.3 136 35,636 47,515 164.5 0.027 60.7 8.1 3.68 02/11/84 96.121 101.8 124 35,317 44,659 182.5 0.029 67.0 8.9 4.02 02/16/84 - 86.013 105.6 135 30,773 41,778 111.1 0.020 45.6 5.3 2.38 * 68 Deg. F. - 29.92 in. Hg. ------- 2-9 TABLE 2-7 SUMMARY OF PARTICLE SIZING TEST RESULTS #312 Baghouse Inlet SAMPLING DATA Dace Stare Time Finish Time Total Run Time, minutes Impactor Flow Rate (1pm) Isokinetic Ratio (%) STACK DATA Temperature (ฐC) Moisture (Z) Velocity (m/mln) EMISSION DATA Concentration (mg/dsm3) Percent Recovery (PS cone./ M-5 cone.) Cumulative X Mass less than 10 microns Concentration less than 10 microns: From PS runs, mg/dsrn^ From M-5 runs, mg/dsm^ Emission Rate less than 10 microns (kg/hr, from M-5 runs) PS Run 1* 2/09,13/84 1556, 1640 1557, 1641 2 21.9 106.0 148 21.4 1,238 37,385 79.0 14.57 ins: 5,070 6,897 93.3 PS Run 2* 2/11/84 1240, 1319 1241, 1320 2 24.4 108.7 149 22.2 1,337 20,970 37.2 33.91 7,840 19,138 279.6 PS Run 3* 2/11,13/84 1452, 1649 1452, 1650 2 24.2 107.0 150 22.8 1,355 20,455 31.9 29.65 6,160 19,036 274.5 Average ___ 149 22.1 1,310 26,270 49.4 26.04 6,357 15,024 215.8 PS: Particle Size Run M-5: Method 5 Participate Run *: Represents two component runs, A & B. ------- 2-10 PARTICLE SIZE DISTRIBUTION COMPANY NAME American Cyanamid Company ADDRESS Savannah. Georgia AVERAGE OF RUNS 1. 2. 3 SAMPLING LOCATION #312 Baghouse Inlet DATE(sJ 02/09/84,,02/-11/8VW _ DENSITY = J GM/CM 100 I I o ID K 0) 13 u 30 * 70 5 50 = rtft.. - 30- = 3 : 8: 7; s: I 3 = .'9 ! .8 ' 7 - s { 2 "" ฉ Q \^f G) ฉ (T) (T> ^y ^ < y I T II ^ ^ I '^'^i^1'' I'lTI III1I1ITT lilllllirilll il!l III) III! IIIIIMII ITI I I I IT. 1 I 1 I I I I 2 5 10 IS 20 30 40 50 60 70 80 85 90 95 98 PERCENT OF PARTICLES LESS THAN INDICATED SIZE ------- 2-11 TABLE 2-8 SUMMARY OF PARTICLE SIZING TEST RESULTS #312 Baghouse Outlet SAMPLING DATA PS Run 4* PS Run 5 Average Date Start Time Finish Time Total Run Time, minutes Impactor Flow Rate (1pm) Isokinetic Ratio (Z) STACK DATA Temperature (ฐC) Moisture (%) Velocity (m/min) EMISSION DATA Concentration (mg/dsm^) Percent Recovery (PS cone./ M-5 cone.) Cumulative Z Mass less than 10 microns Concentration less than 10 microns From PS runs, mg/dsm^ From M-5 runs, mg/dsm^ Emission Rate less than 10 2/09/84 1403, 1615 1512, 1700 110 24.1 109.1 127 18.7 585 9.92 177.46** 83.63 8.21 4.67 0.0836 2/11/84 0930 1300 210 25.8 113.6 134 19.1 481 1.24 48.82 95.20 1.18 2.42 0.0495 131 18.9 533 5.58 113.2 89.42 4.70 3.55 0.0666 microns (kg/hr, from M-5 runs) PS: Particle Size Run M-5: Method 5 Particulate Run *: Represents two component runs, A & B **: Excessive preseparator catch ------- 2-12 PARTICLE SIZE DISTRIBUTION COMPANY NAME American Cyanamid Company ADDRESS Savannah,. Georgia SAMPLING LOCATION #312 Baghouse Outlet DATE(s) 02/Q9/84, 02/11/84 AVERAGE OF RUNS. 4, 5 DENSITY = I GM/CM I u s o in K 0) u u 70 - 50 : no - 3O , : f ft 9 : j . 9 = ft _= 7 = A. S 2 z 5 I 0 I (V) *A* 5 Z (=) 0 3 (I VI 0 ^ ^y 10 : ฉ >0 ( >0 7 0 8 0 ( @. IS 9 0 < ฉ 1 1 IS 9 PERCENT OF PARTICLES LESS THAN INDICATED SIZE ------- 2-13 TABLE 2-9 SUMMARY OF PARTICLE SIZING TEST RESULTS #322 Baghouse Outlet SAMPLING DATA Date Start Time Finish Time Total Run Time, minutes Impactor Flow Rate (1pm) Isokinetic Ratio (Z) STACK DATA Temperature (ฐC) Moisture (Z) Velocity (m/min) EMISSION DATA Concentration (mg/dsm^) Percent Recovery (PS cone./ M-5 cone.) Cumulative Z Mass less than 10 microns Concentration less than 10 microns: From PS runs, mg/dsm^ From M-5 runs, mg/dsm3 Emission Rate less than 10 microns (kg/hr, from M-5 runs) PS Run 7* 2/09/84 521, 1545 522, 1546 2 17.9 76.3 99 15.7 1,757 5,020 52.4 66.64 is: 3,270 6,386 153.5 PS Run 8* 2/11/84 1050, 1155 1051, 1156 2 13.7 81.2 104 16.8 1,031 5,860 62.7 63.67 3,650 5,953 146.3 PS Run 9* 2/11/84 1610 1611 1 12.8 93.7 104 13.6 1,017 4,838 54.8 68.76 3,326 6,066 149.8 Average 102 15.4 1,268 5,239 56.6 66.40 3,415 6,135 149.9 PS: Particle Size Run M-5: Method 5 Particulate Run *: Represents two component runs, A & B. ------- 2^14 PARTICLE SIZE DISTRIBUTION COMPANY NAME American Cyanamid Company ADDRESS Savannah,, Georgia _ SAMPLING #322 Baghouse Outlet 027(19784.. 02/11/84 AVERAGE OF RUNS. 1, 8, 9 DENSITY = 1 GM/CM u i o in U N yj u u on . a 70..,,.,.= go...- .. = 40 ^ 30- : 10 93 3 " : 4 = 9 : o a 7 - 2 ..." z a !> I 0 1 r M 5 2 ฉ o : 0 < ) tiiiiin 10 ! (^ V! mi in iO ( ฎ. Illl III! iO 7 ฉ. ) limn 1 1 0 S Illl 0 { 1 1 1 1 15 9 Illl 0 < 1 1 IS 9 PERCENT OF PARTICLES LESS THAN INDICATED SIZE ------- 2-15 TABLE 2-10 AMERICAN CYANAMID COMPANY SUMMARY OF VISIBLE EMISSIONS OBSERVATIONS SPRAY DRYERS STACK Date: 2/09/84 Run Number: 10 Highest 6 Minute Average Opacity, Z: 7.50 Highest Single Opacity Reading, Z: 10 Set No. 1 2 3 4 5 6 7 8 9 10 Time Start 0935 0941 0947 0953 0959 1005 1011 1017 1023 1029 End 0941 0947 0953 0959 1005 1011 1017 1023 1029 1035 Avg. % Opacity 5.00 5.21 5.63 5.00 5.42 5.21 4.58 6.04 6.67 5.63 Set No. 11 12 13 14 15 16 17 18 19 20 Time Start 1035 1041 1047 1053 1059 1105 1111 1117 1123 1129 End 1041 1047 1053 1059 1105 1111 1117 1123 1129 1135 Avg. % Opacity 5.00 5.63 6.04 5.21 5.63 4.58 6.67 5.63 7.50 5.00 ------- 2-16 TABLE 2-11 AMERICAN CYANAMID COMPANY SUMMARY OF VISIBLE EMISSIONS OBSERVATIONS SPRAY DRYERS STACK Date: 2/11/84 Run Number: 11 Highest 6 Minute Average Opacity, %: 19.4 Highest Single Opacity Reading, %: 25 Set No. 1 2 3 4 5 6 7 8 9 10 Time Start 0902 0908 0914 0920 0926 0932 0938 0944 0950 0956 End 0908 0914 0920 0926 0932 0938 0944 0950 0956 1002 Avg. % Opacity 12.3 12.3 13.3 16.7 14.8 17.9 18.3 19.4 19.4 17.1 Set No. 11 12 13 14 15 16 17 18 19 20 Time Start 1002 1008 1014 1020 1026 1032 1038 1044 1050 1056 End 1008 1014 1020 1026 1032 1038 1044 1050 1056 1062 Avg. % Opacity 16.9 14.8 15.2 15.0 14.0 12.9 14.2 12.5 11.9 13.5 ------- 2-17 TABLE 2-12 AMERICAN CYANAMID COMPANY SUMMARY OF VISIBLE EMISSIONS OBSERVATIONS SPRAY DRYERS STACK Date: 2/16/84 Run Number: 31 Highest 6 Minute Average Opacity, %: 6.46 Highest Single Opacity Reading, %: 15 Set No. 1 2 3 4 5 6 7 8 9 10 Time Start 1005 1011 1017 1023 1029 1035 1041 1047 1053 1059 End 1011 1017 1023 1029 1035 1041 1047 1053 1059 1105 Avg. % Opacity 6.46 6.04 10.0 4.17 4.38 1.46 2.08 2.92 5.00 4.17 Set No. 11 12 13 14 15 16 17 18 19 20 Time Start 1105 1111 1117 1123 1129 1135 1141 1147 1153 1159 End 1111 1117 1123 1129 1135 1141 1147 1153 1159 1205 Avg. Z Opacity 5.00 5.00 4.58 4.79 3.75 3.54 3.13 2.92 2.71 3.54 ------- 2-18 Spray Dryers Stack due to the presence of water droplets in the flue gas. Method 9 was not performed because of cloudy weather conditions. 2.3 Sulfate Process. A summary of the particulate emissions and concentrations at the sulfate process sampling locations is presented in Table 2-13; efficiencies of the control devices are summarized in Table 2-14. Run-by-run data summaries of the particulate and sulfate testing are provided by location in Tables 2-15 to 2-19; particle sizing data is tabulated in Tables 2-20 and 2-21. Nitrogen oxides as NC>2 concentrations at the #2 Calciner Stack, although essentially zero, averaged 2.3 ppm dry for the three runs. Nitrogen oxides results for each run are included in Table 2-21. Average plume opacity readings during the three tests were zero; refer to Appendix 7.4.6 for the field data. \ 2.3.1 General. As shown in Table 2-13 there is some variability in the test results from one test set to the next. Uncontrolled variables which could have affected the testing and influenced the test results include changes in the process operations during the testing, fluctuations in the performance of the control equipment, and particulate and gas flow pattern oscillations resulting from the lack of straight run at the sampling locations (only the stack had enough straight run to satisfy Method 1 requirements). Due to the potential for variability, the average results of the three runs at a given location is more reliable and should be used wherever possible. When comparing flue gas flow rates between locations, it is important to note the increase in excess air due to leakage through the system. There is, in fact, an ambient air vent between the precipitator outlets and the scrubber which is designed to allow excess air into the gas stream. Due to the introduction of excess air into the system, the flow rates increase significantly as the flue gases approach the stack. Plans to perform Method 22 were abandoned when initial observation revealed that emissions were steam rather than product. Consequently, no Method 22 results are presented. 2.3.2 East and West I.D. Fan Outlets. At both the East and West I.D. Fan Outlets, extremely poor flue gas flow patterns were encountered. Of the 24 points in each duct, 12 showed a positive flow, and 12 showed a ------- 2-19 negative flow. For this reason, after the first test set (runs 13 and 16), additional flue gas velocities and flow rates were measured upstream of the 1.0. fans (East and West I.D. Fan Inlets) at locations which provided more stable flow patterns; the flow rates measured upstream of the fans were used to calculate the particulate emissions rate. The participate concentrations were still measured at the I.D. Fan Outlets by sampling only the positive flow points. The decision to continue sampling at the I.D. fan outlets was justified by assuming that the majority of the particles were less than ten microns in size and that the minute particles would tend to behave like gases, minimizing the importance of isoklnetics and stable flow patterns. Particle size distribution data from these locations does indicate mass median diameters of less than ten microns. Six particle size runs were performed at each of the I.D. Fan Outlets. Run S-13-A, performed on the East Side, was underloaded and therefore was not presented in the summary of results section. All six particle size runs performed at the West Side I.D. Fan Outlet are presented. 2.3.3 East and West ESP Outlets. No major problems were encountered at the ESP outlets although the flow patterns were somewhat erratic. Particle sizing was not performed at the ESP outlets because of the presence of water droplets in the flue gas. Method 3 was not performed for particulate runs 19 and 22 at the East and West ESP outlets, respectively. Flue gas composition data from subsequent runs at the respective locations was used for calculation purposes: data from run 20 was used for run 19, while data from run 23 was used for run 22. 2.3.4 #2 Calciner Exhaust Stack. Particle sizing was not performed at the #2 Calciner Exhaust Stack because of the presence of water droplets in the flue gas. 2.3.5 #2 Calciner Product Outlet. The performance of Method 22 was abandoned when the observers determined that the fugitive emissions were steam rather than product. ------- 2-20 TABLE 2-13 PARTICIPATE EMISSIONS & CONCENTRATIONS SUMMARY Sulfate Process Emission Rates, Ib/hr; #2 Calciner Stack Runs 25-27 Test Set 1 2 Average I.D. Fan Outlet East, Runs 13-15 West, Runs 16-18 ESP Outlet East, Runs 19-21 West, Runs 22-24 #2 Calciner Stack Runs 25-27 Emission Rates, kg/hi: I.D. Fan Outlet East, Runs 13-15 West, Runs 16-18 ESP Outlet East, Runs 19-21 West, Runs 22-24 #2 Calciner Stack Runs 25-27 Concentration, Gr/DSCF: I.D. Fan Outlet East, Runs 13-15 West, Runs 16-18 ESP Outlet East, Runs 19-21 West, Runs 22-24 #2 Calciner Stack Runs 25-27 Concentration, mg/DSCM: I.D. Fan Outlet East, Runs 13-15 West, Runs 16-18 ESP Outlet East, Runs 19-2.1 West, Runs 22-24 181.2 98.5 4.80 3.82 2.13 146.7 33.2 2.18 1.73 0.87 1.956 1.504 0.0411 0.0402 0.0057 4,474.5 3,440.2 94.1 92.0 283.8 113.1 9.42 3.73 0.43 239.6 33.7 4.27 1.69 0.19 2.989 1.810 0.0739 0.0405 0.0011 6,839.8 4,141.9 169.0 92.7 270.4 144.7 4.28 4.20 1.01 206.2 39.1 1.94 1.90 0.46 2.993 2.112 0.0451 0.0448 0.0026 6,847.7 4,832.7 103.1 102.5 245.1 118.8 6.17 3.92 1.19 197.5 35.3 2.80 1.77 0.51 2.646 1.809 0.0534 0.0418 0.0031 6,720.6 4,138.3 122.1 95.7 0.87 0.19 0.46 0.51 ------- 2-21 TABLE 2-14 COLLECTION EFFICIENCIES OF CONTROL DEVICES Sulfate Process Test Set 1 2 3 Average Peterson Scrubber Emissions Rate, Ib/hr Inlet* 8.62 13.15 8.48 10.08 Stack 2.13 0.43 1.01 1.19 Collection Efficiency, 75.29 96.73 88.09 86.7 Percent "Inlet" emissions are the sum of the East and West ESP Outlet emissions; "Stack" emissions are .the #2 Calciner Stack emissions. ------- 2-22 \ TABLE 2-15 PARTICOLATE TESTS SUMMARY OF RESULTS Sulfate Process //2 Calciner, East I.D. Fan Outlet 13 14 15 Run Date Test Train Parameters; Volume of Dry Gas Sampled, SCF* Percent Isokinetic Stack Parameters; Temperature, Deg. F Air Flow Rates** SCFM*, Dry ACFM, Wet Method 5 Test Results; Catch, Milligrams Concentration, Grains Per DSCF* Milligrams Per DSCM Emission Rate, Pounds Per Hour Kilograms Per Hour 02/14/84 02/14/84 02/14/84 19.512 95.7 603 10,809 30,684 2,472.5 181.2 146.7 20.785 95.4 598 11,078 31,517 4,026.1 283.8 139.6 11.396 87.4 560 10,539 29,850 2,210.0 1.956 2.989 2.993 4,474.5 6,839.8 6,847.7 270.4 206.2 * 68 Deg. F. - 29.92 in. Hg. ** Air flow rates are taken from velocity traverses performed at the #2 Calciner East I.D. Fan Inlet after Run 14 and Run 15; the average of the air flows from Run 14 and Run 15 were used for Run 13. ------- 2-23 TABLE 2-16 PARTICULATE TESTS SUMMARY OF RESULTS Sulfate Process ฃ2 Calciner, West I.D. Fan Outlet 16 17 18 Run Date Test Train Parameters; Volume of Dry Gas Sampled, SCF* Percent Isokinetic Stack Parameters; Temperature, Deg. F Air Flow Rates** SCFM*, Dry ACFM, Wet Method 5 Test Results; Catch, Milligrams Concentration, Grains Per DSCF* Milligrams Per DSCM Emission Rate, Pounds Per Hour Kilograms Per Hour 02/14/84 02/15/84 02/15/84 14.415 93.1 523 1,404.4 98.5 33.2 12.470 95.5 480 1,462.7 113.1 33.7 12.748 98.2 482 7,641 20,219 7,289 19,295 7,992 21,143 1,744.7 1.504 1.810 2.112 3,440.2 4,141.9 4,832.7 144.7 39.1 * 68 Deg. F. - 29.92 in. Hg. ** Air flow rates are taken from velocity traverses performed at the #2 Calciner West I.D. Fan Inlet after Run 17 and Run 18; the average of the air flows from Run 17 and Run 18 were used for Run 16. ------- 2-24 TABLE 2-17 PARTIGULATE TESTS SUMMARY OF RESULTS Sulfate Process #2 Calciner, East ESP Outlet Run Date Test Train Parameters; Volume of Dry Gas Sampled, SCF* Percent Isoklnetlc Stack Parameters; Temperature, Deg. F Air Flow Rates 19 20 39.407 100.4 150 44.150 103.0 150 21 02/14/84 02/15/84 02/15/84 32.909 103.0 148 SCFM*, Dry ACFM, Wet Method 5 Test Results: Catch, Milligrams Concentration, Grains Per DSCF* Milligrams Per DSCM Emission Rate, Pounds Per Hour Kilograms Per Hour 13,623 20,282 105.0 0.0411 94.1 4.80 2.18 14,873 22,934 211.3 0.0739 169.0 9.42 4.27 11,081 16,742 96.1 0.0451 103.1 4.28 1.94 * 68 Deg. F. - 29.92 in. Hg. ------- 2-25 TABLE 2-18 PARTICULATE TESTS SUMMARY OP RESULTS Sulfate Process #2 Calciner, West ESP Outlet Run Date Test Train Parameters; Volume of Dry Gas Sampled, SCF* Percent Isokinetic Stack Parameters; Temperature, Deg. F Air Flow Rates 22 23 53.241 99.2 137 52.246 100.4 131 24 02/14/84 02/15/84 02/15/84 52.063 98.3 130 SCFM*, Dry ACFM, Wet Method 5 Test Results: Catch, Milligrams Concentration, Grains Per DSCF* Milligrams Per DSCM Emission Rate, Pounds Per Hour Kilograms Per Hour 11,071 14,949 138.7 0.0402 92.0 3.82 1.73 10,740 14,200 137.1 0.0405 92.7 3.73 1.69 10,932 14,362 151.1 0.0448 102.5 4.20 1.90 * 68 Deg. F. - 29.92 in. Hg, ------- 2-26 TABLE 2-19 PARTICULATE TESTS SUMMARY OF RESULTS Sulfate Process #2 Calciner Stack 25 Run Date 02/14/84 Test Train Parameters; Volume of Dry Gas 71.033 Sampled, SCF* Percent Isokinetic 105.4 Stack Parameters; Temperature,, Deg. F 132 Air Flow Rates SCFM*, Dry 43,650 ACFM, Wet 55,030 Method 5 Test Results; Catch, Milligrams 26.2 Concentration, Grains Per DSCF* Milligrams Per DSCM Emission Rate, Pounds Per Hour Kilograms Pe:r Hour Total Sulfates as H2S04; Catch, Micrograms 5,121 Concentration, Grains Per DSCF* 0.00111 Milligrams Per DSCM 2.55 Emission Rate, Pounds Peir E!our 0.416 Kilograms Per Hour 0.189 * 68 Deg. F. - 29.9.2 in. Hg. 26 02/14/84 91.275 108.7 128 43,421 55,066 6.8 6,248 0.0011 2.41 0.393 0.178 27 02/14/84 91.218 105.5 132 44,748 55,426 15.6 0.0057 11.7 2.13 0.87 0.0011 2.63 0.43 0.19 0.0026 6.04 1.01 0.46 4,902 0.000829 1.90 0.318 0.144 ------- 2-27 TABLE 2-20 SUMMARY OF PARTICLE SIZING TEST RESULTS East I.D. Fan Outlet SAMPLING DATA Date Start Time Finish Time Total Run Time, minutes Impactor Flow Rate (1pm) Isokinetic Ratio (Z) STACK DATA Temperature (ฐC) Moisture (Z) Velocity (m/min) EMISSION DATA Concentration (mg/dsm^) Percent Recovery (PS cone./ M-5 cone.) Cumulative Z Mass less than 10 microns Concentration less than 10 microns: From PS runs, mg/dsm^ From M-5 runs, mg/dsm^ Emission Rate less than 10 microns (kg/hr, from M-5 runs) PS: Particle Size Run M-5: Method 5 Particulate Run *: Represents two component runs, A & B. PS Run 13 2/14/84 1837 1842 5 20.5 97.6 319 22.2 1,293 952.1 21.3 55.46 is: 528.9 2,482 81.4 PS Run 14* 2/15/84 1614, 1700 1629, 1715 30 21.5 97.2 311 24.2 1,017 1,060 15.5 57.64 553.0 3,943 80.5 PS Run 15* 2/15/84 1740, 1825 1755, 1840 30 20.9 94.3 312 23.3 1,015 1,795 26.2 80.08 1,440 5,484 165.1 Average 314 23.2 1,108 1,269 21.0 64.39 840.6 3,970 109.0 ------- 2-28 PARTICLE SIZE DISTRIBUTION COMPANY NAME _ American Cyanamid Company ADDRESS Savannah, Georgia _ SAMPLING LQgATioisi #2 Calciner East I. 'P. Fan Outlet PATE(S> 02/14/84, 02/15/84 _ AVERAGE OF RUNS. , 14, 15 DENSITY = I CM/CM ง 8 u o in 3 (0 u u 70.,.. = 50.. ' 1 I o 5 " 3s A " 9 a a ... a 7 5 3 2 . I (1 V- ฎ (7\ vi' ฉ ^ V G) \*) c \l I I I I I I I I I I I I I ' 5 10 15 20 30 40 50 60 70 80 85 90 95 98 PERCENT OF PARTICLES LESS THAN INDICATED SIZE ------- 2-29 TABLE 2-21 SUMMARY OF PARTICLE SIZING TEST RESULTS West I.D. Fan Outlet SAMPLING DATA Date Start Time Finish Time Total Run Time, minutes Impactor Flow Rate (1pm) Isokinetic Ratio (Z) STACK DATA Temperature (ฐC) Moisture (Z) Velocity (m/min) EMISSION DATA Concentration (mg/dsm^) Percent Recovery (PS cone./ M-5 cone.) Cumulative Z Mass less than 10 microns Concentration less than 10 microns: From PS runs, mg/dsm^ From M-5 runs, mg/dsm^ Emission Rate less than 10 microns (kg/hr, from M-5 runs) PS: Particle Size Run M-5: Method 5 Particulate Run *: Represents two component runs, A & B. PS Run 16* 2/14/84 1834, 1900 1839, 1905 10 16.8 96.3 273 18.3 279.8 598.1 17.4 60.88 >ns: 370 2,094 20.2 PS Run 17* 2/15/84 1600, 1655 1615, 1720 40 10.6 87.9 260 18.1 246.9 321.5 7.76 72.08 231 2,986 24.3 PS Run 18* 2/15/84 1751, 1840 1816, 1905 50 11.4 94.6 259 20.2 248.7 656.4 13.6 71.29 492 3,445 27.9 Average _ 264 18.9 258.5 525.3 12.9 68.08 364 2,842 24.1 ------- 2-30 PARTICLE SIZE DISTRIBUTION COMPANY NAME American Cyanamid Company ADDRESS Savannah Georgia SAMPLING LOCATION #2 Calclner West I.D. Fan Outlet DATE( s) 02/J4/84. 02/15/84 DENSITY = I GM/CM3 AVERAGE OF RUNS. 16, 17, 18 70- -; 50 -: 40 ' CO * S : o 5 10 " 9 l ~ 9 ! S ! i H g : 5 3 i ฐ 4 ^ 0 : in : Q 3 : H ! u : J o I t 9 = 8 : 7 = 2 .1 ^-' ฉ ฉ P. i) I riii "i"""11 5 10 15 20 30 40 50 60 70 80 85 90 95 98 PERCENT OF PARTICLES LESS THAN INDICATED SIZE ------- 2-31 TABLE 2-22 AMERICAN CYANAMID COMPANY SUMMARY OF VISIBLE EMISSIONS OBSERVATIONS If 2 CALCINER STACK Date: 2/14/84 Run Number: 25 Highest 6 Minute Average Opacity, Z: 0 Highest Single Opacity Reading, %: 0 Set No. 1 2 3 4 5 6 7 8 9 10 Time Start 1549 1555 1601 1607 1613 1619 1625 1631 1637 1643 End 1555 1601 1607 1613 1619 1625 1631 1637 1643 1649 Avg. I Opacity 0 0 0 0 0 0 0 0 0 0 ------- 2-32 TABLE 2-23 AMERICAN CYANAMID COMPANY SUMMARY OF VISIBLE EMISSIONS OBSERVATIONS #2 CALCINER STACK Date: 2/15/84 Run Number: 26 Highest 6 Minute Average Opacity, %: 0 Highest Single Opacity Reading, %: 0 Set No. 1 2 3 4 5 6 7 8 9 10 Time Start 0935 0941 0947 0953 0959 1005 1011 1017 1023 1029 End 0941 0947 0953 0959 1005 1011 1017 1023 1029 1035 Avg. % Opacity 0 0 0 0 0 0 0 0 0 0 ------- 2-33 TABLE 2-24 AMERICAN CYANAMID COMPANY SUMMARY OF VISIBLE EMISSIONS OBSERVATIONS #2 CALCINER STACK Date: 2/15/84 Run Number: 27 Highest 6 Minute Average Opacity, %: 0.42 Highest Single Opacity Reading, %: 5 Set No. 1 2 3 4 5 6 7 8 9 10 Time Start 1416 1422 1428 1434 1440 1446 1452 1458 1504 1510 End 1422 1428 1434 1440 1446 1452 1458 1504 1510 1516 Avg. Z Opacity 0 0 0 0 0 0 0 0 0.42 0 ------- 2-34 TABLE 2-25 NITROGEN OXIDES (AS N02) TESTING SUMMARY Sulfate Process #2 Calciner Stack Run Date Sample Numbers Sampling Period Nitrogen Oxides 1 02/14/84 25A-25D 1556-1656 (as N02) Results: &un numoers 2 02/15/84 26A-26D 0941-1045 3 02/15/84 27A-27D 1420-1522 Concentration, ppm, dry 2.1 1.9 2.9 ------- 3-1 3. PROCESS DESCRIPTION AND OPERATION / 3.1 Introduction. Source emission tests were conducted on Spray Dryer #312, Spray Dryer #322, and Rotary Calciner #2 at the American Cyanamid Company, Savannah, Georgia from February 8 through 16, 1984; Table 1 tabulates the tests performed. The tests were conducted by Entropy Environmentalists, Inc. (Entropy) test crew, headed by Mr. Frank Phoenix. The process was monitored by Mr. Yogesh Doshi and Ms. Lynda Carney of Midwest Research Institute (MRI). Mr. William Trees of American Cyanamid coordinated testing with plant personnel and provided process information. Mr. Dan Blvins of EPA's Emissions Measurement Branch (EMB) was present during testing to observe emission testing procedures. 3.2 Pollutants/Sampling Points. 3.2.1 Spray Dryers. Four tests on Spray Dryer #312 and Spray Dryer #322 were completed at the following locations: 3.2.1.1 Particulate Mass and Particle Size. Particulate mass determinations were performed at the inlet and outlet of the #312 Baghouse, the outlet of the #322 Baghouse, and at the Peterson Scrubber Stack. Particle size determinations were performed at the inlet and outlet of the #312 Baghouse and the outlet of the #322 Baghouse during runs 1,2, and 3. Particle size determinations were not performed at the Peterson Scrubber Stack because of the: large amount of water vapor in the gas stream. Entropy and EMB personnel decided not to perform particle size runs simultaneously with mass runs because of the complexity of the test program. 3.2.1.2 Visible Emissions. Visible emission observations were made at the Peterson Scrubber Exhaust Stack throughout runs 1 and 4. Opacity readings could not be made during runs 2 and 3 because of overcast sky conditions. Because: the spray dryer process inlet and outlet were totally enclosed, no process fugitive emission observations were taken. 3.2.1.3 Feed and Product Samples. Feed samples were collected at the inlets to both spray dryers for particle size and moisture analysis. Product samples from the settling chamber of the #312 Spray Dryer and from the ------- 3-2 TABLE 1. EMISSION TESTS CONDUCTED AT AMERICAN CYANAMID COMPANY Sampling point Test type Test method Spray Dryers No. 312 spray dryer feed inlet No. 312 settling chamber product oulet No. 312 baghouse inlet No. 312 baghouse outlet No. 312 baghouse product outlet No. 322 spray dryer feed inlet No. 322 baghouse outlet No. 322 baghouse product outlet Petersen scrubber exhaust stack Rotary Calciner No. 2 Rotary calciner feed inlet Rotary calciner product outlet East conditioning tower inlet West conditioning tower inlet Moisture content Particle size sieve Moisture content Particle size sieve Particulate concentration Particle size Particulate concentration Particle size Moisture content Particle size sieve Moisture content Particle size sieve Particulate concentration Particle size Moisture content Particle size sieve Visible emissions Particulate concentration Moisture content Particle size sieve Moisture content Particle size sieve Particulate concentrations Particle size Particulate concentration Particle size ASTM-D422 ASTM-02216 ASTM-D422 ASTM-D2216 EPA-5 EPA Draft Method EPA-5 EPA Draft Method ASTM-0422 ASTM-02216 ASTM-0422 ASTM-D2216 EPA-5 EPA Draft Method ASTM-D422 ASTM-02216 EPA-9 EPA-5 ASTM-0422 ASTM-02216 ASTM-D422 ASTM-02216 EPA-5 EPA Draft Method EPA-5 EPA Draft Method (continued) ------- 3-3 TABLE 1. (continued) Sampling point Test type Test method East wet ESP outlet West wet ESP outlet Peterson scrubber exhaust stack Particulate concentration Particulate concentration Visible emissions Particulate concentration Acid mist NO Rotary Direct Dryer' (Chloride.ore dryer) Rotary direct dryer feed inlet Rotary direct dryer outlet Moisture content Particle size sieve Moisture content Particle size sieve Steam-Tube Rotary Dryer (Sulfate ore dryer) Steam-tube rotary dryer feed inlet Steam-tube rotary dryer outlet Tunnel Dryer (Sulfate process) Rotary direct dryer feed inlet Rotary direct dryer outlet Moisture content Particle size sieve Moisture content Particle size sieve Moisture content Particle size sieve Moisture content Particle size sieve EPA-5 EPA-5 EPA-9 EPA-5 EPA-8 EPA-7 ASTM-D422 ASTM-D2216 ASTM-0422 ASTM-02216 ASTM-0422 ASTM-D2216 ASTM-0422 ASTM-D2216 ASTM-0422 ASTM-02216 ASTM-0422 ASTM-02216 Grab samples were not collected because the unit was not operating. American Cyanamid will send the samples by mail when the unit resumes operation. ------- 3-4 product hoppers of Che #312 and #322 Baghouses were also collected for particle size and moisture analysis. 3.2.2 Rotary Calciner No. 2. Tests on Rotary Calciner 92 were completed at the following locations: 3.2.2.1 Participate Mass and Particle Size. Particulate mass and particle size determinations were performed at the inlets to the two conditioning towers. Entropy and EMB personnel decided not to perform particle size runs simultaneously with mass runs because of the complexity of the test program. Only particulate mass determinations were performed at the outlets of the two ESP's and the outlet of the Peterson Scrubber; particle size determinations were not possible because of the large amount of water vapor in the gas stream. Acid mist and NOX tests were conducted at the Peterson Scrubber Exhaust Stack. Feed and product samples were collected for particle size and moisture analysis. 3.2.2.2 Visible Emissions. Visible emission observations were made at the Peterson Scrubber Exhaust Stack for the duration of all three test runs. Because feed to the calclner is In a slurry form and feed discharge point is totally enclosed, visible emission observations were not made. Similarly, visible emission observations were not made at the calciner discharge and because it was totally enclosed. Only steam emissions were noticed from the cooler. 3.3 Process Description. This plant operates continuously, except for breakdowns, 24 hours per day and 7 days per week. Titanium dioxide (T102 pigment is produced by both the chloride process, shown in Figure 1, and the sulfate process, shown in Figure 2. The chloride process uses two spray dryers and one rotary direct dryer, and the sulfate process uses two rotary calclners, two steam-tube rotary dryers, and two tunnel dryers. 3.3.1 Spray Dryers. Figure 3 is a simplified flow diagram that shows the emission control systems for both spray dryers. The two spray dryers are used in the chloride process. Spray Dryer #312 was manufactured by Proctor ------- HIHEHAL (ml lit 1(01 All If UllltCI OIIYEli ()) SCIlEENINti COAIINU Ullll S OXIDES CUKE CI2 till OH I HAM UN SOLIDS AEHOUAL OIL 1 CI2 HttVClt MULING HAU TIO, COULINli AHO SOllttS PRECIPITATION OX I DAI ION Hi IHAIIUN AND UtUATElllMU uiiviii in flUII) EHEIttiY Hiit ma SOUIUH AHIMIHAIL 1 PACKAGING U) I U1 1. Simplified flow diagram of chloride process-- American Cyanamid Company, Savannah, Georgia. ------- TITANIUM ^ SIAG STEAM- TUBE-ORE UK VI It (2) ROTARY CALCINER (2) RAW COOLEttS (2) GRINDING K SALTS. PHOSPHATES. CONDITIONING AGENTS i. CONDITIONING PULVERIZING, MILLING, AND SCREENING STEAM II^SO,, INJECTION OltiESTEK FILTRATION. UASH1NG. AND DEMATERING COATING WITH HYDROUS OXIDES T SODIUM ALUtilNATE FLUCCUEANT .1 CONCEHTKATION 2n Oil Al Oft TI2(SOJ3 LEACHING flETKATlON REAGENTS (SOMETIMES) i NUCLEA PRECIPITATION FILTRATION, WASHING, AND DEUATEIUNG STEAM-TUBE BELT DRYER (2) .V FLUID I-IIERGY MILLING Flyure 2. Simplified flow diayraiu of sulfate urocess-- Aiuerlcan Cyanaiuld Company, Savannah, Georgia. PACKAGING ------- AMBIENT AIR r FEED ' " SPRAY DRYER SETTLING BAGHOUSE 1 AIR NO. 312 CHAMBER * Bftt>mju:>t * - - - > ' V J 1 ! i 1 - - t i i i i PETERSON SCRUBBER - -> \ 1 S T A C K I < FEED AIR SPRAY DRYER NO. 322 BAGIIOUSE 1 ' BY-PASS U) I I PRODUCT PROCESS FLOW AIR FLOW Fiyure 3. Flow diagram for emission control system for spray dryers at American Cyanamid Company, Savannah, Georgia. ------- 3-8 and Schwartz (P&S) and Installed in 1965, and #322 was manufactured by Bowen and installed in 1970. The dryers have separate combustion chambers and are fired by natural gas. The process material is dried by a cocurrent flow of hot air. Material entering the spray dryers is in the form of a slurry. During the tests the dryers were processing futile titanium dioxide. Most of the product from Spray Dryer #312 settles out in a settling chamber. The exhaust gas from the settling chamber then goes to a baghouse. The baghouse collects most of the remaining dried product. All of the product from Spray Dryer #322 is collected in a baghouse. The exhaust gas from both spray dryer baghouses is manifolded to one high energy Peterson Scrubber. There is a fresh air inlet in the Spray Dryer #312 system duct going to the Peterson Scrubber. This duct also contains water sprays to improve the particulate collection efficiency of the Peterson Scrubber. 3.3.2 Rotary Calciner No. 2. A simplified flow diagram that shows the emission control systems for the rotary calciner is shown in Figure 4. Rotary Calciner #2 was manufactured by Vulcan. The calciner has a separate combustion chamber and is fired -by natural gas. The feed material is titanium hydrosylate slurry, which is calcined by a counter-current stream of hot air to form titanium dioxide crystals. Particulate emissions from the calciner are controlled by two conditioning towers (low-energy packed towers) in parallel, two wet ESP's in parallel, and a Peterson Scrubber (high energy scrubber). The primary purpose of the conditioning towers is to keep the wet ESP inlet gas temperature less than 71 degrees Celsius (160 degrees Fahrenheit). The two wet ESP's are used is the primarily for the control of acid mist emissions. The Peterson Scrubber is the secondary control device for particulate emissions and operates at a pressure drop of 5.5 kPA (22 to 30 in. w.c.). 3.4 Process Conditions During Testing 3.4.1 Spray Dryers. The operation of Spray Dryer #312 and Spray Dryer #322 was monitored from a control panel that regulated the feed rates and inlet and outlet air temperatures of the dryers. Fuel consumption for ------- CONDITIONING TOWER WET ESP PRODUCT TO COOLER 4 "AIR *" ROTARY CALCINER / i j ~ " 1 ' i 1=1 FEED CONDITIONING TOWER WET ESP \ PETERSON SCRUBBER S T A C K OJ vo Figure 4. Flow diagram for emission control system for rotary calciner at American Cyanamid Company, Savannah, Georgia. ------- 3-10 both dryers was monitored by natural gas meters. MR I recorded the process data during the spray dryer tests. Air temperature and fuel usage were consistent and Indicated steady state process operations during the test runs. The baghouse compartment pressure drops for Spray Dryer #312 were monitored from a control panel, and pressure drops for the baghouse on Spray Dryer #322 were monitored from outside gauges. The Peterson Scrubber was monitored by reading both the pressure drop across the scrubber and candle column (similar to venturl scrubber throat) and the recirculation pump pressure (only one of two pressure gauges was working). The Peterson Scrubber and baghouse pressure drops were within normal plant operating ranges. Water flow rates and pressure drops were constant. The packaging rates provided by American Cyanamld will not be used as exact production rates, since they are estimates. Exact production rates will be calculated from feed analysis data. Percent capacity utilization will also be calculated. The exact production rates and precent capacity utilization is considered confidential by American Cyanamld. Soon after run 1 was completed, Spray Dryer #322 was shut down to repair a squeaking bearing in the fan. It was found that the feed meter for Spray Dryer #322 was not functioning as the feed meter reading was the same after the dryer stopped operating as it had been during normal operation. Also, the natural gas consumption rate was 20 percent less than that during runs 2 and 3. Because of these observations, it was decided to conduct an additional test run. The problem with the feed meter was corrected prior to test runs 2, 3, and 4. During run 2, the feed mechanism of the #312 Spray Dryer automatically shut down for no apparent reason. At this point, testing was discontinued. Plant personnel started the unit up again in 10 minutes, and within 1 hour, the process achieved a steady state. Testing was then resumed. During run 4, particle sizing was not done because it was decided that the three particle size runs completed earlier were sufficient. 3.4.2 Rotary Calciner No. 2. The calclner parameters that were monitored include time per calciner revolution, fuel consumption, and gas and feed material temperatures at 6 ft., 30 ft., and 85 ft. from the discharge end. ------- 3-11 Feed tank level was measured and recorded by a plant operator. Rotary calciner feed rates, temperatures, revolution rates, and natural gas usage were consistent throughout the test runs, indicating steady state process conditions. The process parameters monitored for the conditioning towers were pressured drop and fresh water make up and recirculation rate. The ESP parameters that were monitored included gas inlet temperatures, primary voltage, and primary and secondary current. The make-up water rate, inlet temperature, pressure drop, and pump pressure were monitored for the Peterson scrubber. Control equipment, including the two conditioning towers, two ESP's, and Peterson scrubber, displayed normal operating parameters. The east conditioning tower was partially plugged, causing an uneven distribution in the volume of exhaust gas coming from the rotary calciner to each of the two conditioning towers. The product quality, uncontrolled emission level, and overall control process were not affected by this uneven distribution. The conditioning towers maintained the inlet gas temperature to the ESP's at less than 71 degrees Celsius (160 degrees Fahrenheit) during all three test runs. During runs 2 and 3, the west conditioning tower flow meter was not functioning properly,. Between runs 2 and 3, the natural gas to the rotary calciner was shut off for approximately 10 minutes because several bricks from the calciner lining plugged the discharge end of the calciner. The problem was immediately corrected, and run 3 was started when the kiln achieved normal operation. Plant processes were operated at or near normal operation capacity during all three calciner test runs and during test runs 2, 3, and 4 of both spray dryers. Process conditions were normal. Collected data are representative of normal process conditions. Because of the broken feed meter on Spray Dryer #322, the data gathered during the first run of the spray dryer test may not be useful. ------- 4-1 4. SAMPLING LOCATIONS 4.1 Applicability of Sampling Sites. The primary goal of the testing program was to characterize emissions from the spray dryer system (chloride process) pollution control equipment and from the calciner system (sulfate process) control equipment. In addition, moisture and sieving analyses were performed on feed and product samples. Sampling sites appropriate to these objectives were approved prior to testing. 4.2 Chloride Process Sampling Locations. Figure 4-1 illustrates schematically the chloride process which incorporates two spray dryer systems, i.e., spray dryers #312 and #322. The location of each sampling site is indicated in Figure 4-1. Each of the sampling locations is individually discussed and illustrated. 4.2.1 #312 Spray Dryer Inlet (Sampling Location A). Grab samples of the feed to the spray dryer were collected during each Method 5 run for moisture content determination. The tacky consistency of the feed made sieve analysis inappropriate. 4.2.2 #312 Settling Chamber Product Outlet (Sampling Location B). Grab samples of the product: from the settling chamber were collected during each Method 5 run for sieve analysis and moisture content determination. 4.2.3 #312 Baghouse Inlet (Sampling Location C). Particulate emissions and particle size distribution determinations were made in the 26-inch diameter horizontal duct accessed through two sampling ports spaced 90 degrees apart. The sampling ports were located 61 inches (i.e., two duct diameters) downstream from the spray dryer settling chamber and 15 inches (i.e., one-half duct diameter) upstream from a 17 degree upward bend in the duct. Figure 4-2 illustrates the inlet sampling location. The original test: plan was to sample 24 points for five minutes each (giving a total test time of 120 minutes), but the high particulate loading in the duct made this plan impractical. EPA EMB and Entropy jointly approved a revised particulate sampling plan in which 12 points (six points on each of two traverse axes labeled A and B) were sampled for two minutes each, ------- I.D. FANS SPRAY DRYER #312 SETTLING CHAMBER C -o- iB 90% PRODUCT SPRAY DRYER #322 o PROCESS FLOW AIR FLOW GRAB SAMPLE SAMPLING LOCATION BAGHOUSE B1 10% PRODUCT I.D. FAN T I PETERSON SCRUBBER i BY-PASS I s T A C K BAGHOUSE I 100% PRODUCT A,B,B',b,b' C,D,E F G ASTM METHOD METHOD 5, IMPACTOR METHOD 5 METHOD 9 FIGURE 4-1. CHLORIDE PROCESS AND SAMPLING POINTS AT AMERICAN CYANAMID, SAVANNAH, GEORGIA ------- TO BAGHOUSE TO BAGHOUSE EXTERIOR WALL 2 AXES, EACH WITH 6 'POINTS (TOTAL 12 POINTS) FROM SPRAY DRYER N AND SETTLING CHAMBER INSIDE BUILDING 26" INSIDE DIAMETER ' ' ' I -Q SECTION N-N 4" FIGURE 4-2. #312 BAGHOUSE INLET DIMENSIONS WITH SAMPLING PORT AND POINT LOCATIONS ------- 4-4 resulting in a total sampling time of 24 minutes. Sampling was periodically interrupted and resumed in order to distribute the 24 minutes of sampling over the two-hour period of particulate sampling at the #312 Baghouse Outlet. Two particle size runs were performed after each of the particulate runs (runs 1,2, and 3) for a total of six particle size runs. For each run, either points A-2 and A-5 or points B-2 and B-5 were sampled; sampling times ranged from 20 seconds to one minute depending on the particulate loading encountered. 4.2.4 #312 Baghouse Product Outlet (Sampling Location B'). Grab samples of the product from the baghouse were collected during each Method 5 run for sieve analysis and moisture content determination. 4.2.5 #312 Baghouse Outlet (Sampling Location D). Sampling was performed in a 48-inch diameter vertical duct accessed through two sampling ports spaced 90 degrees apart. The ports were located 12 inches (0.3 stack diameters) upstream and 42 inches (0.8 stack diameters) downstream from the nearest flow disturbances, as shown in Figure 4-3. A total of 24 sampling points were used for the particulate tests (12 sampling points on each of two traverse axes labeled A and B). Each point: was sampled for five minutes resulting in a total test time of 120 minutes. Four particle size runs were performed. The first two runs (performed after particulate run 4) lasted for 45 and 60 minutes, respectively. A third particle size run lasting 120 minutes was done simultaneous with particulate run 5; the fourth particle size run lasted 176 minutes and was performed simultaneous with particulate run 6. 4.2.6 #322 Spray Dryer Inlet (Sampling Location b). Grab samples of the feed to the spray dryer were collected during each Method 5 run for moisture content determination. The tacky consistency of the feed made sieve analysis inappropriate. 4.2.7 #322 Baghouse Product Outlet (Sampling Location b'). Grab samples of the product from the baghouse were collected during each Method 5 run for sieve analysis and moisture content determination. ------- 4-5 2 AXES, EACH WITH 12 POINTS (TOTAL 24 POINTS) B p 48" DIAMETER SECTION M-M TO PETERSON SCRUBBER 2 SAMPLING PORTS FLANGE BUNION I.D. FAN FIGURE 4-3. #312 BAGHOUSE OUTLET DIMENSIONS WITH SAMPLING PORT AND POINT LOCATIONS ------- 4-6 4.2.8 #322 Baghouse Outlet (Sampling Location E). Sampling was performed in a 50-inch by 21-inch tapered duct positioned approximately 15 degrees from vertical. The duct was accessed through four sampling ports located 100 inches downstream and 42 inches downstream from the nearest bend; due to the taper of the duct, no straight run was available. A total of 24 sampling points were used for the particulate tests, i.e., six sampling points on each of four traverse axes labeled A through D, as shown in Figure 4-4. The original sampling time per point was five minutes; however, after 21.77 minutes of testing in port A during the first run (1.77 minutes into point A-5), the sampling protocol was reevaluated and a joint decision was made to sample the remaining points for two minutes in order to shorten the net run time. The 21.77-minute sample of port A was designated run 7A; the 36-mlnute sample was designated run 7B. For runs 8 and 9, all 24 points were sampled for 2.5 minutes, resulting in a total run time of 60 minutes. Two particle size runs were performed after each of the three particulate runs (runs 7, 8 and 9) for a total of six particle size runs. During each run, a single point (either point A-4 or point C-4) was sampled for 30, 45, or 60 seconds. 4.2.9 #312 and #322 Spray Dryers Exhaust Stack (Sampling Location F). Sampling was performed in a 78-inch diameter vertical stack. Two sampling ports (labeled A and B) spaced 90 degrees apart were located 78 inches (one stack diameter) upstream from the stack outlet and 432 Inches (5.5 stack diameters) downstream from the nearest flow disturbance. A total of 24 sampling points were used for particulate testing (12 points on each of two traverse axes labeled A and B) as shown in Figure 4-5. Each point was sampled for five minutes for a total test time of 120 minutes. 4.2.10 #312 and #322 Spray Dryers Exhaust Stack (Sampling Location G). Plume opacity observations were performed at the exhaust stack according to procedures outlined in EPA Reference Method 9. Cloudy weather conditions prohibited the completion of opacity observations for test 3 (run 12) and limited the observer's confidence in the reliability of test 4 (run 31). ------- 4-7 24 SAMPLING POINTS 4 SAMPLING PORTS ^^ - 1 1 A 1 x _ r i T J~ | * *-- - 1 | B >u i i ~~! ~T ~ 1 . * ป 1 I c _ 4. . . 1 1 ~T " ..4 - ป.- - ป 1 D 1 21 i t 4" 1 SECTION L-L FROM #322 BAGHOUSE TO I.D. FAN FIGURE 4-4. #322 BAGHOUSE OUTLET DIMENSIONS WITH SAMPLING PORT AND POINT LOCATIONS ------- 4-8 78" DIAMETER 2 SAMPLING PORTS 2 AXES, EACH WITH 12 POINTS (TOTAL 24 POINTS) 6" =]B SECTION M-M BYPASS FIGURE 4-5. SPRAY DRYERS #312 AND #322 STACK DIMENSIONS WITH PORT AND POINT LOCATIONS ------- 4-9 4.3 Sulfate Process Sampling Locations. Figure 4-6 provides a schematic Illustration of the sulfate process (which incorporates a rotary calciner kiln) and gives the location of each sampling site. Each of the sampling locations is Individually discussed and illustrated. 4.3.1 #2 Calciner Inlet (Sampling Location H). Grab Samples of the feed to the rotary calciner were collected during each Method 5 run for moisture content determination. Sieve analysis was inappropriate due to the tacky consistency of the feed samples. 4.3.2 Water Spray Cooler Outlet (Sampling Location 1). Grab Samples of the product exiting the water spray cooler were collected during each Method 5 run for sieve analysis and moisture content determination. 4.3.3 East Side Calciner I.D. Fan Outlet (Sampling Location K). Sampling was performed in a 72-inch diameter vertical duct which was accessed by two sampling ports (labeled A and B) spaced 90 degrees apart. The ports were located 36 Inches (0.5 duct diameters) upstream and 12 inches (0.2 duct diameters) downstream from the nearest flow disturbances, as shown in Figure 4-7. A total of 24 sampling points (i.e., 12 points on each of two traverse axes labeled A and B) were sampled for particulate. Each point was sampled for 2.5 minutes, resulting in a net run time of 60 minutes. Two particle size runs were performed after each particulate run, one at point A-9 and one at point B-4. Runs S-13-A and S-13-B were each run for five minutes; the other four runs were each performed for 15 minutes. 4.3.4 East Side I.D. Fan Inlet (Sampling Location K'). Velocity traverses were performed in the 65-inch diameter duct which angled downward in the direction of the gas stream flow, as shown in Figure 4-8. Access was provided by a single port (labeled A) which was positioned 35 feet (6.5 duct diameters) downstream from the nearest disturbance and four feet (0.7 duct diameters) upstream from the nearest disturbance. Two twelve-point velocity traverses were made along the single axis for each velocity run. 4.3.5 West Side I.D. Fan Outlet (Sampling Location L). Sampling was performed in a 72-inch diameter vertical duct which was accessed by two ------- EAST ฎ * ROTARY CALCINER KILN #2 O PROCESS FLOW AIR FLOW GRAB SAMPLE SAMPLE POINT OBSERVATION POINT I CONDITIONING TOWER WET ESP M \ NO \ PETERSON I , SCRUBBER ~~U O M1 ^-I.D. I s T A C K -I.D. FAN WEST CONDITIONING TOWER WET ESP K',L' - METHOD 2 H,I - ASTM METHOD K,L - METHOD 5, IMPACTOR M,M' - METHOD 5 N f METHODS 5,7 O - METHOD 9 J - METHOD 22 FIGURE 4-6. SULFATE PROCESS AND SAMPLING POINTS AT AMERICAN CYANAMID, SAVANNAH, GEORGIA ------- 4-11 2 AXES, EACH WITH 12 POINTS, (TOTAL 24 POINTS) TO CONDITIONING TOWER 72" DIA. FLANGE UNION 2 SAMPLING PORTS FLANGE UNION -~ 6.5" SECTION N-N FLANGE UNION I.D. FAN (FROM CALCINER #2) FIGURE 4-7. #2 CALCINER EAST AND WEST SIDE I.D. FAN OUTLET DIMENSIONS WITH SAMPLING PORT AND POINT LOCATIONS ------- 65" DIA. TO I.D. FAN AXES: 1 POINTS/AXIS: 12 TOTAL POINTS: 12 SECTION P-P 1 SAMPLING PORT FROM CALCINER I I-1 IV) FIGURE 4-8. #2 CALCINER EAST I.D. FAN INLET DIMENSIONS WITH SAMPLING PORT AND POINT LOCATIONS ------- 4-13 sampling ports (labeled A and B) spaced 90 degrees apart. The ports were located 36 inches (0.5 duct diameters) upstream and 12 inches (0.2 duct diameters) downstream from the nearest flow disturbances, as shown in Figure 4-7. A total of 24 sampling points (12 points on each of two traverse axes labeled A and B) were sampled for particulate. Each point was sampled for 2.5 minutes, resulting in a net run time of 60 minutes. Two particle size runs were performed after each particulate run, one at point A-4 and one at point B-4. Runs S-16-A and S-16-B were performed for five minutes; the other four runs were 25 minutes in duration. 4.3.6 West Side I.D. Fan Inlet (Sampling Location L')ซ The west side fan inlet duct was a 73-inch diameter duct which was identical to the east side fan inlet duct in all other pertinent respects, as shown in Figure 4-9. Velocity measurements proceeded in the manner described in paragraph 4.3.4. 4.3.7 East and West Side ESP Outlets (Sampling Locations M and M'). The east and west side ESP outlets were identical, and the same testing procedures were used at both locations. Sampling was performed in a 54-inch diameter vertical duct accessed through two ports (labeled A and B) spaced 90 degrees apart, as shown in Figure 4-10. The ports were located 45 inches (0.2 duct diameters) downstream and 12 inches (0.8 duct diameters) upstream of the nearest flow disturbances. For particulate testing, 24 points (12 points on each of two traverse axes labeled A and B) were sampled for 2.5 minutes each, resulting in a total run time of 60 minutes. 4.3.8 #2 Calciner Exhaust Stack (Sampling Location N). Sampling was performed in the 73-inch diameter exhaust stack of the sulfate process. Two sampling ports 90 degrees apart were located 44 feet (7.2 stack diameters) downstream of the by-pass duct from the Peterson scrubber, and 50 feet (8.2 stack diameters) upstream from the top of the stack, as shown in Figure 4-11. For the particulate tests, a total of 12 points (six sampling points on each of two traverse .axes labeled A and B) were sampled. For run 25, each point was sampled for five minutes with a total test time of 60 minutes. For runs 26 and 27, the total test time was increased to 72 minutes (six minutes ------- 73" DIA. TO I.D. FAN AXES: 1 POINTS/AXIS: 12 TOTAL POINTS: 12 SECTION Q-Q 1 SAMPLING PORT FROM CALCINER FIGURE 4-9. #2 CALCINER WEST I.D..FAN INLET DIMENSIONS WITH SAMPLING PORT AND POINT LOOATIONS ------- 54" DIA. AXES: 2 POINTS/AXIS: 12 TOTAL POINTS: 24 54" DIA. 6" SECTION R-R SECTION S-S AMBIENT AIR INTAKE EAST SIDE TO SCRUBBER I M U1 1 R / B ESP A ( 1 12" A 1 j 1 45- ! R - S ' \ A f / o B ESP A. / 1 , s WEST SIDE FIGURE 4-10. #2 CALCINER EAST AND WEST ESP OUTLET DIMENSIONS WITH SAMPLING PORT AND POINT LOCATIONS ------- 4-16 50' 44' BYPASS 73" AIR FLOW -o 73" DIAMETER 1 I 5.5" 2 AXES, EACH WITH 6 POINTS (TOTAL, 12 POINTS) SECTION L-L 2 SAMPLING PORTS FROM' SCRUBBER FIGURE 4-11. jฑ2 CALCINER EXHAUST STACK DIMENSIONS WITH PORT AND POINT LOCATIONS ------- 4-17 per point) in order to increase the total sample volume and particulate catch. For the nitrogen oxides tests, a single point sample was taken. 4.3.9 #2 Calciner Exhaust Stack (Sampling Location 0). Plume opacity observations were performed at the exhaust stack outlet in accordance with the procedures outlined in EPA Reference Method 9. 4.3.10 #2 Calciner Product Outlet (Sampling Location J). Fugitive emissions readings (according to EPA Reference Method 22) were abandoned when judgement was made that steam, rather than product emissions, was being observed. ------- 5-1 5. SAMPLING AND ANALYTICAL METHODS 5.1 Sampling Objectives. This section describes the sampling and analytical procedures which were employed at the American Cyanamid Company manufacturing plant: in order to gather data concerning emissions from the pollution control equipment associated with the sulfate and chloride processes used to produce titanium dioxide. In addition, moisture and sieving analyses were performed on feed and product samples. The sampling program included outlet tests for particulate emissions, nitrogen oxides, particle sizing, and plume opacity. 5.2 Particulate Emissions Testing. Where appropriate, particulate emissions sampling conformed to the standards and procedures set forth by EPA Reference Methods 1-5 and described in 40 CFR Part 60, Appendix 7.3. It was necessary at several locations to modify the test procedures in order to cope with either heavy particulate loading or turbulent flow patterns. 5.2.1 #312 Baghouse Inlet. Due to heavy particulate loading, the run times were reduced by changing the number of sampling points from 24 to 12 and the sampling time per point to two minutes, resulting in run times of 24 minutes. This protocol was approved on site by EPA EMB and Entropy. 5.2.2 #312 Baghouse Outlet. The total amount of available straight run did not allow the placement of the sampling ports to meet the Method 1 criteria for minimum upstream and downstream distances. 5.2.3 #322 Baghouse Outlet. Because the duct was tapered with no available straight run, the placement of the sampling ports did not meet the Method 1 criteria for minimum upstream and downstream distances. Due to the heavy particulate loading encountered at this location during Test 1 , particulate run 7 was divided into two components which were performed, processed, and analyzed as two separate runs. The particulate catch from each component run was analyzed separately. Moisture content and flue gas composition were determined on a total run basis, with the same values used in the calculations for each component run (run 7 A and 7B). ------- 5-2 5.2.4 East and West I.D. Fans Outlets. The total amount of available straight run did not allow the placement of the sampling ports to meet the Method 1 criteria for minimum upstream and downstream distances. Due to the turbulent flow patterns present, the air flow rates measured were used only for the isokinetic sampling rate calculations; air flow rates as measured at the East and West 1.0. Fan Inlets were used for emission rates calculations. 5.2.5 East and West I.D. Fans Inlets. Because only one port was available for the velocity traversing, each velocity run consisted of two traverses of the same port. Due to the large amount of straight run, however, no significant error in the air flow data is expected. 5.2.6 East and West ESP Outlets. The total amount of available straight run did not allow the placement of the sampling ports to meet the Method 1 criteria for minimum upstream and downstream distances. 5.3 Sulfuric Acid Mist. Sulfuric acid mist emissions from the #2 Calciner Stack were determined by analyzing the particulate catch for total 3ulfates and calculating the results as 112804. 5.4 Trace Metals Analysis. For one run at each location, the Method 5 particulate catch and the distilled water reagent from the impingers were analyzed for trace metals by using atomic absorption spectrometry or by inductively coupled plasma spectrometry. These metals are zinc, nickel, iron, manganese, vanadium, calcium, silicon, aluminum, magnesium, fluorine, beryllium, uranium, lead, and mercury. 5.5 Sieve Analysis and Moisture Content. Sieve analysis and moisture content determinations were performed on the product samples. ASTM Method D 2216 was used to analyze the samples for moisture content, while ASTM Method D 422 was used for sieve analysis. Samples which could not be sieved due to moisture content were analyzed using only the second portion of Method D 422 (the hydrometer procedure). ------- 5-3 5.6 Plume Opacity. Visible emissions observations were performed in accordance with EPA Reference Method 9 as described in 40 CFR Part 60. However, cloudy atmospheric conditions prevented some of the scheduled opacity readings. 5.7 Fugitive Emissions. Fugitive emissions were determined in accordance with EPA Reference Method 22 as described in 40 CFR Part 60. 5.8 Particle Size Tests. Particle size determinations were made using a right angle inlet preseparator, followed by an Andersen or Flow Sensor Mark III cascade impactor. The test procedures were based upon the publication, "Procedures for Cascade Impactor Calibration and Operation in Process Streams - Revised 1979," developed by the Industrial Environmental Research Laboratory (IERL) and Southern Research Institute. Particle size testing was not performed at locations where water droplets were observed in the duct. ------- 6-1 6. QUALITY ASSURANCE 6.1 Introduction. The goal of quality assurance for the project was to ensure the accuracy of all data collected. The procedures used are contained in Entropy's "Quality Assurance Program Plan," which was approved by the U.S. EPA EMB in the contract agreement governing the project. In order to ensure continuity among field testing personnel, daily meetings were held before each day of the field testing. At the meetings, results from the testing conducted on the previous day were reviewed. Responsibilities were clearly delineated for each member of the testing team, and questions were addressed and resolved immediately. In situations where more than one person was performing similar activities, consistency was ensured through communication at the meetings. In addition to the general quality assurance measures, specific quality assurance activities were conducted for several of the individual test methods performed. 6.2 Sampling Train Components. Entropy's sampling equipment, including nozzles, pitot tubes, dry gas meters, orifices, and thermocouples, was uniquely identified and calibrated in accordance with documented procedures and acceptance criteria prior to and at the completion of the field testing program. All sampling equipment was manufactured by Nutech Corporation, Andersen 2000, Flow Sensor, or by Entropy. Calibration data for the sampling equipment are contained in Appendix 7.7. 6.3 Preseparator and Cascade Impactors. All internal components and surfaces of the impactors were cleaned in an ultrasonic bath to ensure that all surface impurities were removed, and visual inspections for cleanliness were made prior to shipment to the field. After each sample recovery, the preseparator, the impactor body, and the plates were rinsed with acetone to ensure that all organic residuals and/or particulate matter were removed. 6.4 Sample Collection Substrates. Schleicker & Schuell #30 glass fiber sample collection substrates were used for particle size testing. To prevent contamination of the substrate surface, all filters were handled with laboratory tweezers. This procedure was used during impactor assembly, sample recovery, and weighing of the substrates. ------- 6-2 6.5 Substrate Weighing. An analytical balance capable of weighing to the nearest 0.01 milligram (mg) was used. To ensure that no weight bias was produced from the preparation, transportation, recovery, or weighing procedures, two control samples were obtained during the test program. A reactivity run was performed to ensure that the flue gases did not interact with the substrate to produce extraneous results. For the reactivity run, a solid filter was placed in the front section of the impactor, and the impactor was introduced into the #312 Baghouse Outlet duct, and a sample was pulled through the head using the parameters outlined for a normal particle sizing run. The average difference between the pre- and post-test weights, as shown in Appendix 7.3.2, was 0.14 milligrams, based upon weight differences ranging from 0.00 to 0.34 milligrams. A blank run was also performed to demonstrate that the impactor could be assembled and disassembled without affecting the weight of the substrate. The average difference between the pre- and post-assembly weights was 0.14 milligrams, based upon a difference ranging from 0.02 to 0.34 milligrams. 6.6 Sample Analysis. In order to reduce the probability of errors or inconsistent results, one member of the field crew had sole responsibility for the sample analysis procedure. Sample analysis was performed in a room dedicated exclusively to filter weighing. 6.7 EPA Method 3. All Method 3 analyses were performed in triplicate. Each analyzer was checked for leaks prior to any analysis as specified in the method. Samples were analyzed within four hours of collection. 6.8 EPA Method 9. The visible emissions observers held current certifications issued within the last 6 months. Documentation verifying the observer's certifications are provided in Appendix 7.5. ------- |