EPA-650/2-73-013 August 1973 Environmental Protection Technology Series Ss 2 = 3 % Ly, » 2 etEPA-650/2-73-013 EPA ALKALI SCRUBBING TEST FACILITY: SODIUM CARBONATE AND LIMESTONE TEST RESULTS by Dr. Michael Epstein, Louis Sybert, and Irwin A. Raben Bechtel Corporation 50 Beale Street San Francisco, California 94119 Contract No. PH 22-68-67 Program Element No. 1A2013 EPA Project Officer: Frank T. Princiotta Control Systems Laboratory National Environmental Research Center Research Triangle Park, North Carolina 27711 Prepared for OFFICE OF RESEARCH AND DEVELOPMENT U.S. ENVIRONMENTAL PROTECTION AGENCY WASHINGTON, DC 20460 August 1973This report has been reviewed by the Environmental Protection Agency and approved for publication. Approval does not signify that the contents necessarily reflect the views and policies of the Agency, nor does mention of trade names or commercial products constitute endorsement or recommendation for use iiACKNOWLEDGEMENT The authors wish to acknowledge the contribution of the Bechtel, TVA and EPA on-site personnel at the Paducah Test Facility. The authors are also indebted to Mr. C. Leivo, Dr, C. Wang and Mr. C, Rowland of Bechtel, who aided in the preparation of this report.Section CONTENTS INTRODUCTION AND SUMMARY TEST FACILITY 2.1 Scrubber Selection 2.2 System Description 2.3 EPA Pilot Plant Support TEST PROGRAM 3.1 Test Program Objectives 3.2 Test Periods and Test Program Schedule 3.3 Test Designs 3.4 Analytical Program 3.5 Data Acquisition and Processing AIR/WATER AND SODIUM CARBONATE TEST RESULTS 4.1 Pressure Drop Data from Air/Water and Sodium Carbonate Tests 4,2 Sulfur Dioxide Removal Data from Sodium Carbonate Tests SHORT-TERM FACTORIAL LIMESTONE TEST RESULTS 5.1 SO, Removal Results 5.2 Analytical Results 5.3 Particulate Removal Results Page 2-1 2-1 2-6 2-10 3-1 3-1Section 6 10 ret CLOSED LIQUOR LOOP RELIABILITY VERIFI- CATION TEST RESULTS 6.1 Performance Data 6.2 Material Balances OPERABILITY AND RELIABILITY OF THE TEST FACILITY 7.1 Closed Liquor Loop Operation 7.2 Equipment Operating Experience 7.3 Materials Evaluation 7.4 Instrument Operating Experience 7.3 System Modifications 7.6 System Reliability ANALYSIS OF PRESSURE DROP DATA 8.1 Venturi Scrubber 8.2 TCA Scrubber 8.3 Hydro-Filter Scrubber ANALYSIS OF SODIUM CARBONATE SCRUBBING DATA, 9.1 High Concentration Sodium Carbonate Data 9.2 Low Concentration Sodium Carbonate Data for Chemico Venturi ANALYSIS OF SHORT-TERM FACTORIAL LIME- STONE DATA 10,1 Statistical Models for SO, Removal 10,2 Closed-Form Correlations for Predicting SOz Removal 10.3 Computer Models for Predicting SO, Removal and Slurry Compositions REFERENCES Page 6-1 6-2 6-16 a4 7-15 7-22 7-25 731 10-1 10-1 10-8 10-12 1-1Appendix A CONVERTING UNITS OF MEASURE B CORRECTION FACTOR FOR SO; REMOVAL DUE TO DILUTION EFFECT OF REHEATER GAS AND WATER VAPOR DU PONT CALIBRATION CURVES AND CORREC- TION FACTORS D | WATER BALANCES FOR SCRUBBER SYSTEMS DURING CLOSED-LOOP LIMESTONE TESTING viiFigure 2-1 2-2 ILLUSTRATIONS Schematic of Venturi Scrubber and After-Absorber Schematic of Three-Stage TCA Scrubber Without Trap-Out Tray Schematic of Hydro-Filter Scrubber Typical Process Flow Diagram for Venturi System Typical Process Flow Diagram for TCA System Typical Process Flow Diagram for Hydro-Filter System Scrubber Area Operations Building and Thickener Area Control Room Shawnee Test Schedule Preliminary Results for SO, Removal in the Chemico Venturi with a Nine-Inch Pressure Drop Effect of Gas and Liquor Flow Rates on SO, Removal in the Four Header Spray Tower Effect of Liquid-to-Gas Ratio and Gas Velocity on $Oz Removal in the Four-Header Spray Tower Effect of Inlet Liquor pH on SO2 Removal in the Four-Header Spray Tower (Limestone Depletion Run No, 463-1A) Effect of Height of Spheres and Gas Rate on SOy Removal in the Six-Grid Three-Stage TCA System Effect of Spheres Versus No Spheres and Gas Rate on SO, Removal in the Six-Grid TCA System ix 2-9 2-11 2-12 2-13 3-4 5-25 5-267-7 7-8 7-9 7-10 8-1 Effect of Liquor and Gas Rate on SO, Removal in the Four-Grid Three-Stage TCA System Effect of Liquid-To-Gas Ratio and Gas Velocity on SO, Removal in the Four-Grid Three-Stage TCA System Effect of Gas and Liquor Flow Rates on Oz Removal in the Hydro-Filter with Five Inches of Marbles Effect of Liquid-To-Gas Ratio and Gas Velocity on SOz Removal in the Hydro-Filter with Five Inches of Marbles Operating Data for Venturi Run 501-1A Operating Data for TCA Run 501-24 Operating Data for Hydro-Filter Run 501-3A Schematic of Venturi Scrubber and After-Scrubber After Modification Schematic of Three-Stage TCA Scrubber Without Trap-Out Tray After Modification Schematic of Hydro-Filter Scrubber After Modification Typical Process Flow Diagram for Venturi System After Modification Typical Process Flow Diagram for TCA System After Modification Typical Process Flow Diagram for Hydro-Filter System After Modification Venturi Inspection Venturi After-Scrubber Inspection TCA Inspection Hydro-Filter Inspection Comparison of Experimental Data and Predicted Values (Equation 8-1) of Pressure Drop for the Chemico Venturi Comparison of Experimental Data and Predicted Values (Equation 8-4) of Pressure Drop for the Chemico Venturi x 5-27 5-32 6-3 6-5 6-8 7-28 7-29 7-30 7-34 7-38 7-39 7-44 7-48Figure 9-2 Predicted Pressure Drop for Chemico Venturi: One Hundred Percent Plug Opening 8-6 Predicted Pressure Drop for Chemico Venturi: Fifty Percent Plug Opening 8-7 Predicted Pressure Drop for Chemico Venturi: Zero Percent Plug Opening 8-8 Comparison of Experimental Data and Predicted Values of Pressure Drop for the TCA System 8-10 Predicted Pressure Drop for the Four-Grid (No Spheres) TCA System 8-12 Predicted Pressure Drop for the Six-Grid (No Spheres) TCA System 8-13 Predicted Pressure Drop for the Four-Grid ‘Three-Stage TCA System: Five Inches of Spheres Per Stage 8-14 Predicted Pressure Drop for the Four-Grid Three-Stage TCA System: Ten Inches of Spheres Per Stage 8-15 Comparison of Experimental Data and Predicted Values (Equation 8-6) of Pressure Drop for the Hydro-Filter 8-17 Comparison of Experimental Data and Predicted Values (Equation 8-7) of Pressure Drop for the Hydro-Filter 8-18 Predicted Pressure Drop for the Hydro-Filter with Three Inches of Marbles 8-19 Predicted Pressure Drop for the Hydro-Filter with Five Inches of Marbles 8-20 Comparison of Experimental Data and Predicted Values of SO, Removal from Venturi Computer Model 9-4 Comparison of Experimental Data and Predicted Values of SO, Removal in Chemico Venturi from Equation 9-1 9-5 Comparison of Experimental Data and Predicted Values of SO, Removal in Chemico Venturi from Equation 9-2 9-6Figure 9-4 10-1 10-2 Comparison of Experimental Data and Predicted Values of SO7 Removal for the Low Concentration Soda-Ash Data with the Chemico Venturi Bechtel Limestone and Lime Wet-Scrubbing Sim- ulation Program: Venturi Scrubber System Bechtel Limestone and Lime Wet-Scrubbing Sim- ulation Program: TCA Scrubber System Correction of S02 Removal for Water Vapor and Reheater Gas Pick-Up Free Settling Rates of Shawnee Clarifier Feed Solids xii 9-17 10-15 10-16TABLES Topical and Final Report Description Field Methods for Batch Chemical Analysis of Slurry, Coal and Alkali Samples Example of Phase II Report Example of Phase III Report Data Channels Example of Mini-Computer Printout Example of Liquids and Solids Analytical Data Report Example of Solids Analytical Data Report Pressure Drop Data from Air/Water Runs: Venturi System Pressure Drop Data from Soda-Ash Runs with Air and SO, Gas Mixtures: Venturi System Pressure Drop Data from Soda-Ash Runs with Flue Gas: Venturi System Pressure Drop Data from Air/Water Runs: TCA System Pressure Drop Data from Soda-Ash Runs with Air and SO, Gas Mixtures: TCA System Pressure Drop Data from Soda-Ash Runs with Flue Gas: TCA System Pressure Drop Data from Air/Water Runs: Hydro- Filter System Pressure Drop Data from Soda-Ash Runs with Air and SO, Gas Mixtures: Hydro-Filter System 3-10 3-13 3-14 3-15 3-17 3-18 3-19 4-9Pressure Drop Data from Soda-Ash Runs with Flue Gas;:! Hydro-Filter System Sodium Carbonate Runs with Air and SO, Gas Mixtures: Venturi Scrubber (202-1A to 251-18) Sodium Carbonate Runs with Air and SO, Gas Mixtures: Venturi Scrubber (259-1A to 260-1C) Sodium Carbonate Runs with Flue Gas: Venturi Scrubber Sodium Carbonate Runs with Air and SO, Gas Mixtures: TCA Scrubber Sodium Carbonate Runs with Flue Gas: TCA Scrubber Sodium Carbonate Runs with Air and SO, Gas Mixtures: Hydro-Filter Scrubber Sodium Carbonate Runs with Flue Gas: Hydro- Filter Scrubber Variations in SO, Removal for Sodium Carbonate Testing Test Results for SO, Removal in Limestone Wet- Scrubbing Runs: Venturi System Test Results for SOz Removal in Limestone Wet- Scrubbing Runs: TCA System Test Results for SO2 Removal in Limestone Wet- Scrubbing Runs: Hydro-Filter System Material Balance Results for Factorial TCA Tests Spray Tower Limestone Depletion Run with Four Headers (Run No. 463-1A) Effect of Inlet SO Concentration on SO, Removal in a Six-Grid Three-Stage TCA Average Liquor Compositions at the Shawnee Test Facility During October, 1972 Particulate Removal in Venturi and Spray Tower Scrubber During Factorial Tests 5-6 5-10 5-16Particulate Removal in TCA Scrubber with No Spheres During Factorial Tests Particulate Removal in Hydro-Filter Scrubber During Factorial Tests Average Conditions for Initial Reliability Verifica- tion Runs Average Liquor Compositions for Initial Reliability Verification Test Runs Material Balances for Venturi Run No. 501-1A Material Balances for TCA Run No, 501-24 Material Balances for Hydro-Filter Run No. 501-3A Test Facility Demister Specifications Centrifuge Test Results Corrosion Test Results Comparison of Measured and Predicted $0, Removal from the High-Goncentration Sodium Carbonate Data for the TCA Scrubber Comparison of Measured and Predicted SO, Removal from the High-Concentration Sodium Carbonate Data for the Hydro-Filter Scrubber Predicted Values of \ for Venturi Model for Low- pH Soda-Ash Runs Comparison of Measured and Predicted Slurry Compositions at Scrubber Inlet for TCA Run 412-24 Correction Factors for SO, Removal Water Balances for Closed-Loop Limestone Tests at 10,000 ACFM Water Balances for Closed-Loop Limestone Tests at 20,000 ACFM Water Balances for Closed-Loop Limestone Tests at 30,000 ACFM 6-12 6-17 6-20 6-22 7-4 7-13 7-18Section 1 INTRODUCTION AND SUMMARY In June 1968, the Environmental Protection Agency (EPA), through its Office of Research and Development (OR&D), initiated a program to test a prototype lime and limestone wet-scrubbing system for removing sul- fur dioxide and particulates from flue gases. The system is integrated in the flue gas ductwork ofa coal-fired boiler at the Tennessee Valley Authority (TVA) Shawnee Power Station, Paducah, Kentucky. Bechtel Corporation of San Francisco is the major contractor and test director, and TVA is the constructor and facility operator, Three major goals of the test program are: (1) to characterize as com- pletely as possible the effect of important process variables on sulfur dioxide and particulate removal; (2) to develop mathematical models to allow economic scale-up of attractive operating configurations to full- size scrubber facilities; and, (3) to perform long-term reliability testing. The test facility consists of three parallel scrubber systems: (1) a venturi followed by a spray tower; (2) a Turbulent Contact Absorber (TCA); and, (3) a Marble-Bed Absorber (Hydro-Filter"), Each “The Hydro-Filter scrubber has been recently renamed the ''Marble-Bed Absorber," It is referred to, however, as 'Hydro-Filter" in this report. 1-1system is capable of treating approximately 10 Mw equivalent (30,000 acim’ @ 300°F) of flue gas containing 2300-3300 ppm sulfur dioxide. The following sequential test blocks were defined for the program: © Air/water testing © Sodium carbonate testing © Limestone wet-scrubbing testing © Lime wet-scrubbing testing The air/water and sodium carbonate tests have been completed. As of early August 1973, short-term (less than one day) limestone wet-scrubbing factorial tests were 95 percent complete and longer term (over two weeks) limestone reliability verification tests were nearly complete. Long-term (4-10 months) limestone testing and short-term factorial lime testing are scheduled to begin in September 1973. This report, which is the first of three topical reports to be issued, de- scribes the test facility and test program, and the results, through June 1973, of air/water, sodium carbonate, and limestone wet-scrubbing testing. The short-term factorial limestone tests were conducted at high scrub- ber inlet liquor pH (6.0-6.2). Series operation of the venturi and spray tower produced sulfur dioxide removals of up to 80 percent at a total liquid-to-gas ratio of 80 gal/mef and a pressure drop of 10 inches HO. ‘Although it is the policy of the EPA to use the Metric System for quan- titative descriptions, the British System is used in this report. Readers who are more accustomed to metric units are referred to the conversion table in Appendix A.The TCA scrubber obtained up to 96 percent SO, removal at a liquid-to- gas ratio of 64 gal/mcf and a pressure drop of seven inches HzO. Re- movals of 80 percent were achieved with the Hydro-Filter scrubber at a liquid-to-gas ratio of 40 gal/mcf and a pressure drop of 11 inches H,O. Three initial long-term reliability verification tests have been run at reduced scrubber inlet liquor pH (5.7-5.9), and consequently, at re- duced stoichiometric ratio, in order to increase system reliability and limestone utilization (moles SO, absorbed/moles CaCO, added). For the TCA system, limestone utilization was 83 percent with a sulfur di- oxide removal of 80-85 percent and a pressure drop of seven inches H,0. The operability and reliability of the scrubber systems for the initial re- liability verification tests have been good, There has been little evidence of sulfate or sulfite scale after approximately 500 hours of operation of all three systems, with effluent residence times greater than 20 minutes and percent solids recirculated greater than 10 percent (40 percent of solids is flyash). Presently, more severe operating conditions (e.g., lower effluent residence times) are being tested to determine the re- gions of reliable operation for the three systems. 1-3Section 2 TEST FACILITY The test facility consists of three parallel scrubber systems, each with its own slurry handling system, Scrubbers are of prototype size, each capable of treating approximately 30,000 acfm of flue gas from the TVA Shawnee coal boiler No. 10. Therefore, each scrubber system is han- dling the equivalent of approximately 10 Mw of power plant generation capacity. The equipment selected was sized for minimum cost consis- tent with the ability to extrapolate results to commercial scale. The 30,000 acfm scrubber system was judged to meet these requirements. Boiler No. 10 burns a high-sulfur bituminous coal which produces SO, concentrations of 2300-3300 ppm and inlet particulate loadings of about 2 to 5 grains/scf in the flue gas. The test facility has been designed to provide maximum flexibility and reliability as discussed in References 1, 2, and 3. 2.1 SCRUBBER SELECTION The major criterion for scrubber selection was the potentiality for re- moving both sulfur dioxide and particulates at high efficiencies (sulfurdioxide removal greater than 80 percent and particulate removal greater than 99 percent), Other criteria considered in the selection of the scrub- bers were: © Ability to handle slurries without plugging or excessive scaling © Reasonable cost and maintenance © Ease of control © Reasonable pressure drop Based on the information available in the literature, the following scrub- bers were selected: (1) Venturi followed by an after-absorber (2) Turbulent Contact Absorber (TCA) (3) Marble-Bed Absorber (Hydro-Filter) The venturi scrubber (manufactured by Chemical Construction Co.) con- tains an adjustable throat that permits control of pressure drop under a wide range of flow conditions, Although a venturi is ordinarily an effective particulate removal device, gas absorption is limited (in lime- stone wet-scrubbing systems) by low slurry residence time. For this reason the after-absorber (spray tower) was included for additional ab- sorption capability, The TCA scrubber (manufactured by Universal Oil Products and described in Reference 4) utilizes a fluidized bed of low density plastic spheres which are free to move between retaining grids. The Hydro-Filter scrubber (supplied by Combustion Engineering Co. and described in Reference 5) utilizes a packing of 3/4-inch glass spheres (marbles). A "turbulent layer" of liquid and gas above the glass spheres enhances mass transfer and particulate removal. Figures 2-1, 2-2GAS OUT DEMISTER WASH CHEVRON DEMISTER AFTER-SCRUBBER —~_] GAS IN INLET SLURRY ADJUSTABLE PLUG EFFLUENT SLURRY x —— VENTURI SCRUBBER APPROX. SCALE EFFLUENT SLURRY Figure 2-1. Schematic of Venturi Scrubber and After-AbsorberGAS OUT CHEVRON DEMISTER DEMISTER WASH INLET SLURRY RETAINING GRIDS ‘MOBILE PACKING SPHERES GAS IN 5 —I ‘APPROX, SCALE EFFLUENT SLURRY Figure 2-2. Schematic of Three-Stage TCA Scrubber Without Trap-Out Tray 2-4GAS OUT DEMISTER WASH CHEVRON DEMISTERS TURBULENT LAYER GLASS SPHERES INLET SLURRY GAS IN EFFLUENT SLURRY — _, APPROX. SCALE EFFLUENT SLURRY Figure 2-3. Schematic of Hydro-Filter Scrubber2-2 and 2-3 ( drawn roughly to scale) show the three scrubber systems along with the demisters selected for de-entraining liquor in the gas streams, 2.2 SYSTEM DESCRIPTION ‘The Shawnee test facility contains five major areas: (1) the scrubber area (including tanks and pumps); (2) the operations building area (in- cluding laboratory area, electrical gear, centrifuge and filter); (3) the thickener area (including pumps and tanks ); (4) the utility area (includ- ing air compressors, air dryer, limestone storage silos, mix tanks, gravimetric feeder, and pumps); and, (5) the pond area, The test facility has been designed so that a varied number of different scrubber internals and piping configurations can be used with each scrub- ber system, For example, the TCA scrubber can be operated as a one, two or three stage unit and solids separation can be achieved with any combination of clarifier, filter, centrifuge and pond. Some typical configurations for limestone testing with the venturi, TCA and Hydro-Filter scrubber systems are shown schematically in Figures 2-4, 2-5, and 2-6, respectively, Such process details as flue gas sat- uration sprays and demister wash sprays are not shown, For all systems, gas is withdrawn from the boiler ahead of the power plant particulate removal equipment so that the entrained particulate matter (flyash) can be introduced into the scrubber, The gas flow rate 2-6worsdg tanjue, 10j wer BEI MOTT sso00rq TeOIGhT, *p-7 oand1T nog ONTULRS Nv uum syoam ticw<waishs VOL 103 wes8eIg Mog ssor01g [er1dk] *g-z andr Nod aNrUL3swi9ishg 497[1F-O1phH TOF WBIBVIG MOTT ssad01q TeTEKE “9-7 oandrT won fond ate @ ° ‘Noe ONTI3S w = | aw, onuuvinowio3 av 104 amass aan aaustavio | o< om sseenyos alns-oudaa moetto each scrubber is measured by venturi flow tubes and controlled by dampers on the induced-draft fans, The concentration of sulfur dioxide in the inlet and outlet gas streams is determined continuously by DuPont photometric analyzers. The scrubbing systems are controlled from a central graphic panelboard, An electronic data acquisition system is used to record the operating data. The system is hard wired for data output in engineering units directly on magnetic tape and on-site display of selected information is available, Also, important process control variables are continuously recorded and trend recorders are provided for periodic monitoring of selected data sources. Figure 2-7 is a view of the scrubber area looking toward the power sta- tion, Figure 2-8 is a view of the operations building and thickener area. Figure 2-9 is a view of the scrubber control room, 2.3 EPA PILOT PLANT SUPPORT Two smaller scrubbing systems (300 acfm each), which are capable of operating over a wide range of operating conditions, have been installed at the EPA facility in Research Triangle Park, North Carolina, in support of the Shawnee prototype testing activities, The small pilot scale scrubber systems are capable of simulating the TCA scrubber system and have generated large quantities of closed liquor loop data on certain TCA configurations.Figure 2-7. Scrubber Area,Figure 2-8. Operations Building and Thickener Area,Figure 2-9. Control Room.Section 3 TEST PROGRAM This section contains a description of the test program. Other descrip- tions have been presented in References 2, 3, and 6, In Table 3-1, a description of the reports which are presently scheduled for general dis- tribution is presented. 3.1 TEST PROGRAM OBJECTIVES The overall objectives of this program are to evaluate the performance, reliability and economics of closed liquor loop limestone and lime wet- scrubbing processes, The following are specific goals of the program: © Investigate and solve operating and design problems such as sealing, demister plugging, corrosion and erosion, e Generate test data to characterize scrubber and sys- tem performances as a function of the important process variables. © Develop mathematical models to allow economic scale-up of attractive operating configurations to full size scrubber facilities and to estimate capital and operating costs for the scaled-up system designs. © Determine op2rating conditions for optimum SO, and particulate removal, consistent with operating cost considerations. © Perform long-term reliability testing. © Study various sludge disposal methods. 3-1Lot ‘Aine PL6r “yore £261 ‘xoquTEAON EL61 Gsndny Teaypmys spurouoss pue uBysap dn-ovos ‘s[apour [espeuroyyeur ‘sz]nsex 3893 AWIqet192 oucysaur] pue surt| Uo syseydurs axemonaed yyym wesdord 4893 [e307 Jo Azeuiung *Burjs03 Asrmiqettes ouoys oust Jo sngejs pur eiep Jo uoreesdremut ‘yuourdotoaop Tepour ssevoad so sngeys ‘Bu13803 ouuTT TeTL039eF Jo synsex ‘suSysop 3803 jenjoe pur pauueyd ‘But -is0} uoeorstsen AITTEQETIOx OWL YIM parETooSse suornjoses pur suisjqoad yeuoryexado jo Axeurumg +aunsoa Arqertes uisey- Buoy sucysoury] 107 sxoyoureaed Jo UOT;D9[98, pu juowdoraaap [epout ssao0.1d Jo snyeys ‘ezep Jo uorwoadsoqur ‘uspsop 389} pengoOw pue pouueyd «Surjso3 uoTeoT49A AGTTEGRTIOE Ya poyersosse suoynjoses pure suxstqord Suryersdo jo Axeurumg veyep Jo worRerdsaqUE YsTM Bursar auoysousy] [epx0}0%} Jo synsox ‘usudojeasp [apour oy wyep JO woHeZTTTIN ‘Buysa; §OO%eN pur royEM /are jo sy[neex ‘sudzsap 389) enqOe pue pouueyd ‘suornjosos pur sura[qord Teuoryexado Jo Axeuiung qaodey yeurg ‘Aye ase, Berqqns9s HeXLY Vas synsay ys0L urqqnssg -39M OUT QTR asx, Burqqnsog Tey Vdc syinsoy yay, Burqqniss 39M ouo3souNPT HGHTFORT aseL Suyqqnsg HexIV Va si[nsoy ys0q, euoysowry pue ageuogzep umypes soe ase Burqqnsog TeITy Vast 1 eve uoneotiand yesouay, payeurnsa papnyour aq 03 uoreuLt0suy py, a0doy NOILGIYOSAd LUOdAY IVNIG GNV TvoIdOL Ire o1qey 3-23.2 TEST PERIODS AND TEST PROGRAM SCHEDULE ‘The following sequential test blocks have been defined for the test program: a) (2) (3) (4) Air/water testing Sodium carbonate testing Limestone wet-scrubbing testing Lime wet-scrubbing testing The test program schedule is presented in Figure 3-1, As can be seen in the figure, the air/water and sodium carbonate tests have been com- pleted. As of early August 1973, limestone wet-scrubbing short- term factorial tests were approximately 95 percent complete and longer term limestone reliability verification tests were nearly complete, 3.2.1 Air/Water Testing These experiments, which use air to simulate flue gas and water to simulate alkali slurry, are designed to determine pressure drop model coefficients* and observe fluid hydrodynamics (e.g., Hydro-Filter tur- bulent layer) for all three scrubbers in clean systems, Mathematical models describing pressure drop, particulate removal and sulfur dioxide removal for the three scrubber systems have been presented in Reference 7.ainpeyss say, eoumeys *[-¢ oand SHIGALS UVWILSI LSO9 8 ONISTINIONG 5ys9) Aunaeti0u S4sa] voNeOYLEA ANLIRHOY SySa] jels0,2e4 ul19-YOYS *ONILSA. ONI@GNYDS-13M 3WIT SNOLLVDISIGOW WALSAS —EE P20¥1NO WOE sys01 AMIR HEN - in SySa] lelsoyoe4 w91-Y10YS ld s1s01 uoneoyli0/ AULgeHOY ieee $982], e140}924 Wa ]-YJOUS, *ONILSL ONI@@NYOS-13M 3NOLSAWIT oe ‘ONILS3L ULYNOYVD WN1GOS 8 YaLVM-8IV | 4N0-493H9 W3LSAS sefveyez| zz UAT STIST [Pere tor] 678] 2] 9] S[Pyeye|t viwisirla vir [riwiviwistr[o[Nfolstwir [riwiy [w SNOLLONNJ WYU9OHd 1S3L v 6 26 3-43.2.2 Sodium Carbonate Testing Two series of sodium carbonate tests have been designed, The first, or high concentration series, utilizes concentrated (~1 wt % sodium ion) water solutions of sodium carbonate to absorb SO, from flue gas and from a synthetic flue gas composed of air and S02. These tests are designed to determine uncertain model coefficients where gas-side mass transfer is rate controlling, The second, or low concentration series, uses dilute (0, 1-0, 5 wt % sodium ion) sodium carbonate solu- tions to absorb SO2 from flue gas and synthetic flue gas. For this series, gas-side mass transfer is not rate controlling and liquid-side mass transfer uncertain coefficients can be calculated using relation- ships for gas-side coefficients developed from the high concentration tests. These runs also help ascertain the absorption capability of liquors associated with some variations of the Double Alkali scrubbing process (see Reference 8) over a range of operating conditions. 3.2.3 Limestone Wet-Scrubbing Testing The primary objectives of these test sequences are: (1) To characterize, as completely as practicable, the effect of important independent variables on partic- ulate removal and SO, removal. (2) To identify and resolve operating problems, such as scaling and demister plugging. (3) To identify areas or regions for reliable operation of the three scrubber systems, consistent with rea- sonable SO2 removal, and to choose economically attractive operating configurations from within these regions,(4) To determine long-term operating reliability with attractive configurations for one or more of the scrubber systems and to develop more definitive process economics data and scale-up factors. To accomplish the first objective, a large number of short-term (over four hours) factorial tests have been made for each scrubber system, To accomplish the second and third objectives, a relatively small num- ber of longer term (over two weeks) reliability verification tests will be made on each scrubber system. These longer term tests will also be useful to: © Obtain more reliable material balances, © Quantify any variations in SO, and particulate re- moval and system slurry compositions with time. The fourth objective will be accomplished by running reliability tests, lasting from 4 to 10 months, on attractive operating configurations for one or more of the scrubber systems. During these tests, the systems will be carefully monitored for potential long-term reliability problems, such as erosion and corrosion of system components. The ability to effectively operate such systems under varying gas rate, particulate loading and SO; inlet concentrations will also be studied during this period. During the short-term factorial test period (see Figure 3-1), it became apparent early that it was not feasible to operate the test facility in a 3-6totally closed liquor loop without facility modifications." A closed-loop test is a test wherein the raw water input to the system is equal to the water normally exiting the system in the humidified flue gas and the waste sludge transferred to the pond. In an open-loop system, raw water input is greater than the water outflow in the exit gas and sludge. Therefore, process liquor must be discharged from the system to maintain an overall water balance, In a commercial sys- tem such discharge may not be acceptable due to potential water pollu- tion problems. Also, during open-loop operation reliability may be un- intentionally enhanced since the additional raw water added tends to desaturate liquors returning to the scrubber, thereby tending to reduce scaling and plugging. Open-loop operation was not considered to be a serious problem during the short-term factorial testing, since, ata specified scrubber inlet liquor pH, SO, removal is not significantly affected by liquor composi To date, therefore, the order of limestone testing has been (sce Figure 3-1): (1) Open-loop short-term factorial testing (2) Closed-loop long-term reliability verification testing The modifications were completed during a five-week boiler outage in February and March, 1973 (see Figure 3-1), The major modifications included: eliminating pump seal water on the Allen-Sherman-Hoff pumps by changing from Hydroseals to Centriseals; humidifying the hot inlet flue gases with slurry instead of with raw water; and washing demisters with process liquor diluted with raw water instead of with vaw water only, Other major modifications to the systems during the boiler outage, not necessarily affecting the water balance, are dis- cussed in Section 7 and Reference 1.3.2.4 Lime Wet-Scrubbing Testing This test series, which involves introduction of hydrated lime (calcium hydroxide) directly in the scrubber circuit, will resemble the limestone wet-scrubbing test program, The major difference will be the absence of any open-loop tests. Again, tests will be divided into three general categories (see Figure 3-1): short-term factorial tests; longer term reliability verification tests; and, long-term reliability tests. 3.3 TEST DESIGNS The test sequences for the air/water, sodium carbonate and limestone and lime wet-scrubbing experiments are all full or partial factorial de- signs based upon the chosen independent variables, their levels, and the restraints of time (outlined in Figure 3-1), The choice of the indepen- dent variables and their levels was based upon pilot plant test results, the restraints of the system, and results from mathematical models which relate the dependent and independent variables. ‘The air/water and sodium carbonate experiments have been completed at the test facility and a summary of the test results and the independent variables and their levels can be found in Section 4 of this report. A majority of the short-term factorial limestone tests have also been completed at the facility and a summary of the test results and the in- dependent variables and their levels can be found in Section 5 of this report. 3-8Since each limestone reliability verification test will last about two weeks and assuming one-third downtime for each system (for inspec- tions, cleanings, etc.}, only about six tests can be made for each scrubber system, given the restraints of time outlined in Figure 3-1, Obviously, not all variables which are assumed to affect system reli- ability can be comprehensively studied for each scrubber system within the six-run limitation, * The variables being investigated are: © Percent solids recirculated © Effluent residence times © Gas rate © Scrubber inlet liquor pH © Demister types (e.g., plastic versus stainless steel chevron) Solids separation tests for the clarifier, filter and centrifuge are also being made on the three systems during the test period. Results from three initial limestone reliability verification test runs are presented in Section 6 of this report. 3.4 ANALYTICAL PROGRAM Samples of slurry, flue gas, limestone and coal are taken periodically for chemical analyses, particulate mass loading and limestone These tests will be supplemented with reliability verification tests with the EPA pilot TCA scrubbers at Research Triangle Park, N.C. (see Section 2.3)reactivity tests. Locations of slurry and gas sample points are shown on Figures 2-4, 2-5, and 2-6, A summary of the analytical methods for determining important species in slurry, coal and alkali is pre- sented in Table 3-2. Table 3-2 FIELD METHODS FOR BATCH CHEMICAL ANALYSIS OF SLURRY, COAL AND ALKALI SAMPLES Field Method Sodium Atomic Absorption Potassium Calcium Magnesium X-Ray Fluorescence Chloride Total Sulfur Total Sulfite and Bisulfite Dead Stop Iodometric Total Carbonate and Bi- Infrared Analyzer carbonate Nitrite Ultraviolet Technique Nitrate Six DuPont photometric analyzers are being utilized for continuous SO, gas analyzing at the inlets and outlets of all three scrubbers. Values of pH are monitored on a continuous basis using fifteen Universal InterloxpH analyzers, and three Universal Interlox electrolytic analyzers are used to monitor electrical conductivity. A modified EPA particulate train (manufactured by Acrotherm/Acurex Corporation) is being used to measure mass loading at the scrubber inlets and outlets. 3.5 DATA ACQUISITION AND PROCESSING Operating and analytical data are recorded automatically onto magnetic tapes at the test facility. These are sent to the Bechtel Corporation offices in San Francisco for processing. Additional data is recorded manually in operating logs and graphs by on-site personnel. 3.5.1 Operating Data (Scan Data Acquisition) Over 150 pieces of "scan data" (flow rate, temperature, pH, etc. } are recorded automatically at fixed time intervals onto magnetic tape at the test facility. Each piece of scan data has an associated channel number, The scan data acquisition system was designed and installed by Electronic Modules Corporation, and the tape recorder was supplied by Cipher Data Products Corporation, A backup printed record on paper tape is available if the recorder malfunctions. ‘The scan data tapes are mailed to Bechtel Corporation in San Francisco for processing. Preliminary processing consists of reading the tapes, translating the coded data into comprehensible numbers and producing a "Phase I" file of the raw data in "time order (successive channels at a given time).