ites Agen andards -ark NC 2 EMB Report S3-CDR-11 April 1984 Calciners and Dryers Emission Test Report • C.E. Minerals Muicoa Plant Andersonville, Georgia ------- NSPS DEVELOPMENT PARTICULATE, SULFUR DIOXIDE, AND NITOGEN OXIDES EMISSIONS AND PARTICLE SIZING TESTING #4 ROTARY CALCINER C.E. MINERALS MULCOA PLANT ANDERSONVILLE, GEORGIA APRIL 17 & 18, 1984 Compiled by: Entropy Post Office Box 12291 Research Triangle Park, N. C. 27709 68-02-3852 Work Assignment No. 8 EMB Project No. 81/08 EMB Report No. 83-CDR-ll Task Manager Dennis Holzschuh Emission Measurement Branch Emissions Standards and Engineering Division Research Triangle Park, N. C., 27711 OFFICE OF AIR QUALITY PLANNING AND STANDARDS OFFICE OF AIR, NOISE, AND RADIATION U.. S. ENVIRONMENTAL PROTECTION AGENCY RESEARCH TRIANGLE PARK, N. C., 27711 ------- TABLE OF CONTENTS SECTION PAGE 1. INTRODUCTION 1-1 1.1 Background 1-1 1.2 Scope of the Project 1-1 1.3 C.E. Minerals Mulcoa Plant Testing Program 1-1 1.3.1 Source Applicability 1-1 1.3.2 Outline of Testing Program 1-2 1.4 Report Organization 1-4 2. SUMMARY AND DISCUSSION OF RESULTS 2-1 2.1 Summary 2-1 2.2 Discussion 2-1 3. PROCESS DESCRIPTION AND OPERATION 3-2 3.1 Production of Calciner Feed 3-2 3.1.1 Raw Material 3-2 3.1.2 Fuel 3-2 3.1.3 Pellet Formation 3-2 3.1.4 Pellet: Drying . 3-2 3.1.5 Pellets as Feed 3-4 3.2 Calcining; Process 3-4 3.2.1 Kilns 3-4 3.2.2 Calcine 3-4 3.2.3 Exhaust Emissions 3-6 3.2.4 Control Equipment 3-6 4. SAMPLING LOCATIONS 4-1 4.1 Suitability of Sampling Sites 4-1 4.2 Rotary Calciner Feed Inlet (Sample Loc. A) 4-1 4.3 Vibrating Grate Cooler Product Outlet (Sample Loc. B) . . . 4-1 4.4 Vibrating; Grate Cooler Multiclone Outlet (Sample Loc. G). . 4-1 4.5 Multiclone Inlet (Sample Loc. C) 4-1 4.6 I.D. Fan Inlet East & West (Sample Loc. D & E) 4-4 4.7 Scrubber Exhaust Stack (Sample Loc. F & Observation Loc. G) 4-2 (continued next page) ------- ii TABLE OF CONTENTS (continued) SECTION PAGE 5. SAMPLING AND ANALYTICAL METHODS 5-1 5.1 Sampling Objectives 5-1 5.2 Particulate and Sulfur Dioxide Emissions Testing 5-1 5.3 Trace Metals Analysis 5-1 5.4 Sieve and Moisture Content Analysis 5-1 5.5 Plume Opacity 5-1 5.6 Particle Size Testing 5-1 5.7 Nitrogen Oxides Testing 5-1 6. QUALITY ASSURANCE 6-1 6.1 Introduction 6-1 6.2 Sampling Train Components 6-1 i6.3 Preseparator and Cascade Impactors 6-1 6.4 Sample Collection Substrates 6-2 6.5 Substrate Weighting 6-2 6.6 Sample Analysis 6-2 6.7 EPA Method 3 6-2 6.8 EPA Method 9 6-2 7. APPENDICES 1 7.1 Test Results and Example Calculations 2 7.1.1 Particulate and Sulfur Dioxide 2 7.1.1.1 Multiclone Inlet 2 7.1.1.2 I.D. Fan Inlet East & West 5 7.1.1.3 Scrubber Exhaust Stack and Example Calculations ... 10 7.1.2 Particle Sizing 16 7.1.2.1 Multiclone Inlet 17 7.1.2.2 I.D. Fan Inlet East & West 33 7.1.3 Nitrogen Oxides, Scrubber Exhaust Stack 62 7.2 Field and Analytical Data 66 7.2.1 Particulate and Sulfur Dioxide 66 ( continued next page) ------- ill TABLE OF CONTENTS (continued) SECTION APPENDICES 7.2.1.1 7.2.1.2 7.2.1.3 7.2.2 7.2.2.1 7.2.2.3 7.2.3 7.2.4 7.2.5 7.3 7.4 7.5 7.6 66 76 90 100 100 Multiclone Inlet l.D. Fan Inlet East & West Scrubber Exhaust Stack Particle Sizing Multiclone Inlet . l.D. Fan Inlet East & West 112 Visible Emissions, Scrubber Exhaust Stack 130 Nitrogen Oxides, Scrubber Exhaust Stack 145 Trace Metals Analytical Results 150 Sampling and Analytical Procedures 153 Feed and Product Analytical Data 239 Entropy Test Participants . 259 Calibration Data 260 ------- iv LIST OF TABLES Number Title Page 1-1 Testing Protocol and Run/Sample Numbering 1-3 Cross-Reference 2-1 ParticulLate Emissions and Concentrations, Summary . . 2-2 and Control Equipment Efficiencies Particulate Tests Summary of Results 2-2 Multiclone Inlet 2-3 2-3 I.I). Fan Inlet, East 2-4 2-4 I.I). Fan Inlet, West 2-5 Particulate and Sulfur Dioxide Summary of Results 2-5 Scrubber Stack 2-6 Summary of Particle Sizing Test Results 2-6 Multiclone Inlet 2-8 2-7 I.D. Fan Inlet, East 2-10 2-8 I.D. Fan Inlet, West 2-12 Nitrogen Oxides Emissions Rates and Concentrations 2-9 Scrubber Stack 2-14 Summary of Visible Emissions 2-10 Run 1 2-15 2-11 Run 2 2-16 2-12 Run 3 2-17 3-1 Data For Rotary Kilns 3-5 ------- LIST OF FIGURES Number Title Page 3-1 Simplified Process Flow Diagram 3-3 4-1 Process Flow Schematic Showing Sampling Locations . . 4-2 4-2 Multiclone Inlet 4-3 4-3 I.D. Fan Inlet East & West 4-5 4-4 Scrubber Exhaust Stack 4-6 ------- 1-1 1. INTRODUCTION 1.1 Background. 'Che Emission Measurement Branch (EMB) of the United States Environmental Protection Agency (EPA) is directing a project designed to generate support data for New Source Performance Standards (NSPS) for calciners and dryers in the mineral industries. Emission standards for the various industries may be developed based upon process-related emission factors determined from the testing of controlled sources. 1.2 Scope of the Project. The EMB is responsible for coordinating the efforts of Entropy and Midwest Research Institute (MRI) to achieve the goals of the testing program. Entropy has been retained under the EMB Contract No. 68-02-3852, Work Assignment No. 8 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. 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 C.E. Minerals Mulcoa Plant Testing Program. The present report covers stationary source sampling performed at the C.E. Minerals #3 Plant in Andersonville, Georgia on April 17 and 18, 1984 to characterize emissions from the #4 rotary calciner and associated air pollution control equipment. Dilip Jain and Siva Soora of C.E. Minerals and Dennis Holzschuh of EPA EMB were present to coordinate the testing. Amy J. Kowalski of MRI monitored the plant process and recorded operational data during the testing. 1.3.1 Source Applicability. The C.E. Minerals Mulcoa plant uses rotary calciners for the drying of pulverized or extruded clay. The plant's use of coal-fired rotary calciners represents the most difficult emissions control situation in the clay refining industry. The plant is considered to be well operated and well maintained, as well as providing feasible opportunities for inlet testing. ------- 1-2 1.3.2 Outline of Testing Program. Emission measurements were performed at the multiclone inlet, at the I.D. fan inlets (east & west) and at the scrubber exhaust stack. Table 1-1 outlines the testing program, giving test dates, sampling locations, test methods, and run numbers. ------- TABLE 1-1 TESTING PROTOCOL AND RUN/SAMPLE NUMBERING CROSS-REFERENCE ------- Sampling Objective Method Particulate ' EPA 5 Participate/ EPA 5 & 8 Sulfur Dioxide Particle Sizing Nitrogen Oxides Sieving/ Moisture Opacity Cascade Irapactor EPA 7 Grab Sample EPA 9' Location* 4/17 Test Set 4/17 4/18 MI IE IW SE MI IE IW SE CI VP VM SE 1 4 7 10 S1A&B S4A&B S7A&B** 10 1 1 1 1 2tm 5tm 8tm lltm S2A&B S5A&B S8A&B 11 2 2 2 2 3 6 9 12 S3A&B S6A&B S9A&B** 12 . 3 3 3 3 tm Method 5 particulate catch and distilled water from impingers analyzed for trace metals * Sampling Location Legend: MI - Multiclone Inlet IE - I.D. Fan Inlet East IW - I.D. Fan Inlet West SE - Scrubber Exhaust Stack CI - Calciner Inlet VM - Vibrating Grate Cooler Multiclone Outlet VP - Vibrating Grate Cooler Product Outlet ** The results of runs S7B and S9B are not tabulated in this report. Run S7B was underloaded; run S9B was overloaded. ------- 1-4 1.4 Report Organization. Immediately following is the "Summary of Results" section. Appendix 7.1 presents the complete results of each run; field data can be found in Appendix 7.2. The source and the process are described in the "Process Description and Operation" section. 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 7.3, while Appendix 7.4 presents analytical documentation. The final section, "Quality Assurance," notes the procedures used to ensure the integrity of the sampling program; Appendix 7.6 provides pertinent calibration data. Appendix 7.5 contains a listing of the Entropy test participants and their roles in the testing program. ------- 2-1 2. SUMMARY AND DISCUSSION OF RESULTS 2.1 Summary. Table 2-1 presents a summary of the particulate and sulfur dioxide emissions and concentrations at the sampled locations, as well as particulate collection efficiencies for the multiclone. Run-by-run summaries of the particulate testing are provided for the multiclone inlet and for the I.D. fans east and west in Tables 2-2 through 2-4, respectively. Table 2-5 summarizes the results of particulate and sulfur dioxide testing performed at the scrubber exhaust stack. Detailed results of all particulate and sulfur dioxide testing appear in Appendix 7.1.1. Tables 2-6 through 2-8 present the particle sizing test results for each of the sampled locations; particle sizing was not performed at the scrubber exhaust stack due to moisture in the flue gas. Appendix 7.1.2 presents the detailed results of particle size testing. Nitrogen oxides (as M^) results are summarized in Table 2-9; complete results are given in Appendix 7.1.3. Opacity observations (runs 1-3) are reported in Tables 2-10, 2-11, and 2-12. No visible emissions were observed throughout the testing; field data is presented in Appendix 7.2.3. The results of trace metals analyses are reported in Appendix 7.2.5. 2.2 Discussion of Results. At the I.D. fan inlet west location, particle sizing runs 7B and 9B were not tabulated in the results due to an extremely low catch (underloaded), and extremely large catch (overloaded), respectively. In order to calculate particulate removal efficiencies of the multiclone and scrubbers, a particulate concentration representing a combined inlets value is necessary. A technique for eliminating any bias due to uneven air flow distribution through the two fans was used in calculating the equivalent, weighted average concentrations as follows: Sum of A-!>ide & B-Side Emissions, Ib/hr 7,000 gr/lb Ceq= * = gr/DSCF for Sum of A-Side & B-Side Flow Rates, SCFM 60 min/hr combined inlets 554.15 + 463.07 7,000 = * = A'°278 Sr/DSCF ------- 2-2 TABLE 2-1 PARTICULATE EMISSIONS & CONCENTRATIONS SUMMARY AND CONTROL EQUIPMENT EFFICIENCIES Emission Rates, Ib/Hr: Multiclone Inlet I.D. Fan Inlet, East I.D. Fan Inlet, West Scrubber Stack Concentration, Gr/DSCF: Multiclone Inlet I.D. Fan Inlet, East I.D. Fan Inlet, West Equivalent I.D. Fan Inlet Scrubber Stack Collection Efficiency, %: Multiclone Scrubber Emission Rates, Kg/Hr: Multiclone Inlet I.D. Fan Inlet, East I.D. Fan Inlet, West Scrubber Stack Concentration, mg/DSCM: Multiclone Inlet I.D. Fan Inlet, East I.D. Fan Inlet, West Scrubber Stack 1 2,192.95 554.15 463.07 8.37 7.5227 4.3930 3.6634 4.0278 0.0336 46.46 99.16 994.7 251.4 210.0 3.80 17,212 10,051 8,382 76.89 - iest aec 2 2,361.38 564.37 471.38 8.08 8.2405 4.3858 3.7308 4.0614 0.0315 50.72 99.21 1,071.1 256.0 213.8 3.67 18,855 10,035 8,537 72.12 3 1,947.90 553.04 458.11 8.98 7.1672 4.1514 3.7454 3.9570 0.0344 44.79 99.14 883.5 250.9 207.0 4.07 16,399 9,499 8,570 78.77 Average 2,167.41 557.18 464.18 8.48 7.6434 4.31 3.7132 4.0154 0.0331 47.32 99.17 983.1 252.7 210.0 3.85 17,489 9,862 8,496 75.93 ------- 2-3 TABLE 2-2 PARTICULATE TESTS SUMMARY OF RESULTS Multiclone Inlet 1 2 3 Run Date 04/17/84 04/17/84 04/18/84 Test Train Parameters: Volume of Dry Gas 31.526 29.831 30.040 Sampled, SCF* Percent Isokinetic 107.5 103.5 109.9 Stack Parameters: Temperature, Deg. F 593 601 602 Air Flow Rates SCFM*, Dry ACFM, Wet Method 5 Results (English): Catch, milligrams Concen. , grains/DSCF* Emissions, pounds/hour Method 5 Results (Metric): Concen., milligrams/DSCM* Emissions, kilograms/ hour 34,010 78,921 15,367.5 7.5227 2,192.95 17,212.4 994.7 33,432 78,066 15,929.3 8.2405 2,361.38 18,855.4 1071.1 31,708 73,375 13,951.5 7.1672 1,947.90 16,399.4 883.5 * 68 Deg. F. - 29.92 in. Hg. ------- 2-4 TABLE 2-3 PARTICIPATE TESTS SUMMARY OF RESULTS I.D. Fan Inlet, East Side 456 Run Date 04/17/84 04/17/84 04/18/84 Test Train Parameters: Volume of Dry Gas 25.334 26.926 27.172 Sampled, SCF* Percent Isokinetic 102.4 106.7 104.0 Stack Parameters: Temperature, Deg. F 549 545 555 Air Flow Rates SCFM*. Dry ACFM, Wet Method 5 Results (English): Catch, milligrams Concen. , grains/DSCF* Emissions, pounds/hour Method 5 Results (Metric): Concen., milligrams/DSCM* Emissions, kilograms/ hour 14,717 33,312 7,211.5 4.3930 554.15 10,051.4 251.4 15,013 33,970 7,652.4 4.3858 564.37 10,035.4 256.0 15,542 34,752 7,309.4 4.1514 553.04 9,498.8 250.9 * 68 Deg. F. - 29.92 in. Hg. ------- 2-5 TABLE 2-4 PARTICULATE TESTS SUMMARY OF RESULTS I.D. Fan Inlet, West Side Run Date Test Train Parameters: Volume of Dry Gas Sampled, SCF* Percent Isokinetic Stack Parameters: Temperature, Deg. F Air Flow Rates 7 8 04/17/84 04/17/84 27.582 105.6 543 26.633 102.0 539 04/18/84 25.955 102.7 545 SCFM*, Dry ACFM, Wet Method 5 Results (English): Catch, milligrams ' Concen. , grains/DSCF* Emissions, pounds/hour Method 5 Results (Metric): Concen., milligrams/DSCM* Emissions, kilograms/hour 14,747 33,246 6,547.5 3.6634 463.07 8,382.2 210.0 14,740 33,331 6,438.7 3.7308 471.38 8,536.6 213.8 14,270 32,223 6,299.2 3.7454 458.11 8,569.8 207.0 * 68 Deg. F. - 29.92 in. Hg. ------- 2-6 TABLE 2-5 PARTICULATE AND SULFUR DIOXIDE TESTS SUMMARY OF RESULTS Scrubber Stack 10 11 12 Run Date 04/17/84 04/17/84 04/18/84 Test Train Parameters: Volume of Dry Gas 88.220 91.896 91.630 Sampled, SCF* Percent Isokinetic 99.0 100.2 98.2 Stack Parameters: Temperature, Deg. F 140 140 141 Air Flow Rates SCFM*, Dry 29,064 29,915 30,432 ACFM, Wet 41,994 43,217 43,558 Method 5 Results (English): Catch, milligrams 192.1 187.7 204.4 Concen., grains/DSCF* 0.0336 0.0315 0.0344 Emissions, pounds/hour 8.37 8.08 8.98 Method 5 Results (Metric): Concen., milligrams/DSCM* 76.8895 72.1231 78.768 Emissions, kilograms/hour 3.80 3.66 4.07 Method 8 Sulfur Dioxide (English): Catch, Milligrams 2,871.8 3,006.8 2,772.0 Concen., ppmbyvol., dry 432.06 434.27 401.52 Emission, pounds/hour 125.15 129.48 121.78 (continued on next page) ------- 2-7 TABLE 2-5 PARTICULATE AND SULFUR DIOXIDE TESTS SUMMARY OF RESULTS Scrubber Stack (continued) 10 11 12 Run Date 04/17/84 04/17/84 04/18/84 Method 8 Sulfur Dioxide (Metric): Concen., milligrams/DSCM* 1,149.46 1,155.35 1,068.22 Emissions, kilograms/hour 56.77 58.73 55.24 * 68 Deg. F. - 29.92 in. Hg. ------- 2-8 TABLE 2-6 SUMMARY OF PARTICLE SIZING TEST RESULTS Multiclone Inlet SAMPLING DATA Date Start Time Finish Time Impactor Flow Rate (1/min) Isokinetic Ratio (%) STACK DATA Temperature (degrees C) Moisture (%) Velocity (m/min) EMISSION DATA Concentration (mg/dscra) Percent Recovery (PS cone./ M-5 cone.) Cumulative % Mass less than 10 microns Concentration < 10 microns: From PS runs, rag/dscra .From M-5 runs, mg/dscm Emission Rate < 10 microns (kg/hr, from M-5 runs) PS Run 1 4/17/84 1323,1412 1325,1413 21.90 108.5 309 12.3 643.4 13,297 62.0 42.0 5,670 8,996 418 PS Run 2 4/17/84 1751,1846 1753,1847 21.90 105.3 322 12.2 650.1 6,655 32.0 58.0 3,850 12,116 621 PS Run 3 4/18/84 1401,1434 1403,1436 15.30 103.9 320 11.6 471.1 8,019 44.0 34.0 2,600 6,164 300 Av e raj 317 12.0 588.2 9,324 46.0 45.0 4,040 9,091 446 PS: Particle Size Run M-5: Method 5 Particulate Run ------- 2-9 COMPANY NAME ADDRESS. PARTICLE SIZE DISTRIBUTION CE Mineirals Mulcoa Plant Andersonville, Georgia AVERAGE OF RUNS la,lb,2a,2b, 3a,3b SAMPLING LOCATION Multiclone Inlet DATE!s) 4/17/84 , 4/18/84 DENSITY = 1 GM/CM I i O 0. O o in LI N U) U O 90 •• " eo- s 70 - 60 I 50 " 40 - 30 : "O I 0 q * 8—! 7 — : s — : 5 - 4 — 1 •5 - 2— ~ 1 * .9 — = a -, = . 7 = . 6 — ; .5 —I . 3 —I 2 n 1 ' ' 2 < O •r> j \ \ i 5 I T} i 1 1 1 0 I 5 2 (?) \LS i ill in ilium 0 30 t (?) v£x ( ( l) \ ^D i i;.i;;ii mi in 1111 1.1 iiniiin nu 0 50 60 70 80 ( 1 1 1 1 1 1 1 1 5 90 ! i i IS 9 PERCENT OF PARTICLES LESS THAN INDICATED SIZE ------- 2-10 TABLE 2-7 SUMMARY OF PARTICLE SIZING TEST RESULTS I.D. Fan Inlet, East Side SAMPLING DATA Date Start Time Finish Time Impactor Flow Rate (1/min) Isokinetic Ratio (%) STACK DATA Temperature (degrees C) Moisture (%) Velocity (m/min) EMISSION DATA Concentration (mg/dson) Percent Recovery (PS cone./ M-5 cone.) Cumulative % Mass less than 10 microns Concentration < 10 microns: From PS runs, mg/dscm From M-5 runs, mg/dscm Emission Rate < 10 microns (kg/hr, from M-5 runs) PS Run 4 4/17/84 1243,1258 1247,1302 17.70 103.8 289 13.1 538.4 8,777 87.0 47.0 4,120 4,724 118 PS Run 5 4/17/84 1745,1755 1747,1757 17.10 105.9 281 13.4 528.5 9,406 94.0 47.0 4,400 4,716 120 PS Run 6 4/18/84 1414,1424 1416,1426 17.60 110.7 294 11.8 661.5 8,884 93.0 32.0 2,770 2,944 78 Averaj 288 12.8 576.1 9,022 91.0 42.0 3,763 4,121 105 PS: Particle Size Run M-5: Method 5 Particulate Run ------- COMPANY NAME 2-11 PARTICLE SIZE DISTRIBUTION CE Minerals Mulcoa Plant AVERAGE OF , 5b, ADDRESS Andersonville, Georgia SAMPLING LOCATION DATE! s ) 4/17/84. 4/18/84 1-D- Fan Inlet East- side DENSITY = I CM/CM 6a,6b ft n ' on = 70.. - 50 - -: £ 40 : 30 • : 1 i u IT i - I 0 i . * H 8—| 26 = 6 -- $ 5-i U i A -. . = O = _"> = Q , 3 W : N : — f tn 2 a u • j o I .— : ? .9 * a = 7 r .= . 6 — : .5 — : : 2 . -" i — CO 1 0 ^•^ S / ^ y i) 0 ^ i i rm i r n""r"i 5 10 IS 20 30 40 SO 60 70 SO 85 90 95 98 PERCENT OF PARTICLES LESS THAN INDICATED SIZE ------- 2-12 TABLE 2-8 SUMMARY OF PARTICLE SIZING TEST RESULTS I.D. Fan Inlet, West Side SAMPLING DATA Date Start Time Finish Time Impactor Flow Rate (1/min) Isokinetic Ratio (%) STACK DATA Temperature (degrees C) Moisture (%) Velocity (m/min) EMISSION DATA Concentration (mg/dscm) Percent Recovery (PS cone./ M-5 cone.) Cumulative % Mass less than 10 microns Concentration < 10 microns: From PS runs, mg/dscm From M-5 runs, mg/dscm Emission Rate < 10 microns (kg/hr, from M-5 runs) PS Run 7 4/17/84 1350 1352 30.00 109.3 293 13.3 852.4 6,191 74.0 72.0 4,429 5,951 149 PS Run 8 4/17/84 1833,1857 1835,1859 23.80 109.9 286 13.9 682.9 6,241 73.0 55.0 3,430 4,695 118 PS Run 9 4/18/84 1454 1456 14.80 108.4 279 13.6 423.2 5,273 62.0 46.0 2,425 3,942 96 Averag 286 13.6 652.8 5,902 70.0 57.0 3,428 4,862 121 PS: Particle Size Run M-5: Method 5 Particulate Run \ ------- 2-13 COMPANY NAME ADDRESS _. PARTICLE SIZE DISTRIBUTION CE Minerals Mulcoa Plant AVERAGE OF RUNS^a .83,813,93 Andersonville, Georgia SAMPLING LOCATION I.D. Fan Inlet West-side DATE!s) 4/17/84. 4/18/84 DENSITY = I GM/CM3 ft n a 70 , - 50- : 40 = 30 " ? n i - 1 O _ «- 9 * 26 '' ^ 3 1 o = _" : Q 3 3 UI i N : 01 2 H u : u : OL 9 = a . = 7 .S 2 • . . 1 — 1 ( V_J ^1 ^ G ;) o V^> v_x ( D c V ^ i riii i 5 10 IS 20 30 40 50 60 70 SO 85 90 95 98 PERCENT OF PARTICLES LESS THAN INDICATED SIZE ------- 2-14 TABLE 2-9 NITROGEN OXIDES (AS N02) EMISSION RATES & CONCENTRATIONS SUMMARY OF RESULTS Scrubber Stack - Run Date Sample Number Parameters per Run: Air Flow Rate, dry SCFM Nitrogen Oxides (as N02 ) Results: Concentration, ppm, dry Emissions, Lb/Hr 10 04/17/84 10A-10D 29,060 265.5 55.2 - K.un numoers - 11 04/17/84 11A-11D 29,920 311.4 66.7 12 04/18/84 12A-12D 30,430 321.0 69.9 ------- 2-15 TABLE 2-10 SUMMARY OF VISIBLE EMISSIONS Run 1 Date: 4/17/84 Type of Discharge: Stack Height of Point of Discharge: 120' Wind Direction; West-North-West Color of Plume:_White Observer No.: Distance from Observer to Discharge Point: Direction of Observer from Point: South Type of Plant: Clay Location of Pischarge:Multiclone Description of Sky;Partly Cloudy Wind Velocity; 8-12 Detached Plume: No Duration of Observation; 197 min. 950 ' Height of Observation Point; Ground level Description of Background; Partly Cloudy Set Time Number Start End SUMMARY OF AVERAGE OPACITY Opacity Set Time Sum Average Number Start End Opacity Sum Average 1 2 3 4 5 6 7 8 9 10 11 12 0958 1004 1010 1016 1022 1028 1034 1040 1046 1152 1158 1204 1004 1010 1016 1022 1028 1034 1040 1046 1152 1158 1204 1210 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 13 14 15 16 17 18 19 20 21 22 23 1210 1216 1222 1228 1234 1240 1246 1252 1258 1304 1310 1216 1222 1228 1234 1240 1246 1252 1258 1304 1310 1315 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 - 3 O 2 o U 2 1 HR 30 TIME ------- 2-16 TABLE 2-11 SUMMARY OF VISIBLE EMISSIONS Run 2 Date: 4/17/84 Type of Discharge: Stack Height of Point of Discharge: 120* Wind Direction; West-North-West Color of Plume; White Observer No.: Distance from Observer to Discharge Point: Direction of Observer from Point: South Type of Plant; Clay Location of Discharge;Multiclone Description of Sky:Partly Cloudy Wind Velocity: 12-15 Detached Plume: No Duration of Observation: 150 min. 800' Height of Observation Point; Ground level Description of Background: Partly Cloudy Set Time Number Start End SUMMARY OF AVERAGE OPACITY Opacity Set Time Sum Average Number Start End Opacity Sum Average 1 2 3 4 5 6 7 8 9 10 11 12 13 14 1500 1506 L512 1518 1524 1530 1536 1542 1548 1554 1600 1606 1612 1618 1506 1512 1518 1524 1530 1536 1542 1548 1554 1600 1606 1612 1618 . 1624 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 15 .16 17 18 19 20 21 22 23 24 25 26 1624 1630 1636 1642 1646 1652 1658 1704 1710 1716 1722 1728 1630 1636 1642 1646 1652 1658 1704 1710 1716 1722 1728 1730 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 I HR 30 TIME ------- 2-17 TABLE 2-12 SUMMARY OF VISIBLE EMISSIONS Run 3 Date: A/18/84 Type of Discharge; Stack Height of Point of Discharge: 120' Wind Direction; West-North-West Color of Plume: White Observer No.: Type of Plant: Clay Location of Discharge;Multiclone Description of Sky: Clear Wind Velocity; 8-10 Detached Plume: No Distance from Obseiver to Discharge Point: Direction of Observer from Point: South Duration of Observation; 150 min. 800 ' Height of Observation Point; Ground level Description of Background; Clear Set Number Time Start End SUMMARY OF AVERAGE OPACITY Opacity Set Time Sum Average Number Start End Opacity Sum Average 1 2 3 4 5 6 7 8 9 10 11 12 1203 1209 1215 1221 1227 1233 1239 1245 1251 1257 1303 1309 1209 1215 1221 1227 1233 1239 1245 1251 1257 1303 1309 1315 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 13 14 15 16 17 18 19 20 21 22 23 24 1315 1321 1327 1333 1339 1345 1357 1403 1409 1415 1421 1427 1321 1327 1333 1339 1345 1351 1403 1409 1415 1421 1427 1433 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 O I HR 30 TIME ------- 3-1 STATEMENT OF CONFIDENTIALITY All information referenced in the Process Description as (Confidential Addendum No. 1 through No. 7) have been deemed confidential by the C.E. Minerals Mulcoa Plant officials. Due to this fact, this information has been deleted from the final report and put under separate cover. Pending determination by the Environmental Protection Agency of the confidentiality of this information., they have been submitted as described to us for official entry into our confidential files. ------- I 3-2 3. PROCESS DESCRIPTION AND OPERATION 3.1 Production of Calciner Feed. 3.1.1 Raw Material. A simplified process flow diagram representative of plant operations is shown in Figure 3-1. Kaolinitic clays are obtained from nearby mining operations, transported to the plant by truck, and deposited in outside storage piles. Various clays are withdrawn from storage piles and mixed in predetermined proportions to obtain the desired product composition and properties. (See Confidential Addendum, No. 1, for a description of processing methods). 3.1.2 Fuel. The fuel used in this operation is natural gas. No. 2 fuel oil is a standby fuel. 3.1.3 Pellet Formation. The clay is pulverized (see Confidential Addendum, No. 2, for particle size information) in a roller mill swept with heated air. The pulverized clay produced by the roller mill is mixed with water in a pug mill, and the mixture is extruded to form 1.3 to 2.5 cm (0.5 to 1 in.) diameter pellets (referred to as "noodles") of varying lengths up to about 0.6 m (2 ft.). Some of the raw material bypasses the mills and is only processed through the pug mill and extruder before being calcined. Mulcoa 47 (and Mulcoa 44, a product very similar to Mulcoa 47 in composition) are produced using the bypass method. C.E. Minerals personnel believe these bypass materials generate the most difficult to control emissions. (Mulcoa 44 was being processed during the testing). 3.1.4 Pellet Drying. Pellets produced by the extruder are dried on a moving pan dryer (natural gas is used as fuel). This pellet dryer dries only the surface of the pellets so that they do not stick together and their handling properties are improved. The moisture content of the dried pellets is 20 to 22 percent, and they have a loose fill density of 1,600 to 1,760 kg/m3 (100 to 110 Ib/ft3) . The average water evaporation rate for the pellet dryer is about 1,810 kg/h (4,000 Ib/h). ------- Outside Storage Piles Truck Tiamporl Vent Vent Collected . Dust Water Vent Wot Cyclone Scruljljor • Pallet Dryer (Moving Pan) 1/2 - 1 In. Diameter Pellets To Bulk Loading To Bugged Shipping Figure 3-1. Simplified process flov; diagram for C-G Minerals plant at Andcrsonvllle, Georgia, ------- 3-4 3.1.5 Pellets as Feed. As shown in Figure 3-1, dried pellets are used as feed material for the rotary calciner (kiln) and vibrating-grate cooler system. The operations described above for mixing, fine grinding, and extruding the clay are all designed to effect intimate contact of the clay particles and to promote a chemical reaction that produces mullite during calcining. All moisture and other volatile matter are removed during calcining. The chemical reactions are as follows: Heat ~ 2H20 > A1203 - 2Si02 + 2H20 Heat 3 (A12(>3 - 2Si02) > 3A1203 - 2Si02 + 4Si02 Mullite Pellets produced using the bypass method contain particles that are less uniform in size than those produced with the additional milling. This causes them to break apart more during calcining, thus making emissions from bypass materials more difficult to control than the emissions from other mullite products. 3.2 Calcining Process. 3.2.1 Kilns. C.E. Minerals operates seven identical rotary kilns in Andersonville, and each kiln is operated at its design capacity. Data for the rotary kiln equipment is shown in Table 3-1. The kilns are operated continously throughout the year except for occasions when a shutdown is necessary to repair equipment. The maximum kiln temperature is 1540° to 1760°C (2800° to 3200°F) and the heat application method is counterflow. The pulverized coal used as fuel has a heating value of about 30,260 kj/kg (13,000 Btu/lb) and contains 5 to 6 percent ash and less than 1 percent sulfur. 3.2.2 Calcine. The hot calcine discharged from the rotary kiln is fed to a vibrating-grate cooler (see Confidential Addendum, No. 3, for cooler ------- 3-5 TABLE 3-1. DATA FOR ROTARY KILNS USED AT C-E MINERALS MULCOA PLANTS AT ANDERSONVILLE, GEORGIA Equipment dimensions Design production capacity Method of determining actual production rate Hours of operation Hours/day Hours/week Hours/year Retention time (min) Maximum kiln temperature (°F) Heat application method Fuel used Fuel to product ratio (ton/ton) Feed moisture content (%) Feed particle size Feed density, loose fill (lb/ft3) Product moisture content (%) Effect of over-calcining Heat recovery system Normal life of rotary kiln (yr) Maintenance and repair practices 8 ft dia. by 150 ft long (See Confidential Addendum, No. 5) Electronic scale on conveyor . feed belt 24 168 8,760 120 2,800 to 3,200 Counterflow Coal (pulverized) ("See Confidential Addendum, No. 6} j 20-22 \ to 1 in. dia. pellets 100-110 0 Reduces quality ~ 80% of exhaust air from cooler used as secondary air for kiln 50 Good preventive maintenance; scheduled shutdowns for repairs as necessary. Patching of refractory lining is infrequently required. ------- 3-6 dimensions). The clay pellets are moved through the cooler by the horizontal vibration of the bed along the longitudinal axis. (See Confidential Addendum, No. 4, for a description of cooler operation). 3.2.3 Exhaust Emissions. Air passes upward through the grate and the vibrating bed of calcine. About 80 percent of the air leaving the cooler is sent to the discharge end of the rotary kiln as secondary air for that unit. The remainder of the air from the cooler is ducted through a multiclone collector, an induced draft fan, and a vent stack. Exhaust gases from the rotary kiln are ducted through a multiclone collector (manufactured by Zurn Industries) , an exhaust fan, a venturi scrubber, and a vent stack to the atmosphere. (See Confidential Addendum, No. 7, for vent stack dimensions). 3.2.4 Control Equipment. At the inlet to the scrubber the gas temperature is about 2H6°C (600°F). This scrubber is constructed of 316 low-carbon stainless steel. Sulfur in the clay and coal results in acid buildup in the scrubber water and causes corrosion problems. A system for adding calcium oxide (CaO) to the scrubber water has recently been installed. The water flow rate to the scrubber is 1,363 1/min (360 gpm). The pressure drop across the scrubber is 4.5 kPa (18 in. w.c.). The design efficiency of the wet scrubber is greater than 90 percent. ------- 4-1 4. SAMPLING LOCATIONS 4.1 Suitability of Sampling Sites. The primary goal of the testing program was to characterize emissions from the #4 rotary calciner dryer. Additionally, physical properties of the process feed stock and the product were investigated. Sampling sites appropriate to these objectives were approved prior to testing. Each sampling location is discussed individually, and the position of each site within the system is illustrated in Figure 4-1. 4.2 Rotary Calciner Feed Inlet (Sampling Location A). Grab samples of the feed to the rotary calciner were collected for sieve analysis and moisture content determination. Samples were taken during each set of simultaneous Method 5 runs. 4.3 Vibrating Grate Cooler Product Outlet (Sample Location B). Grab samples of the product were collected for sieve analysis and moisture content determination. Samples were taken during each set of simultaneous Method 5 runs. 4.4 Vibrating Grate Cooler Multiclone Outlet (Sample Location G). Grab samples of the product were collected for sieve analysis and moisture content determination. Samples were taken during each set of simultaneous Method 5 runs. 4.5 Multiclone Inlet (Sampling Location C). Particulate emissions and particle size distribution testing was conducted in the 55-inch by 95-inch expansion flume. Four sampling ports were positioned 40 feet from the ground, 7.6 feet from the nearest upstream disturbance and 4.7 feet from the nearest downstream disturbance. A schematic of the sampling location is shown in Figure 4-2. Particulate sampling was done using 24 points (i.e. six points located on four traverse axes); each point was sampled for 2.5 minutes, resulting in a total test time of 60 minutes. Particle size runs were performed for either 1.5 or 2 minutes. During each run, two points were sampled for equal lengths of time. ------- 4-2 ATMOSPHERE u . STACK I WET CYCLONE SCRUBBER OBSERVATION POINT-I SAMPLING POINT-F ATMOSPHERE STACK SAMPLING POINT-D FAN T 4 EAST 'CD (£>" WEST SAMPLING POINT-E SAMPLING POINT-C SAMPLING POINT-A MULTICLONE SAMPLING POINT-G FAN MULTICLONE I PRODUCT IN ROTARY CALCINER VIBRATING GRATE COOLER AMBIENT AIR -*—TO BULK LOAD SAMPLING /TO SCREENING, POINT-B CRUSHING & BAGGING A METHODS 5&8,7 <-—* TRACE METALS • METHOD 9 ® GRAB SAMPLE O METHOD 5, IMPACTOR, TRACE METALS FIGURE 4-1. ROTARY CALCINER PROCESS SCHEMATIC SHOWING SAMPLING LOCATIONS ------- 95" 4-3 55' I.I P B 24 SAMPLING POINTS SECTION M-M TO MULTICLONE FROM CALCINER .4 SAMPLING PORTS FIGURE 4-2. MULTICLONE INLET DIMENSIONS WITH SAMPLING PORT AND POINT LOCATIONS ------- 4-4 4.6 I.D. Fan Inlet East & West (Sampling Locations D & E). Particulate emissions and particle size tests were performed in a 104.5-inch by 24.5-inch rectangular duct. Five sampling ports were located 164 inches upstream and 120 inches downstream from the nearest flow disturbance, as shown in Figure 4-3. For particulate tests, each of the I.D. fan inlet cross sections (east and west) was divided into 25 equal areas (i.e. five sampling points along each of five traverse axes). Of the 25 possible points, only 20 points were sampled; the first point along each traverse axis was not sampled due to the disruption of air flow along the air duct wall caused by high negative pressure. Each of the 20 points was sampled for three minutes, resulting in a total run time of 60 minutes. Particle size runs ranged in length from 1.5 to 4 minutes. During each run, two points were sampled for equal lengths of time. 4.7 Scrubber Exhaust Stack (Sample Location F, Observation Point I). The particulate and particle size tests were performed in a 60-inch diameter round duct. Two sampling ports spaced 90° apart are located approximately 26 feet downstream from the nearest flow disturbance (straightening vanes) and 48 feet upstream from the stack gas exit point. A schematic of the sampling location is provided in Figure 4-4. The stack cross section was divided into 24 equal areas (i.e., two traverse axes with 12 points each) for particulate and sulfur dioxide emissions sampling. Each point was sampled for five minutes, resulting in a total run time of 120 minutes. Visible emissions observations and nitrogen oxides testing were also performed at the scrubber exhaust stack. Particle size testing was not performed at this location due to the presence of moisture in the flue gas. ------- 4-5 5 AXES 4 POINTS/AXIS 20 TOTAL POINTS 4"~1_ 1 1 ^ _^ l_i_ ' !— ' — '_t_- 1 1 A U U U U B C D E 1 T 24.5" ~T SECTION M-M TO SCRUBBER WEST A - V /\ i 1 1 I \ y| i 1 t -24.5»_ I . 1 1 FAN TO SCRUBBER X 1 1 , / EAST A M • FIGURE 4-3. I.D. FAN INLET POINT LOCATIONS >1 V ,. FRC 1 - 1 MULTICLONE - i n A s " i 00 A B \ V / / I \ \ \x l i C D E / \ \ \ . i • 1 FAN / / / ^^'S i \ 164" v • 1 1 67" M I t DUCT DIMENSIONS WITH SAMPLING PORT AND (TYPICAL FOR EAST AND WEST INLETS) ------- 4-6 r — H 60" i 4 2 5 8' 6' 4" 1 — o — A I !|> 1 ' i ! i B 2 AXES 12 POINTS/AXIS 24 TOTAL POINTS 60" DIA. SECTION L-L 2 SAMPLING PORTS STRAIGHTENING VANES FIGURE 4-4. SCRUBBER EXHAUST STACK DIMENSIONS WITH SAMPLING PORT AND POINT LOCATIONS ------- 5-1 5. SAMPLING AND ANALYTICAL METHODS 5.1 Sampling Objectives. This section describes the sampling and analytical procedures which were employed at the C.E. Minerals Mulcoa plant in order to gather data concerning emissions from the #4 rotary calciner and associated air pollution control equipment and to investigate physical properties of the process feed stock and the product. The sampling program included tests for particulate and sulfur dioxide, trace metals, and nitrogen oxides emissions, sieve and moisture analysis on feed and product samples, plume opacity, and particle size distribution. The sampling methods used are fully described in Appendix 7.3, portions of which are extracted from 40 CFR Part 60. 5.2 Particulate and Sufur Dioxide Emissions Testing. Where appropriate, particulate emissions sampling conformed to the standards and procedures set forth by EPA Reference Method 5. Method 8 was combined with Method 5 testing at the scrubber exhaust stack for the determination of sulfur dioxide. It was necessary at some locations to modify the test procedures in order to cope with heavy particulate loading and/or high negative pressure,, 5.3 Trace Metals Analysis. The Method 5 particulate catch and the distilled water reagent from one run at each location were analyzed for trace metals by using atomic absorption or inductively coupled argon plasma spectrometry. These metals are zinc, nickel, iron, manganese, vanadium, calcium, silicon, aluminum, magnesium, fluorine, beryllium, uranium, lead, and mercury. 5.4 Sieve Analysis and Moisture Content. Sieve analysis and moisture content determinations were performed on all feed and 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. f 5.5 Plume Opacity. Plume opacity observations were performed in accordance with EPA Reference Method 9 as described in 40 CFR Part 60. ------- 5-2 5.6 Particle Size Testing. Particle size determinations were made using a right angle inlet preseparator, followed by an Andersen 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. 5.7 Nitrogen Oxides Testing. Nitrogen oxides emissions were determined by utilizing the sampling and analytical procedures outlined in EPA Method 7. Each Method 7 run consisted of four samples taken concurrently with the Method 5 sampling. ------- 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 sind 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 or by Entropy. Calibration data for the sampling equipment are contained in Appendix 7.9. 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 and a blank run. The 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 stack, 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 Section 7.6, was 0.01 milligrams, based upon weight differences ranging from 0.00 to 0.02 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 0.05 milligrams, based upon a difference ranging from 0.01 to 0.10 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 7.2.3. ------- |